Document jgkEQGzZxgJ93nQXx3b6KzvRp

DEFENDANT'S 1 EXHIBIT I paoms FOR THE K&HWACmCS OF BXPHEMYL & SAWOWkX CompHad "by E. Mather* Bovenb** 1950 Mstritratien Lists Mr. 8. A. 0v8o*l# A*., London I*. H Oorrott, London Er V D. Scott, London Mr. J. 8. Brough# London It*. D. V. Vtwdxt,, London Rmbon. Rwwttdh FU@ (Mr. V.H. Ritchie) Mr. 6. V. ffegrlor, mmport (2) 1ft*. P. J. 0. Bo<di Heuport (Amlj^tioal seotlon only of the report) Mt. 0. B. Durgin# AtmlMtm. A. M EHeaburg# Anniston Mr. J. V. Fetmlx^tan of K.O.L.# ' (*t Aaalstwi,, Borwrtwr 3550) St. Louis LlMtrj St. Louis Jt.C.L. file (E.Mithar) A#055 WATER PCB-SD0000045422 OTOODOCTOig VOTE 1 FrtHMn&ry Information mm seat from Anniston to Hr. E. A. 0 *%, in London, 3mm 1946, If* B, S. Bavarereft and th writer paid a brief visit to Aanil ton in Septertser 1947 to collect information needed for craltsatieta aM design work la London, and they produced to report "lot* on the Process for to Hanufaotur of Diphenyl & Saatewax at Anniston", September 1947. A set of Anniston drawings, out of over 350 drawings on file, was sent to London shortly afterwards, the selection being such as would giv full constructional details relating to Anniston's preferred designs. Since then there has been a great deal of correspondence be tween M.C.L. and. Anniston; Hr, H. L, Barden visited Anniston in August 1950 to review the process from the angle of pro duction work rather than design work, (see the relevant chapter of his "Report on a Visit to U.S.A. w, August 1950)# and the present writer visited Anniston November 6-10, 1950, mainly to deal with certain questions raised by the M.C.L. mechanical engineers. This present report is intended to condense the information, collected as above, into a fora convenient for use within Monsanto Chemicals Limited, particularly in production work. It is hoped that it will be of use in the final stages of toe construction of the Newport plant, and that it will form the basis of an operating manual feu* use at Newport, to be supple mented and kept up to date as new informtion ernes forward. r \ OSW 462056 WATER PCB-SD0000045423 EAMjm REBOOTS la a letter to fte*. D. S. Surereroft, S@pt.XlA7, Mr. K BuIb listed the following, nlx reports which were already la London files* derma Chaaieal industry Report Series derma Production of Biphenyl, Terpheayls aad OU.orlm.ted D@rTatiw@s, by Wayne B Alexander, K.C.O., St.Lowis, Oct,4.1948. Extract fram. Qema Report, G.I.O.S. XXH-14 pp,56-57, Mph&nyX. - Design Bata 4th Diphenyl t&slt, D.A,Roper, with Study of Biphenyl Costs, E.H.Alford, 8.9.39. Final Report on Plant Seats oa Ho.6 Biphenyl Chit - Part 1. Job Ho. 171=41 PH Ho. 138, 17th Sept. 1941. R.A.Ewlng. Design Data for Biphenyl Still, D.A,Roper, Sept, 1939 Report Ho.1924 Final Report on Separation of Biphenyl High Boiler Into fractions or known Mixtures Part III * Dereloping Plant Processes for Production of Santowaxes R.O.K.P. & MP. Job Ho. 171-61, File Ho2l8-B. Prepared by A.K.Elleaburg. "Equipment Design for Santowax R Plant, May 20A3% Job 1-352-Rsport #31 by G.R.Shockley, accompanied this report. 2a September 194j, B. S Bayercroft & E, Mather wrote a report Hote 0 the Process for th Manufacture f Biphenyl & Santo- wax at Aunlitm. " Ota S@pt.25A7 copy #H of Anniston report? 1640, Pinal Report on Study of the Biphenyl Process Part 11. A Rerteiir of the Process. Job 171-41, Pll 138, F.E.Hubbard, Anniston, 0ct.l5Al, was handed to lft% IfcYereroft for London, also a copy of Addesdtm to 1712, Pinal Report on Study of Biphenyl Process, ^artlll, Oootinufms Let-down Procedure, Job 171-41, Pile 138. A. M. EXlenburg, Anniston, Jhn.3lA5 DSW 462057 WATER PCB-SD0000045424 Earlier Reports, ootaM 3 On Oet,13/47* microfilm eople# of the following two reports wwm seat to Mr% W. M. Cooper* London: 1542. Pinal Report cm Mphenyl Operations, J.E.Moose. OctobF 1WT" ` ' 1T12. flml Report on Study of Diphenyl Process, Part til, HuFbartiV SUraTfe Kilee, Anniston, Oet. 19/42. Cm lar,ll/48, a oepy of report 1937t ''Highly <30.orlmt@d Qmterpheayla" ms seat I5c^f7LmE& to RrnWi. Kr. Ellehburg, Jhnu&ry 20/48, revered the following reports s 214 "Benzol Losses in- Waste Hydrogen, frost. Diphenyl Plant*, J.L.Ecnrerton, Sept.22/33. 445 "Reooameadatioas for the Operation of the Crud Diphenyl Still*, J.H.Cai*othrs, June 23/33. 948 "Investigation of Benzol Losses --- at the Diphenyl Plant", Borton Harris, Aug,21/35* _ Mr. EUenborg, Apr.28/48, cited the following reports on the (}ma tube process* (1) Z.G.F&rfeesiMttstrie at Leverkusen Germany, Jol^25^45^)A Y1s It hy Turnoclc & LovderBilk, (2) B.I.O.S. Pinal Report #893* Itea #1, (1947) Pay & Richards. A copy of Anniston report 2211 "Interim Report on Alloy Test ing , 171-429* V.V.mde, Apr.22/48, discussing the corrosion erosion of the lead pots lay the vapour blast, ms sent to London (lir. B&vercroft)* July 1/48, A glorofUs copy of the Organic Dlrlsion report "Diphenyl from Benzene", H7-881, Oet. 5/35* on the effect of lsf>urities la benzene, we sent to Mr. Thrift of M.O.L., fey 9/49* The prooess description in this report is said to hay Wen "bailed largely on that of the report ''Design Data for 4th Diphenyl Ttoit", hr D.A.Roper. DSW 462058 WATER PCB-SD0000045425 QWLTSE OF PROCESS AS WORKED AT AKNISTOK, 1950 5 Bmsem vapour Is passed continuously through aoXtea. lead, at a high temperature, causing soe 16% to 20$ of the benzene to be converted, In a single pass through 3 lead baths In series, into a mixture of diphenyl, tsrphenyl, etc, with the volu tion of hydrogen, ffh resulting mixture of hydrogen with the reaction produoti and the unchanged benzene is passed up a fractionating coluoat which has a condenser and reflux split box, so that the sensible heat of the vapours is used to give a rough separation cf the organic components of the mixture. The fra,otionst ion system yields a forward flow of liquid ben zene, and an underflow of a Mixture of benzene, diphenyl, terphmsyl, etc,, while the hydrogen passes forward, saturated with benzene* This hydrogen stream is cooled and cospressed for the recovery of more benzene. The column underflow is fractionally distilled batehsriLee at atmospheric pressure to yield distillates of benzene and of saleable diphenyl, and of course,intermediate fractions which are recycled to the still. The still bottoms, containing the higher boiling covenants of the Mixture, are called crude Santowax. -<-- Soiae of the crude Santowax is distilled "straight-over, under vacuum, to yield Santowax R, and scuse 1 put to permanent storage because the supply exceeds the demand. Crude Santowax has also been distilled under vaeuma, with fraotion&ticm, giving ortho terphenyl of about 9%$ purity. Centrifuging of the distillate, or better, fractional distilla tion, gives a better product. The -p fraction from distillation, Ms been allowed to cry stallize in pans, slurried with water at about 85C, centri fugated and washed in the centrifuge with hot water. Tb centrifuge cake is then about 95$ para terphenyl. The oil from, the centrifuge liquors, separated and dried, is called "Santowax K", See Anniston report #192%, Jhn.8/%5* See page 50 below for a not on the flaking of Santowaxes, All the recovered benzene 1* recycled and there is a practi cally continuous mke-up of fresh Material. This is believed to ensure the presence of a certain catalyst which is present in the raw benzene, but eliminated by the processing. (See under "Consents, on Process", page 111 below). DSW 462060 WATER PCB-SD0000045426 HOTE OH CHOICE OF PROCESS Sec til Anniston. Report 1640, Oct,15Alj F.E.Hubbard, also A* K. EHeaburg's latter of April 28/49, siting B.I.O.S. te. reports on the "tube" process. The research dpartrouts at Rmbon and Anniston agree la be lieving the tribe process my be superior to the lead pot process. Sew pilot plant work 1ms bees done in this direc tion at Anniston. See page U6 below for the choice of the nethod of recover ing eensene fro* the offgam. 6 DSW 462061 WATER PCB-SD0000045427 OWLETS FOR PRODUCTS T At Anniston seam of the diphenyl is flaked for sale, hut by far the greater part la used either at Anniston or at Monsanto, Illinois, for the Manufacture of Aroclors. Monsanto Chemicals Limited do not aspect to @U diphenyl, A little also Is used at Monsanto, HI,, for the Manufacture of o. & p, amino diphenyl, A Mixture of crude Saatowax and diphenyl my be chlorinated to give th Arcelor 2565 used as a roofing compound, Saatowax R Is used as th starting Material for Aroclors 5442 & 5^60, also for tb hydrogenated product HB-40, which Is used as aa Bextetader* in plasticizer, for example in Vinyl film. The Saatowax R 1ms com little application In high tem pera ture greases for valves. Monsanto Limited have given boss consideration to the possi bility of usefully disposing of still residues. Dr. Scott, January 29/48, considered that the residues would not be suitable for asking firelighters. Dr. Bsrdy, March 4/48, passed on Mr, Ellenburg's review of the possibility of chlor inating the residues to about 60-65$ chlorine content to oak a cable Joint-box eomosition, Mr, ELlenburg thinks that chlorination at 250-2o00. to 35-40$ would be about the best procedure, but warns us that the residues are not of constant composition. It was thought at one time that M.O.L, markets would call for a higher ratio o.f high boilers to diphenyl than is normally obtained in th Anniston process, and sea thought was given to the possibility of shipping some of the Anniston excess stock of high hollars to Britain, and calculations of th to itish i^jort duty were made. Ur, 3". Y. Head's note of March 2/48, however, indicates it is now Jjiprohabl that such shipments will be necessary. Reference is made to a Memoran dum by Dr. D, Scott of Rusbon, dated June 20A?, on the long ter development of outlet for diphenyl. In th distillation of crude Saatowax to give Saatowax R, about 15$ of th weight of th crude is left aa a residua, and aom of this is sold as "tontar 9n. , Seat of the hydrogen after cooling and egression, as out lined above, 1 used for th hydrogenation of Santowax R to give HB~40, Any excess of hydrogen is vented to atmosphere after being eos^ressed and cooled. At on time Anniston put the excess hydrogen Into the fuel gas for the furnaces, but th consequent change* in th air requirement of the burners were troublesome. DSW 462062 WATER PCB-SD0000045428 scale eg uomam 8 About 950,000# diphenyl par north, and 80,000# Bmtamx R per nth. w produced at Anniston. during the first alee months In Septeasber 19^9# slaa imits were In operation, each rated at about 4000# diphenyl per day In love^ber 1950, there tper twelve units, auabared 2-13, in existence, the original Ho# 1 having been taken out lenport need were estimated by Hr# Cooper, Oet.lA?, to be 1,000,000 lb diphenyl & 240,000 3b Sa&towx per year# 5b asnml sales of tbs ortho tarpheayl have averaged only around 4000 lb, &ssd those of ^Saatowax MB around 10,000 lb. There has been very little sale for the para isomer# c \ DSW 462063 WATER PCB-SD0000045429 PATKBT POSUIOT 3 Aimlstcm Reaoareh Dspartawitj Hebert H l64-05 page* 6, 9 r DSW 462064 WATER PCB-SD0000045430 PROPEBTES OP MATERIALS OOBGgRHro 10 Benzene N.Vt. 1C. Ft. B.Pt. Specific rarity Specif1 Heat* solid liquid Vapour Op 78 A3 0 800 0,883 to 0.886 15.5A5.5C W (1*0.T.) 0,463 Formula for Sp.Et, at eons taxit pressm**" Cp s 0,258 f (0,000875 X 0) Perry 1st Edn. 0.266 * (0,0006732 x OO) led,Eng,Ch., July 1935. Latent Boat, B.t.U./lb: fusion rporatlon 54,5 169. Flash. Point Ft closed Clsreland 12 ExplosiY Limit 1n air* Lower i> tipper ^ Awto-i^ltloa temperature 1.4 8 1076f. DSW 462065 Wpour Pressure* Constant In Y,Pr. Forsala Log10 pr, bus*. Hg Range AB *B IPeBp.ats. 58 to -30 -30 to -81 5 0 to 42 42 to 100 42,904 44.222 34,172 33.295 '-- a ,*_ ^----- _____________ ea m T.f&f 7.6546 TAaO * a /m WATER PCB-SD0000045431 Properties of Materials OonegroM, eostd 1. Benzene (eoutd) Thermal Gonduetirity, (liquid & gas) See sheet 3, Design Data for Utaita 4 & 5# D. A. Roper, fog* carrot. 11 2. Diphenyl See Beserii>tiesi of Process used in Dept,246 \ Sept,27/46, Igrles, Sofrraalco t; Becker, pages 49 & 61. . See also Desiga Data for 4th Biphenyl Halt Aug.9/39, Specific Gmrityi 0.992 @ 75C/4C The Swan, Chemical Co. "bulletin of 1930 gare thermal data <m. dlphmxjl, YlMOOBltr of Diphenyl (from Amistoa files) Ceatipolses ISO 170 180 190 200 220 250 300 350 400 m 1.439 1. 1. 1.114 1.034 0.901 0.75? Specific Beat (from Amiston file*) F B.t.U. Ab 200 300 400 500 600 700 800 900 1000 0.416 0.658 DsW 462066 WATER PCB-SD0000045432 Properties of Materials Oonoern&dj oontfi' 2, Diphenyl (oontd) /' Another reeoM gi^es the following values for llqtd.4 . dlpbstqrlt e gpBbat ealg./gra 100 0.3g0 150 O.ffto 200 0.*12 250 0.460 300 0.5X8 ?S2 0*575 0.610 450 0.625 V&POOT op 0.460 25W o.< 4! (D.A.Hoper, Design Data for Halts 4 & 5) Density of Liquid Dipfaaayl (fro Amis ton files) gTMS./oO 75 100 150 200 250 300 450 Beat of Wp-erlmtlottt . 65.4 g.csl/g 6 258.5C< 12 0SVJ 462067 WATER PCB-SD0000045433 Properties of jfatortala Concerned, omtd 33 3# Santamx R eont&im about 2^ diphenyl Iw ortho tesrphai^l nata terpfaenyX 22^ par taxphanyl 22^ trlortJttrabe^rla.qxatesTh3yls etc. (Amlstm Flml Hsport 3$42) . Ufcper bold point Lovwr bold point 137-l430* 45-o00a Changed ) 13Tl45c Sept. 23/4? 5" 45-63C Th density of tbs Santow&x- my b@ acs4 to b the sam is both, tbs erod and distilled form. Viscosity also is tb sfiat, Specifle Orarity of Prude Santemx; X4O0 175 215 300 1.026 1.000 0.98 0.984 (est. from curve of other points). Viscosity of Saatowg H 155C 225 32.4 Saybolt TSiiversal S&eonds 3.5 "" MoXtoa. Santomx flow about Ilk water at 25C. (A.K.Elleoburg' s letter Jto,6/49). Specific Boats (estimated) Solid 0.4 Liquid 0.5 latent Seats (estljatad) Fusion 63 B.t.TT./Lb Vaporisation 140 B.t.tf./lb Boiling Brag* 36q-4500 Flash Points 01. open otp 191C. dS^ 462 FXaaa Fointt d. ep osp 2380 Another aeeotat glv Flash Point 190Cj Plane point 220e. WATER PCB-SD0000045434 Properties of |fafeerlal OoaeeroM^ eontd 3* Saatonmx R (eogrtd) %1ms asstnwd la th design of the Santowax still at Asmlateai Sp,Baat - 0,5 . Bs&t of Vaporization - 140 B,t,T?,A& Vlsooslty at 250C - 5 cenfcipolses * Viscosity at 350C - 2 oeatlpcd. doi * * (Mr. Bllenburg said fches mXues war too high),, 14 Cmd ortho fSaatomx 0) Crude isata. (Santowx M) Oral pars (S&ntowax P) a - p eutectic Ternary eutectic . fEoXd Point" B,Pt, 30 aan 1C ) 2050 xir0* ixfctffe 240C about 74C. See also Konsaat Toobnie&l Bulletin #F-103, Jan,4/47 issue, fee? the properties of the separated crude isomers sold. DSW 462069 WATER PCB-SD0000045435 -I HEAT BALAfCE 15 Th& hd&t balance Is discussed In the Anniston Design Data A 4th Unit, by D, A. Roper, Aug.9/39t page 6. Tb heat of reaction of bensene to diphenyl la given as 59.29 lbC per lb at T*0G. . Irans.AJt.Cbea.Eog, V, 41, p.l44, (1938)* gives 61 lbC per lb. This 18 calculated to b lets than ^ of the heat needed in a 3-pot unit. ^oi os^ WATER PCB-SD0000045436 SAFETY COBSrDGRATIOJB 16 {Proa AtmlaUm report 1642 of October 1941, section "Health & Fir Hazards, ", and fro* discussions at Anniston in 194? and 1950). . Health It is obviously advisable for the operator* to ainiialB their contact with benzene vapours and with the vapour from the hot lead, but there Is no history of trouble fro either of these in the Diphenyl plant. We are warned that lead vapours may be evolved during the burning out of lead traps and carbon traps. When lower grade benzene was used for ssaking diphenyl in 1930-31, the operators In the Aroelor departmnt suffered from skin eruptions (acne), thought possibly to be due to chlorine deri vative from styrene in the diphenyl. The disappearance of the trouble coincided with the change to batter benzene. For a tine the Aroelor operators had to bathe on leaving work and a change of work clothing was provided, but this practice was discontinued. See notes on pages 20 & 82 below relating to the general venti lation of the building. Fire The converts lem units contain hydrogen and organic vapours at high pressure and tesperatures so any failure of gaskets or of the units themselves my lead to the escape of & cloud of inflaanable vapour, near to the pot furnaces. The aaomt of organic material present in the conversion unit at any on moment is, however, quite small, and the flow of benzene to the units can be shut off fro outside the building. In the early toys at Anniston, fires were not infrequent, but there has been none of consequence In recent years. B^haais is laid oa good workmnship in the construction and mintenanee of the tmlts. There were twelve conversion units at Anniston in Hovosber 1950, with their columns and other auxiliary eqmljwMt, two of the units being In on room, four in another, and six In a third room. The three rooms are separated by fir walls with eorasunieating doors, sons of them autcmtieally closing, but held open by chains having a fusible link. There are two DSW 4G2071 WATER PCB-SD0000045437 Safety Considerations, eentd 17 Fire, eontd diphenyl stills, each in its own j^oa, these two room baring connecting doors into one another, but not into the conweraion room, Tim still, rooms contain th receiwers for the finished diphenyl, th heads and tails freetions, and the still bottom, but the benzene receiver ia ia & pit, behind a fir wall out side th building, Th erode diphenyl frets th ooaswertor olinms fleers to two receivers which are outdoors, alongside the benzene receiver. The min store tanks for fresh, benzene are in a fenced area, wen away fro* any manufacturing buildings, and th benzea feed tank and pumps are in a imller feaeed area, somewhat nearer to th diphenyl plant. Benzene weasels are systematically grounded (earthed). See th aot on page 83 below on the objection to internal steam colls in th benzene tanks. ' The department is well supplied with extinguishers, both CO2 and CClh types, and there is a permanently piped Poamite connection to the min benzene weasels. There ia a drum of 0034 on a stillage on th ground floor of the conversion room for recharging extinguishers, and all the appliances are sub ject to routine inspection. . Cloths soaked in CCI4 are used to stop off pipe openings etc. during repair work and the units may be filled with C02 during welding repair, The eoawertor rooms are not treated as hawing a dangerous atmosphere. It is not at all unusual to haws scaping vapours burning round the cower of the convertor pot (especially now some of the convertors are being run at over 20 psig). If vapour leaks from the pot flange, it my not ignite, especially if th seal between pot and furnace is good, but it is better to ignite th vapour rather than to hare diphenyl subLiming about the building,and lodging on roof members, etc. Welding is done in th building, and of course, some of th vapour pipes are red hot. Naked flams are used to deal with blocked pipes in the conversion system. The diphenyl still rooms do, of course, contain large amounts of eoa&uatibl material because of th batch mture of the operation. Tim heating coil furnaces for th two stills are side by side in a room of their own, cut off from all other room. Those of the still receivers which are indoors have went pipes, carried out through the roof of the building, and the outdoor n.9\A/ /1G0IV70 WATER PCB-SD0000045438 Safety PenalAerations* eonfed 18 Fir, entd bonssen# r@eeY@r has Its Teat pipe carried well up into the air, Each itill body has a bursting disc la a pipe leading through th roof# (set page 96 below), ' Amistan are a little restricted in doing welding repairs to their Smtmmx distillation system because of its proximity to the 815-40 plant*which uses hydrogen tasder high pressure* Shi receivers for the hydrogen at each stage of oppression tawlWli bursting discs* in pipe Tenting abore the roof of the greaser room* Care is needed* of course* in restarting the gas-fired, furnaces. There is a powerful draught up the furnaces and the pilot Jet my easily be blown out. Mr. SHenburg* Augl8y48* stated that Class 1* Oroqp D motors are specified for pusping diphenyl and Santotsax. Be also stated that the bottom fro the diphenyl stills* if discharged at arotssd *00C* may take fir. At one time it was the prac tice to purge the stills with COg before recharging, but this Is not now thought necessary* and all that is done is to allow the atIlia to cool to about 2000 or lower before re charging. hs the crude diphenyl* hot froa the store tanks* is pusped into the hot still, there my be a great rush of vapoua? through, the condensing system. Since the introduction of the restriction orifices after the coarertor pots* these pots hare been running at about 20 pelg* that there is a greater risk of blowing out the gasket on the etiTsrtdr orer. Some of the conTertora hare been fitted with a loose sheet iron ring fence about 6B deep* ronad the oorer Joint* to deflect any possible burst of flam. Fir Fighting Equipment Mr, Harden* August 1950* reported a follows 1 "An?! 00a M fmm extinguisher are prorided, Annis ton hu two standard foam extinguishers on each floor of the otsvertor section and soreral in the distilla tion section. On th ground floor* available for use throughout the diphenyl aroeler shed was a large hand cart fern* appliance. The h&nsmm tanks are permanently piped* to top of each tank and into th swp* for fmm which is implied froa * central point11 DSW 462073 WATER PCB-SD0000045439 Safety Considerations, ontd 19 Ptre Fighting Equipment, oootd. Each convertor tmit 1ms about a 56 lb cylinder of GQp per manently connected to a valve leading Into the benzene feed line where it mass below the operating floor before rising to the top of the vapourizer. These cylinders are supported against the stanchions on the ground floor* Mo provision is mad for warning the* A drtna of 0CX4 is kept on a stillage oa the ground floor for easy recharging of the extinguishers. There are numerous safety shower, each with the usual yellow painted ring oa the floor below the*. Hydrogen The conversion units contain hydrogen, and @0 do the crude diphenyl store tanks, because they are vented Into the hydro gen min. The vent pipes from the crude diphenyl tank to the hydrogen min are usually very hot* Air must of course be purged from the system before any hydrogen is taken to the eDepressors, and usually COg Is used for this purpose (kOO cu.ft. for a convertor unit), also to replace hydrogen before a unit is opened for repairs. Thar is no bar* in allowing the COg to go through to the hydrogen aengrossers, in fact there is the advantage of recovering its benzene content. It is no longer thought necessary to do oxygen determinations on the hydrogen stream. The crude diphenyl rocelvers are vented into the hydrogen collecting ays ten, and there is a risk that if they are pumped ts^pty, the hydrogen my escape into the diphenyl still system* Welfare As already mentioned, only ordinary common sense care is taken against poisoning by lead or benzene, and no special clothing is supplied beyond face masks and leather gloves for mm dealing with molten lead. Sisfile Hfire screens" of sheet iron cm pipe frames are used to shield the sen and the equipment during the collection of the sajples for the $ conversion test. See page 75 below. Mr. ffitrden reported, August 1950s "High temperatures are fairly general throughout the department particularly above th@ convertor. All floors are of the vertical strip lattice eonstruct ion to improve ventilation, and large portable WATER PCB-SD0000045440 Safety goaeiderations, eooM 20 Welfare, eoaM .- ^en-eoollng fans are used to blow through thee floors whenever a ms lma to work tpstairs. Hormlly all operations ar controlled fro the growl floor* all posaible controls and instruments being located there The writer regard* attention* to this detail a* agential If conscientious main tenance of equipment is to be obtained. * Hepalr and mintemae work cm the conversion unit at Aml*ton is mad more difficult by the radiation of heat fro the Bttrromdlng unit#* specially In the room which eontain* six wait. b lead traps* in particular* offer a big radiating surface. The diphenyl building* with good ventilators In the roof, is very high, and the open-work steel floors permit a strong qpdrst^gfit of fresh air to flow through the room fro the ground floor, which in every ease is eospletely open on the east side. When molten lead is being baled about on the operating floor, the ground floor below is roped off. See page 39 below. DSW 462075 WATER PCB-SD0000045441 c 21 BAWJ^ SSM FROM ASHISTOH TO BOHSAHTO CHEMICALS LIMITED The following sables were sent tnsm Anniston, Rovl3A7* g4070 gAoti aA0r2 @4073 0-4074 0-4075 Benzol - Orode diphenyl Finished diphenyl BMOtomx R'",;' . ' -- Still bottow from diphenyl itm Still bottoms from Saatow&x still (also 10 lb Montar Ho,9 requested June 22AS) but osly tfa first tiro reached Ruabon, so the last four were repeated J&snsstry 25A9# to London, (and were received there Feb.21/49). Tb foilicing saaples also were seat to M.C.L., on the dates stated? . <5te 22AB Saatowax H MovA9 Betszeae as used at Anniston. DSW 462076 WATER PCB-SD0000045442 c 0QHROSI0I 22 Beasene and Biphenyl under the working conditions ar not corrosive* but It Ma been found advisable to use stainless steel for the laad pots and connecting vapour pipes* Anniston InterIn report 2211. toted April 22/48, describes pot failures by '"mailing erosion* of th weld and the pot bottoms, failure of th welds* external erosion by lead* and by other suaes, and also recommend the us of 310 stainless welding reds..or of 309 rods with subsequent annealing of the pot at 2050%. Copy #11 of this report was sent to Hr* D, 8. fever- reft ia Lotsdeti* 1/48. . . See page 57 below for a discussion of the harmful effects which foreign element in tin* lead night Imre on the stainless steel of the pot. In tonuary 1949 it was reported, the Anniston experience up to that tote showed 309 type stainless =efceel to give better ser vice than 316 type. She Texas City Research Report Ho,52 "Special Report on Lead Pot Corrosion** S.FItxger&ld* Feb. 17/50* (copy seen at Annis ton* Hot,/*50)* deals with the corrosion or lead pots used to crack propane at 80OoC to ethylene (formerly for pyrolysis of ethylbenzene to styrene). It reviews the infonsation avail able up to April 1947 Thermowells had suffered badly* and the pot bodies became pitted around the level of the lead surface and became eroded where there was turbulence of the lead. laboratory te*ts showed that lead oxide was highly cor rosive to tb stainless steel used. Sasple of different stainless steels iraaersed in the lead pots gave inconoluslY results* but festelloy and fescroae appeared to have high resistance. Pure nickel* laonel* and nickelchrosii* alloys with 8o nickel dissolved in the lead in a few hour, W.ad@* Anniston* Apr,22/48* reported poor resistance with 68 nickel - 18 chroaiaa alloy, C&rburation of the metal was suspected* with the formation of brittle coating easily removed by the potrading action of the lead, A patent search revealed that the resistance of high chrome alloys ms known. The report @odad with a recowaendatlon to mm all the pot at a low rate to diminish turbulence rather than to m a few pots at high rate. It was reoowsnded too to put carbon in the pots at the outset* to reduce lead oxides* but this recosnentotion bm not been adopted at Anniston, DSW 462077 WATER PCB-SD0000045443 Qerroalon^, oatd LmA la town to neap so tias through the eorer Joints on the pots at Anniston, It y fora lead oxide outside the pot* aad this 1mA oxide n; f attack the outer surface of the pot# There is no point In trying to detect lead In the stack gases heearns there It always scne lead lying about in the furn&e#*. 23 DSW 462078 WATER PCB-SD0000045444 GASKETS Anniston report 1642, Oct.15/41, recommends Oarlock 721 gas kets for temperatures up to 500C, and Goetz corrugated steel-asbestos gaskets above 500C. For the cover of the second preheater a 5/l6n round soft copper gasket Is used with an asbestos gasket inside It. This double gasket originated at Texas City, but the asbestos ring there is outside the copper. For the cover of the convertor a gasket of 1" braided asbestos rope Is used, (see pages 42 & 87 beloer), but if the distortion of the flanges could be pre vented, the 5/16" copper gasket would be better. Copper and its alloys hive given poor service in the hydrogen system, apparently because of HoS. Copper gaskets in the compressors have completely failed, and Babbitt metal has been proposed. DSW 462079 WATER PCB-SD0000045445 L* t raw shect 25 The attached flow sheets of materials, pages 26 k 27, are taken froa Analton Research Department,. Report HO. 1642, October 15# 19*1. The seao report gives the following data,?- 0.1796 tF.S.Ctell benzene eonsiesod per 1 lb distilled diphenyl produced (eospare cost records given on page U8- below, @f the present report). The 8htrt-down time on the conversion systems averaged 1.6j over a period of 8 months. See also page 28. OS\N 462080 WATER PCB-SD0000045446 D i fa heny/ Process* f-7o-w SAeef 26 G, #6 Feed cut p,bo*^ Q di *& 3 o a 7~- 2YaC GP ' c J7 VoL - 11**60/ r ft 3 o ft Va.h orrz inq . t- 3 sec. o.Go ft/tF c 3 *0 a.v<) C t = 1HC(0 Qf. --H,7Sft/%K (p 3*0 ci* fst . Preheater r- 5tfo *Cl/ejd> t - ? -Sec. 3 g / /^ 1 <G/^ /a/f * JJr SSC' V op =- / # &/06 * 47^0 cT* 6/e ^ 7> # /Vo - # PA - > H 4V,o 5 /7 fir ^ fts ere C(, H t - OH k? 0 P~ 4trno t_6) 7 - 56" er & mses ' p 3oon/ n * Ccir\'i\r*ssin-7 x.-,6 I C rt\ cu.^/v 1 Cunc(?nS-Zr I 2rc* Pr*r, eater r- T/fj/ r- ? Sec - -jofiftF Cs. ft0 ~ (1 Y 17O 0 >/= - ?ZCX>Cf /y_B - //a * <7o// ?7 op ^cn^rfor 7 - S VC 7 /<v V " ** Sc1 7 ^ //) 3 Cc, Fk " W-c H _ r5 720 *c Z>P - Hu op ^ r- IF V '` oj- /^5 - s-v.ov toV -V-V'. e P:~ t i 11 Curb or) - ? H /G * 3-# Gu-bon t* ? # Pb - f# ' P- V"5' # /,/o 7- Co Pb ~ ?-?/ O 0 Z)P - r>>2-0 t/ //e -- *6-.0 t - 0-0 TV C U*t O ft' 'd/S ; . e if .. 1/c/ Car-Pen ' > ft TV Pb tf 3 - 3 *s DSW 462081 WATER PCB-SD0000045447 Flow SKe at -for hqooHmfl off ^agg-s ~i-o^ ^0 1 ^ln ^ 27 BqftK ^K'esswf'-/ Rogulotor v t H a_ ft A7 >r_ DSW 462082 WATER PCB-SD0000045448 COMPOSITIBM OF SOM UTERMEDXATS LIQTOH3 %% %* % < % % High % Benzene Toluene StynjM Biphenyl naphthalene Biphenyl benzene Tri ortho Boiling Unldentifiec o m P phonylane Mtls Jldf phenyl 4-8 20 adart >r rrene lotion 20: 0.5 20 35 1 Ly abo lit 220 1b of thi fraotion produe id in each o onver ;or pel year. 19 See also page 4 8,4 U6below. phenyl LH fctons m phenyl Lll fctOlU }kl 0.9 trao4 * 4.3 58!#** 2925* 7 1.1 5.4 - 6--10 53-68 15-30 1-3 2-4 a Soof these values will naturally vary a little, depending % on the exaot node of operating the plant units. MO0> CO CO croo WATER PCB-SD0000045449 PROCESS IN DETAIL Benzene Handling Benzene is received at the plant in tank cars and is unloaded "over the top" by pump to 5 large horizontal storage tanks (#1) situated some 300* from the diphenyl building. Water is used to prim the ptoqp, and of course it Bust be separated afterwards by draining from the store tanks,or from the recycle tank. From the Storage Tanks the benzene is puzped by (#2) to ($3) Recycle Feed Tank. Eero recycled mterlal is constantly Bade UP with fresh benzene. This is necessary in view of the fact that a catalyst, apparently present in the fresh benzene, is removed in one pass through the convertors. (Soe under "Comments on Process * pages HI & XL2 below). A float within the Recycle Feed Tank automatically operates the pifl^p, item #2. There are also two floats within the tank for high and low level alarm. There la a history of a little trouble due to the sticking of those various floats^ 3ee no tea on iters #3, page 84 below. The recycle feed tank now in use is a horizontal cylindrical vessel with bilged ends, and the benzene outlet line to the pumps, item #4, is taken from the bottom by a Jacketed line ( jacket, however, is not used), cemented through the containing wall which surrounds the tank. This take-off line rises a few inches inside the tank to trap any water and solid matter, and ths tank has a sump, with a drain valve for tapping off the water, etc. Regular and frequent operation of this valve is a very important part of the operation of the plant because a shot of water, placed through to the vapour iser, my flash off almost explosively, and Might break some Joint in tho pressure system. Water gets in from its use, in prising the overhead suction lines from tank cars, and may get in from perforation of the tubes of any of the condensers. The following streams of benzene enter the recycle feed tank; (1) A continuous stream of condensate from the convertor condensers, item #11, (2) An intermittent stream from the receivers, item #27, of the hydrogen cooling and compression system. This stream comes at s-.bout hourly intervals, under hand control of the puqp, item #28. (3) The benzene distillate from the benzene receiver, item #21, of the diphenyl still. This distillate comes for ward in batches at Anniston, via the pump, item #2la, but Hr. EUenburg's letter, J&n.20/48, indicated that a similar procedure at Newport might cause too great a DSW 462084 WATER PCB-SD0000045450 Process in Detail, ontd Hettfene teadling# eontd 30 variation In the ratio of fresh bmzem to recycled bonze* because the flow of fresh benaene would b vkt wish smaller at Hewport tMa at Aimiaston* but the diphenyl a till batches probably not much salw, BUeoburg suggests interposing a buffer tank between the receiver. item #21# and th recycle food tank# item #3* so that Urn stream of recycled mterial from #21 can be smoothed out. ' At Anniston* thm am rater wait* irntH the float alarm on item #3 is Vinglng oa lotf!r before puoplng in benzene fro the diphenyl distillation cm the hydrogen eo^jresslon* then he steps when the alar Vings on high19. There Is a ease cm, record la which the recycle feed tank was overplayed* and the excess benzene backed tp the distillate lias and Sato the converter reflux split boxes of the conver sion imits* apd escaped dowa. the coltms into the orude diphenyl tore tank. Shis errerptasking was detected by the fall in tem perature of the colum underflow stream. There are two (2-etag k>uld) (#4) centrifugal pts^)s for feed ing benzol at approximately 100# pressure from the recycle feed tank to the conversion tmits* and one or both my be in opera tion depending on the nuhbar of units oprating at the tine. There ii a Fisher strainer before the ptan>@* awl there are two filter pots* after the pt^ts# Sm the Cetxteol roes - only one In operation at a tin* to allot for cleaning. These two filter pots are vertical cylindrical vessels about 6s i.d. ty 9 deep with bolted-an. covers* fit of course for working presets*# arotssd 100 psig. They bm baskets inside to ^pporfc cotton fUtercloth* bat In Hovertter/50 the cloth bad rotted aad ted not been replaced. It is thought that glass doth night serve. There art lordstrow 3-way cocks on the inlet and outlet lines for easy switching of the pots* and there is a pressure gauge cm each lln@# to indicate the filter resistance. The min purpose of filtration is to protect the flow controllers. Solid natter carrying forward to the vapourixer would be sisply carried through in the vapour stream# and probably end in the lead trap or the carbon trap of the converter# It is said that a little dust (free the pots) cones forward In the recycled bensets # and there Is pipe scale from the benzene lines. DSW 462085 WATER PCB-SD0000045451 Prooeeg' In Detail e entd Benzene Handling, oafcd 31 Th filter pet* deliver to a header* serving a row of 13 Foxbore recording flan osstroHers* me for each unit* plus one spar#* the piping being so arranged that the spare controller em be switched in to replace acy of the others. These con trollers r@ in a special roc* which.is entered from outdoors sad which ban a eewmleatlng door to the min control room* otherwise It is completely shut off Area the rest of the plant. Apert fToa the benzene flow controllers this room contains only the Mters for the fuel gas to the furnaces, find a controller for water to the BS1 absorber for the Arocler plant). Mr. J. C. CXegora* the department Hunger, mentioned that Rota meters were formerly used* set In a glass box draining to out doors* to take away any benzene leakage. There was a certain advantage la having the visible flow, and he would like sight boxes (fit for 120 pslg) In the present flow lines. The benzene delivery lines fro the controllers are cemented through, the wall between this room and the convertor rooms, at about the level of the convertor pot lids, a separate line to each conversion unit. Each line dips to a stop valve within easy reach of the ground floor, inside the convertor room, and then rises to the top of the vapowlzer .uafc. Dasaedlately after the stop valve there is an inlet for COg fro a cylinder chained to a of the stanchions of the building. No provision is . ad@ for w&rssing the CO2 cylinders, though the ground floor, being completely open to the air cm one side* is not very warm. The aorml flow of benzene is lyo TOO per conversion unit per how. DSW 462086 WATER PCB-SD0000045452 Process In Detail, eoatd 32 Cooteraion There were 12 conversion, wilts, item #5, at Ajmisten in Soveiaber 1950* two of then (imit3 4 & 5) being somewhat different fnoa the rest in that they had a tubular preheater* then two lead pots* whereas the other ten units each had the preferred aoral arrangement of three lad pots and no tubular pro heater. (See page 85 below for the reasons for choosing the three pot arrangement). Each of the 10 normal units consists of a (#6a) Vapourizar* (#5&# 5B* & 50)* three lead pots la series, (called respectively 1st preheater* 2nd preheater*and convertor)* (#7)* lead trap* (#8) fractionating eoltam* with (#11) condenser and (#12) reflux split box. The underflow fro the column passes through item (#9;* carbon trap* and then by gravity through steamJacketed lines to the crude diphenyl receivers* item (#10). The vapouriser consist of a coil (formerly two colls in parallel) within a stack through which the exhaust gases fro the pot furnaces are passed countercurrent to the benzene flow. There is also (#6b) * another stack for the purpose of by-pass ing the furnace gases* if necessary* away from the vapourlzer coil. The temperature of the vapour leaving the vapouriiar is about 250C, but see below* pages 3334If the vapourlzer ha two coils in parallel* an attempt mist be Bade to share the flow between the by manipulation of the valves at the exits from the individual oils. See the notes below* under item #6A* page 91 * relating to the possible loss of benzene vapour by perforation of a vapourizer coil. Each conversion pot i of stainless steel about 22-3/4n I.D. by about 6'"0 deep, and eontains molten lead. The following figures are given for the depth of load in each pot* Depth of Lead; Anniston report 1642* Oct.15/41, 1st Preheater pot 2nd Preheater pot Convertor pot Height of Distributer inlet above botto* of pot given as 4'-0n 4'-0" 3'-6" 10B H.L.Barden, Aug/50. Xoonfiraed Nov/50) 2'"lw dry dip 2*-6" dry dip dry dip out of 5'"11-3/3* internal depth There is little antrainstant fro the first preheater to the second* and not such from the second preheater to the convertor* but considerable entrainment fro the convertor pot to the lead trap* so the depthof lead are liable to vary a little. If it is not desired to open a pot* the loss of lead may be made up with molten load poured in through the nock which carries the therm? well. DSW dGor\sr7 WATER PCB-SD0000045453 CONNECTION FROM VAPOURIZER TO FIRST LEAS POT Scale l!-Of All other piping omitted r ^/rwir- 33-jf DSW 462088 WATER PCB-SD0000045454 Process la Detail, eentd Conversion, coatd Each pot cover arri (1) a d3p pipe to carry the vapours dews into the molten lead, (2) a thenao well, and (3), a gas outlet. There are horizontal taffies or splash plates to diminish the entrainment of lead. The first and second pre heatera also hare a onaeetion to an equalising line with a stop Tin, These equalizing lines connect into the hottow of the convertor coltsms, Item #8, and are normlly closed. They provide a convenient location for pressure gauges (oa tranches below the stop valves), and could be used to by-pass a pot in eaergenoy, and they can be used to diminish the chance of forcing lead back vpotrmm during an Interruption of the benzene flow. The lead pots Mag, by their rims, in a row, each in a gasfired, fire-brick lined furnace, the first preheater being between the other two pots. Anniston report 1642 of Oct15/50 gives the following approxi mate figure# for1 temperatures in the conversion system: Thpourissr XKuBIeTooO. type) 1st Preheater Benzene in 25C Flue gas in 70OC . out 340C (137 reported AugA 7 out 190G . Combustion gases Lead temperature Vfcpour exit 650-700C 570-600oC (38oC,Aug/47) 550-580c 2nd Preheater Lead teEperature 720-740C Vhpour exit o50-o70c Convertor Lead tesp. controlled at 840 *5C. (but see "Coi^snts on Process",pages 111- below) Vhpour exit 710-720C. CelUM Top Bottom 60C - sometimes higher--up to 970 235-250C - normally about 200C 7b furnace casings had a temperature of about 100C as Judged by Mad, So?bsr 195C. OSW 462083 WATER PCB-SD0000045455 L Froomm to Detail, ooatd Peaversleo, ttd . 3* Jft\ Barden reported the following tefiperaturea la August 1950 s Ait Vo, VHjxsriiier Vo.l Preheat e2 Preheat averter Tep GeltM Flu gaa Inlet Flu @a Otttlat Benson now 6 7 a 9 10 11 12 -soo 320 18 150 ISO 300 35 48o 720 530 450 go 495 750 480 74o 560 740 570 740 745 85 775 800 820 790 90 83 as 80 85 90 All oouples C/3 1 -Sheaths burnt out 175 235 322 316 230 190 250 170 7,3,0, per hour H 310 540 zg 825 8 200 Earlier records or glv9& to a copy of the plant record sheet pag 51 below, Timrm is a Multipoint temperature recorder for each conversion wit and a recorder-controller for feh conversion pot teaperatur, A saaple strip f the Multipoint chart was sent to Kr,V.M.Cooper. 0et,3lA7. Tb pressure drop ttoougfc the double coil vapouriser, at 170 TOG be&adi/houQ was,. 8-10 pal* Pressure ot vp@w? entering 1st preheater Pressure of vap#w living 1st preheater Presage of vapms* leaving 2nd preheater Pressure at vapow leaving convertor 50-60 pslg 38-45 pslg 15-25 psig 4-7 psig 5b presages msy a little as th depth of lead elmngea by entrainment of lead fTm the pot, @M as carbon builds^* in the gas passage, The gauges mv@r a little because of the trabb Itog and fftfingiag of the load to the pots, Oartn baUds %q> arornd tho tefH.es aad to the pot <xit lines during operation,, causing a slew increase to back pressure, This increases th retention tin of the vapour to th system, sad causes th MUrcnitm reaction t oontlme a little heyoni th point thought best, so the operator lowers his pot tempera-, twes a little to compensate, See Effect of variables, page U4 below. Recently, the back pressure cm sow of the unit ha# been purposely increased by the insertion of orifice plates In th lines from th converters to th oolraans, to the top of WATER PCB-SD0000045456 Process in Detail f eoatd Conversion,, ceetd 35 attaining th sane degree of reaction with usefully lower pot te^erutures, so that th pot, would last longer. (The vapours those units as he heard roaring into th# lead trip). Thla is eaperlaantal, and e^perlonee is howing that th increased pressure on the convertor gasket m&j earn troubles which outweigh the possible advantages. Mr. Ellenburg's letter f D,l4A9 states that two orifice plates of stain! steel l/BH thick are used, one with a I.31 orifice between lead trap sad vapom* pip and the other with a 1.14" wlflce, betimess vapour pip and liras. This arrangeosat gives the required pressure drop without using too small an orifice. The pressure gauge on the vapour pipe thus reads the pressure between the two orifices. * Mr. ELleaburg gives the following eoaparlson of conditions with and without the orifice plates 1 Gauge Pressure Locatiea of pressure gaugt? lo.lO wait old conditions SO. 12 unit with orifice plates After #1 preheater After #2 preheater After Converter After 1st orifice plat After 2nd csrifie plat ( colon) 29 palg 18 -- 3 46 paig 33 21 13 3 Converter temperatures in th ^pressurised" pot were around 785-7900c for 17.5^ conversion. TO lower tac>eratur8 nay av a little fuel gas as well as lengthening the life of the pots, and in the early runs, the deposition of earbon in the gas passages appeared to have been greatly diminished. In Sovesfoer 1950 pressures 1 to 20 psig were ebs@pved after the first orifice plate. Th following operating conditions were reported In September 1947: Mi btmsem pui>s deliver at pressures of vp to 100 psig, and th benzene reaches the first lead pot at . about 50"60 psig (fan In pressure through th# con trol itt8trwettt), the second pot at about 38-45 P*lg, and th# third pot at about 15-25 psig, and leave th third pot at about 4-7 pig, the drop in pressure in each pot being d@ mlaly to the tydrostatic head of aoiwi lead,". n^\A/ /iconcH WATER PCB-SD0000045457 Process to Patau* eontd Conversion, onfcd Ratwral gas 1 nm&& to heat the convertor# and stills od ther is a separate gas aster for each unit. Thm wfcw# ar lastailed In the room Mentioned above* page 31* which also contains the bonsen# flow containers Shew is a atop cock cm th gas min iMadiateXy inside the room* with a long taadle by which, it could be operated tram outdoors. Tbs min than Ms a branch to each unit, each branch haring its own step valve, then a pressure reducer. The line then branches again* one branch serving the burners on tbs #1 preheater* under ptn*ely wntal control, and serving the pilot burners cm an the units* and the other branch serring the control valves for So,2 preheater and the converter. ^ee page 107 below). The flue gases from the #2 preheater and fros the coarertor go downwards to cross flues leading to the bottoa f the setting of #1 preheater* so that that unit gets a good deal of its heat fro the flue gases. The #1 preheater setting Ms gas burners of its own to supply any additional heat needed and for use in starting tf> from cold. The temperatures of the lead in the two preheater pots are e atrolled by hand operation of the gas mires* but there is a high temperature alarm which would cut off the gas on #2 if the te^>er&tur should run away, say, lay leakage of benzene vapour into the furnace. See also under instruasentation* page 107 below. Typical operation records are given on page 5L below. 36 OSw 462092 WATER PCB-SD0000045458 Process in Betall a eontd 37 goto on Starting a Ooaversloa tfalt 8te* H. L. Itrden, August 1950, reported & follows: l'Tb start-*5> was witnessed of a diphenyl wait from cold; after leaning and minor repair. Tha following instructions apply to an Aanistcs unit using natural gas. Other fuels nay necessitate slight modifications. Put m cue burner of each vsilt. Throttle hack until war enough to keep alight. The us# of the pilot light will assist in keeping the burners alight. Flu gas is to go up the by pass stack to &Yeid burningnop the raporisr coil. All vents cm the convertor should be open in the early stages of warming Txpe As the setting warss u& the other burners are lit one by cm, till all are alight and burning steadily. Burners are ad justed (by hand or automtieally by controller) to obtain the desired tmg>emtures. Only the convertor teaserstore appears eritioal. Whoa fce^eraturos are approxiaately correct, start COg through vaporiser, the preheat vessels and convertor to the Colusa and out by the ooXtasn vent. Divert flue gas from by-pass to vapouriaer to warm up the latter, and close rents on the preheater. Pressure on the preheaters should then build np and enable leaks to be discovered, Development of ,20 psig c Ho.l and . 10 psig on Ho.2 takes about - bottle of COg and it Is assumed that the pressure build-up is a sufficient guarantee that the air has been adequately purged, There should of course b@ no pressure to speak of in the convertor if the coltm is properly vented, Then, provided teaperatures (inclu ding vaporiser) ay# about right, cut off OO^ cut in benzol feed at a low rat {S TOG per hour). As soon as the lead - trap begins to mbk, indicating that benzol feed Ms reached it, close the eoltm vent, put water mi the condenser and opssi valve to reflux split box, benzol run-back and biphenyl line to rude tank. The latter line mist be hot before start ing until sufficient feed of crude diphenyl is available to prevent ih line from Baking "Cautiously increase the benzene feed by approximately 10 TOO per hem* every half-hour or so. Tim governing factors in effect ing this Increase are Maintenance of preheat temperature (which tends to fall a the benzene feed increases) and the avoidance of high convertor temperatures "The preheater Bust on no account b aUotred to cool to anything approaching the welting point of the load. Bsxlm* temperature of the converter should be 830-8^OG (8000 if operating trader pressure). The beazea feed should also be checked frequently until confidence is established because any mechanical cr electrical failure here will cause a suck back of lead into the vaporise oil, ns\N 462093 WATER PCB-SD0000045459 Process la Detail, oontd. 38 ypta cm Stopping a Conyers ion tfait It Is of course iaportant to prevent Ingress of air to the imlti and to take are that the lead Is not f arced 'backwards through, the aystea by allowing the pressure to fall at the inlet md of the system, When the gas burners bars been cut off, the .benzene feed is stopped/ and CO2 is forced into the betusene inlet line to the rapourlxer until liquid ceases to condense in the eonrertor condenser. A full bottle (about 56 lb) of CO2 is used. ZXff*sg this period the uncondensed gas atreas* consisting of hydrogen and some COg, will hair been going forward to the hydrogen ecwpressioa system* to prerent the loss of its content of beasene* and the OOg-hydroges nixture my be rented to waste after e ogress ion. and cooling. When the distillation ceases t the system is closed off from the hydrogen collecting header * and. fro the crude diphenyl tank/ and the rua-bsek line to the benzene recycle feed tank* and rented through the pipe which passes fro the top of the reflux iplit box to a point above the roof. The conversion unit my then be opened up for inspection and repair. DSW 462094 WATER PCB-SD0000045460 PT&cman la DataH, eontd 39 yofca on B^>tying a Lead Pot Wm. a pot has to ho eaptied, the usual shut-down routla# Is applied, toe systoa allowed to cool a little, the pip Joint* arid cover Joint broken, the space en to ground floor below roped off for safety, then to cover, with its dip-pip and . fchwao w@U hoisted out her aeass of a stlm^ bolted to to central flange. The lead in the pot is, of eours, still oltn, and a little drips off to dip-pipe, Th cover is laid oa to floor in a convenient place. The surfae of the lead in the pot is usually covered with floating solid debris, and this is dredged out by means of the long-handled perforated ladle (see sketch #1) and knocked out in the well of to box fr&a on to furaa.ee cover. It is convenient to remove th , lead trap, to mke room to work, and in most eases the trap WlU contain load which has to be molted out as described later, page 92 and will contain solid carbon, iron oxide, etc. Th lead molds are mde of eh&tmel iron, about 2" deep overall aad up to 36" long, 6W wide, with sloping ends welded in. Tea of toes molds are then placed, five on each side, near the top of the pot, and two coloured men take turns to dip out th molten lead by means of th unperforated ladles, (see sketch 2) and pour it carefully into each mold in turn until all ar full. This is rather hot work, especially in Suisser, and th ladles of lead ar rather heavy, tot the Job is not too bad. Th operator uses the edge of the pot as a fulcrum to lift th ladle, and step backwards a little, dragging th Ml upwards until he oaa get a sufficient purchase on th handle to lift the ladl over to the row of molds. H wears a face mask, and leather gloves, but no other protective clothing. Th lead nay spit a little if there is soistur in to molds, and casual passers-by have to take oars not to step into to acids, Th ladl handle is occasionally wiped with a wet rag to cool it. When ten molds ar full, to two am take a breather for about 15 minutes until to lead 3ms frozen ever (tested by poking with a rod), tom to molds ar dragged a few yards away, and inverted to <5mi> th ingots, Double handled tongs are used. Th mold* ar to@n refilled in exactly the same way, and so cm until th pot i practically eaf>ty, about 60 ingots in all. Th pot is tom hoisted out of tot setting by Beans of a sling chain, bolted to th o^>anion flange, car being taken that th bolt holding to halves! of th flaag are still ffestiva, and th pot is run along until it ossos over th hinged part of th floor, so that it can bo lowered to to ground floor, Cpr is taken to close to hinged part issaodlately the op@ra.tlcm is @nd#d. DSW 462095 WATER PCB-SD0000045461 c Handles of 1" piping 6 6~ " 3A6k arfcal* holes Sketch Hod DSW 462096 Sketch Ho. 2 WATER PCB-SD0000045462 c Process in Detail* eoatd *0 got# cm Bi#tying a Lead Pot* cmM 8@t*e8 pot la ttorod with the load still in it, for exug>le* If the distributor assembly will not break loose because f earbs tnerwst&ticfi* or If a sotmd pot is to be ot4 from, om setting to another* but such eases are quite rare# The lead would be allowed to solidify before the pot was wndi The usual procedure Is to bale out the lead as described above. The lead ingots usually leaT the wide quite easily* and they are atasked nmx> the mit until the new pot J In place* Uutt they are packed* cm end* in the pot* and salted down# and any lead needed for aakenup is added#' Tbe.eorer with the dip pipe and thermo well can* of course* b@ lowered into position only while the 1mA is nolton. DSW 462097 WATER PCB-SD0000045463 c Process la Detail, contd *1- Sot on tb IfalnteBaaee of th Lead Pots (See alio the notes on its* #5# pages ' below) * 121 Tbs practise sheets, pages 12Q, tofoelow, glv aoa figures for tb frequency of repair* Th first preheater with it welded-oa sorer, lew vapetsr veloities M relatively low temperature an no for years without attention. The second preheater, and more partieulsrly, the oarertor, suffer fro deposition of carbon la fcb vapour passages of the over, damage to the dip pipe, thermowell, and baffles hr high temperature and by the mechanical and possibly corrosive effect of the lead, failure of the pot nil, usually by corrosion-erosion from inside, at or below th level of th lead, era eking of the weld between the pot and its rim (this weld carries the weight of the pot and contents and there is oatlnued gentle bussing of th lead, and vibration of the pot), failure of the eover gasket or warping of the over flanges, and from entp&lnnsnt of lead in the vapour stream, If lead nag in eosstact with the outside of the pot, fros a gasket leak or from a perforation of the pot wall, it my cause marked erosion, apparently from the solvent effect of lead oxide on the stainless steel, but this is not a tmjor cause of failure. If there is a partial blockage in the vapour outlet, it my show tg as a darker patch on th glowing pipe. Th pip leav ing th convertor needs cleaning about each 3 weeks and that from the second preheater about once every 8 weeks, Carbon ay also build up inside the eover, round the vapour exit, or in th orifices of tbs baffle plates around the distributor, Th baffle plates slowly sag, apparently purely from high te^eratra*. A eoirrertor pot usually rtms 5 to 9 weeks before needing overhaul. . Th carbon my be burnt out of a pipe by beating with an xy- acetylea torch, then taming off th acetylene, but are must be taken not to overheat the metal when the carbon bums in th oxygen stream, and th welder should take are not to breath too mah of the vapow. There has been sew discussion of possible overheating of the pot walls abov th level of th lead, but apparently the splash ing of the load, cm to the mils does a little cooling, and of oourse th furnace draught is downwards in the cases of the imoM preheater and the ecrertor, Mr. Barden, August 1950, suggested to Anniston that a stream of 02* passed through the hot convertor, might remove th carbon deposit by converting it to carbon monoxide. Anniston have DSW 462098 WATER PCB-SD0000045464 Prologs la Detail, eontd Not on the Maintenance of the Lead Pots, eontd 42 ad a few trial of this, 'kj passing two cylinders full of C0 through a unit one a week, and though th tmit finally choked with carbon, it waa believed that th choking ted been delayed by tha us of OO2. Although th pressure Inside the eonvertor is relatively. low, tha joint of th trrarter over gives a great deal of trouble, beeause the temperature is near the yield point of the natal,, Th edges of th over gradually bend downwards and the edge of th eoafxtnicm (backing) flange under the pot lid bend upwards irntH they met, and th gasket no longer holds. The gaskets on the convertors are mde Up from round braided asbes tos rope 1" in diameter, See page 87 below. Leakage of lead fro a defective pot will probably be detected first a a drip of lead from the furnace casing, (Note that it my drip from the wrong casing by penetration through cracks in the furnace setting, and care should be taken to examine the undersides of all three pots before deciding which actually is leaking). The pressure gauges on the pots may help to indi cate which pot is losing its lead. Leakage of vapour into the furnaces may show up as black smoke in the stack, or as an increase in furnace teeperature. See also the stack test dis cussed under item #6a, page 91 below. If a pot is sound in some parts and defective in others, it my be Bade good by welding, for example, a new bottom y be welded in.' A pot which has seen service in the #3 position my be shifted to th lighter duty of #2. position and so on. See notes under ^Corrosion*, page 22 above, for an accotmt of th corrosion of th pots. DSW 462099 WATER PCB-SD0000045465 Process in Dotall,, eontd *3' . Til Mixture or vapours and hydrogen leaving the convertor pet passes through the centrifugal lead trap, ifcea #7. where Host f the entrained lead separates, and Into the bottom of the fractionating eolum, item #8. The tmderflotf of the eolusrn leave* via (#9) a cartwo trap, through steam Jacketed lines to one of (#10) two snap tanks. These tanks are vented to the "off-g&a" Use fro* the to|) of the celums. At the top of the coIumi there is a (#11) Condenser and (#12) refit split box, with an equalising vapour line batween the two. The reflux split box is adjusted to give a benzene forward flow containing at the Host a few parts percent of diphenyl, and to give an underflow of crude diphenyl containing as low a ben- sene content as can be attained. The Anniston report 1642, Oct.lsAl, states that the crude diphenyl flow contains about 4 to 8^ of benzene. Diphenyl still records seen in Kovesber 1950 Indicated, that about 17$ of the crude diphenyl was recover ed as benzene fraction. See page 53 below. Mr, A. K, Ellenburg, Hot, 12/47. wrotes " The reflux flow Is used to control the temperature of the underflow from the oolum at about 200C. The reflux ratio varies according to the temperature of the condensed benzene. --.---------(which) varies according to the length of time the condenser has been in service. As the film builds up on the water side of the eondenser, the cooling efficiency drops off, and sore of th hot reflux must be used to obtain, the sane amount of cooling. These ratios vary from 70/30 to 90A0---------- The vapour line from the convertor to the bottom of the Colton has a branch for sampling the vapours for the purpose of mking the ewersion test, (& below under "Conversion Test", page 75,)and another branch carrying a pressure gauge, Thm conversion test is performed once a day on eaoh unit, usually ia the morning shift. DSW 462100 WATER PCB-SD0000045466 Process la Detail, eontd 44 Treatment of Off-gas Th off-gas fro*. the eonvertar eolums, eons1bts of hydrogen, saturated with bnsoa@, and It goes via (#25), a fian@4 oolr with water Jacket, to (#26) a swg tank, fro which it goal to either of two coMpressors (#29) . Tbs scares sore work la two stages, 60 p&% and 300 psdg., and th expressed ga from th first stag goes downwards through, a vertical interstage cooler (#30; to a low pressure tank (#31) wfaer condensed bensea is deposited, theft the hydro gen goes a to the second stag of ospresaioa. After th second stag the gas goes downwards through th second cooler (#32) into the high pressure tank (#33 % where it deposit* ware bmmemjc Th surge tank (#26) has a 55 water seal to & hooded vent pip through the roof of the eoepressor room, and there is aa auto matic control tostznaaaat which, mintains th pressra* in the urge task between 11 aad 16 os per aq.ia, above atmospheric, by reacting oa th ualoadlag valves of tha eonpressors. Th bens:oe which collects in the surge tank gravitates to the bcasene receivers (#27) and that which collected in the pres sine wi formerly discharged by float traps, also into (#27)# hut tha trap seating failed by corrosion, see page 1 03 below, aad the trasfrrene is now done at about hourly intervals by means of band-operated valves. The pressure vessels have gauge glasses, and th discharge lines hav sight glasses. Corrosion f copper and alloys in tha hydrogen compression system is rather marked and i attributed to the effect of BgS. See page 101 below. Oxygen dttendnhtiena were mde on tbs hydrogen at first, but ar so laager thought necessary. After assy shut-down, the hyth^egea is vented to ate)sphere and the systets purged with 40 eu.ft, of OOj0' At Plant "H" ther is a hot wire combustible gas recorder per manently installed in the hydrogen strea* going from th chlorine Us to compressors fer the hydrogenation plant, wired up to stop thi on>rssor* if war than. a trace of oxygen is present in th hydrogen stress, Hr. EUeaburg, Jim 30/43, wrote* DSW462ioi * -----A yon kamf, ow Worthingtcm o^r@er has two stage* and operates at 150 psig sad 300 pslg at th dis charge of th low and high stage respectively. These presstsres are not critical and tha choice of pressures depends taxm the sis of the cylinder hanbof as well as the amount of gas to be toadied-------", See under it* #29 below (page 101) for his fwibar retries, WATER PCB-SD0000045467 Process in Detail, eooM 45 Diphenyl Distillation Cmd diphenyl is pushed through steam traced lines fro the stag) teak* to either of two horizontal diphenyl batch stills (#13). Each still is fitted with (#133), an external gam- heated coil, on. the side of a fir* mil remote fron the till, through which the ebarg* is circulated by assaaa of (#12A), a submerged centrifugal The spread" or te*~ peratur difference between inlet and outlet of the coil I automtieally ccm.troiled through the gag supply to the burners, and is automatically recorded. The controller is set for a spread of 20C, but when seen In Efeventber 1950 It was running at about 16 to 18 spread, i,@. the heat input of the btsmers ms falling short; of the control limit. See tinder "instrumen tation", page 108 below, for details of the control Instamssanis. 1 typical still charge (Sept/47) ms 34-00 0S0 crude diphenyl pita 450 tSO reeylea "heads & tails" fraction, and the still cycle took about 18 hours. The vapours pass to (#14) a 20 plat eoltam with (#15) conden ser, aisS (#16) reflux box working at atmospheric pressure. Cuts are taken based os F.P. determination, (but set Me, Barden's caveats below). The reflux is changed during toe distillation and the follow ing is typical of operation (in SepteBber/47) : At Start Benzene Fraction (tp to 80 C at top of eoltam) Beads Fraction Diphenyl Fraction Tails Fraction .Reflux / Product 100 0 25 75 50 50 30 20 Mr. Barden, August 1950, however, reported! "The total reflux period seeas to be practically, confined to the still charging operation. The still and eolum are usually still hot from the preceding batch and toe iaconing charge starts distilling immediately. Total reflux operation at this stage rapidly cools the eolum. It an happen that this initial distillation 1 too rapid for toe split box to deal with it. In such a. case it Is anal to relieve the box by sending a portion to the heads and tails receiver for return to the still. It is essential to avoid sending any of this initial ds~ fciHat to the bens to recovery system sine it is liable tp be contaminated with diphenyl and so lead to axe*# production of high boilers. The charge used at toe time of the visit was 38OO B5Q of crude diphenyl and heads end WATER PCB-SD0000045468 Process in Petall* eontd Diphenyl Mstlllatlonj o-cratd k6 "tails from, prwious run (about 4*200 USQ total) *Sa %xmm pressure la apt te<ferelep at start of distillation* presumably by plugging of eoadenar by condensate If this Is bserred* a rent Is available for tenperery relief Chi pressis* buildwas not apparent to th* wlter bat the operator elaised that fee could tell by the flew In the split box "Gireulatiofi through the oil is started before light ing burners As the syctea Is usually hot* the burner mn b put full m quite widely The btmmrv are oatrolled by th "spread* between Inlet sad outlet te^mraturea This is aormlly set to 20C* but is re duced to 10-15C when distilling heads to siMats carry over of good diphenyl ' "Officially* th change-over froa heads to good diphenyl should be based cm Cr.Pt. (68.4C)* In practice It is tsssal to change-over arbitrarily after one hour8# dis tillation because the tiae spent in testing staples mans unnecessary direr ion of product to heads for redistillation. The arbitrary tine factor obrlously depends on distillation rate and my not apply mx another installation. "SiMil&rly. th tail fraction Is cut out as soon as tem peratur (#e gpecinan chart) indicates need* as delay la f.p. determination* results la contamination of good diphenyl Pwttero, it has been found that fpt. can be 0E* but boSling rang out of specification If the cutting out of tails Is delayed General rules i- - - Wm top of ooluaa tn?emtur@ to cut into heads. PSe tiie sod coll Inlet temperature to out Into diphenyl. 13k eoH Inlet fcf>emture (345-355) to cut into tails ttoe top of eolum te*>mtup@ to out off tails " Che fere m Is benren* which is mm off to (#21) a tuoall buffer tank (situated near the stap tanks)* tram which It Is periodi cally pwm>ed tefhe resole feed tank ' DSW 462103 WATER PCB-SD0000045469 Prop la Beta12 ,, emtd 47 filphagyl Dlatlllatloa, eooM E&ch a till ha# three other receiverst (#18) Emda and TaHa^ which are pushed b&ck into the still, by mesas of a aubtaorged pump, for the next batch. (#19) Bipbeayl Hecelver. Proa her the finished produet my be pu^#4 tty mmns of a mlwrged ptmp to storage tanks, to the Arcelor plant, to teak ears, or to a small flaker (#20) Bottom, Beceiver, Crude Santowax is pu^>ed her at the rad of txm distillation, using the aubeerged puap of the stiU This mtari&l my b pts^ed to the Santemx still r 4mm off into drum for permanent storage * Excess aatari&l my bo pushed into a prad. The distillate flows through (#17) small open box fro which it my bo saapled and diverted to either the diphenyl or the "Hoads and Tails" receiver. The benzene fore running by-pass this box. Each of the# three receiver is fitted with a sterna oil and submerged ptnp, A typical operating record is given on page52 below, and a uemry of records on page 53 This record includes figures for the reflux ratios used. A saapie chart from the Multipoint tesperatup recorder ms sent to Mr. If, K Cooper, is London, Oct,31/^7* Anniston recycle the cooling water in their cendensersat atmos pheric PM88W0, ling it in a s^arate heat exchanger. This i# to prevent sealing; of the condenser by iapurities from the pond water. They rely ai^ly on hand control of the cooling water to the heat exchanger to give sufficient condensation without causing freezing of diphenyl in the condenser. The twparatur of th recycled water need not ordinarily be above the freezing point of diphenyl, but it is allowed to rise to 80"85C the collection of the "tails" fraction. Instru mented control of the ling water ms abandoned in favor of toad control, Tim benzene distillate is examined before being punped to the recycle feed tank, to make sure it does sot contain soar than 2-3J5 at most of diphenyl. The operators Judge by a greenish colour which appears if there is much diphenyl, and by evapora ting a few drops between the fingers, but a freezing point test would be the safer criterion. The diphenyl may mv@ flashed over at the start f th* (Sihtillation, a described cm page j above, or ay have com over through inefficient fraties (Insuffleifsfst reflux). DSW 462104 WATER PCB-SD0000045470 Process la Detail, eontd 48 Biphenyl Distillation. cart, A Km build in th heads fraction, of mtert&Xa other than benzene and diphenyl is very slow (only about 0*065$ on the dipbanyl according to Amis ton report 1642^ but as th frac tion is recycled to one batch after another, styrene and other contaminants do slowly aemaulat la It, (see tmder Sheet", page 28 above, for typical valuesj see also page iifi below), and the .out between benzene and diphenyl becomes less sharp* Occasionally therefor a heads fraction ct*ter from about 900 to 200G,aiaaimtlng to about 10 gallon, is side-tracked, allowed to cool to deposit diphenyl, which Is drained off and returned to the system, and the liquid con taminants discarded. Mr. EUehburg, 3&n.14/49, la answer to a suggestion from London, agreed that the heads fraction might be acounulated until there was enough to charge a still. Instead of being recycled each time, but he advised against that course on the grounds that a larger store tank would be needed, and that the Anniston method is general^ more conveni ent. Any is^uritlas boiling |ust above diphenyl will go into the tails fraction, but tais fraction is sisply recycled so that th impurities finally go out in the rude Saatowas. Hr. SHenburg advises against handling or shipping diphenyl in drums because of th difficulty of re-melting* Anniston flake any diphenyl not handled in tank cars or by pipe line* London, Feb/49, did not expect to sell any diphenyl. The dlphetsyl still bottoms (Crude Santowax) are kept molten in steam-heated feassks if they are to be processed further. Th excess production of bottom at Anniston is put into old drum, and acre of it has been ptapped away into an excavation* If th stored Material is needed again, it la put into a melting pot and them sieved by pulping. At on t when smaller (direct fired) stills were used, Anniston purged the diphenyl still system with C0g between batches, but discontinued this as being tsmeoessary with th pres eat stills. Th still is singly allowed to cool a little after being discharged, then a little care takes in pumping in the new (hot) charge of crude diphes^l. Still bottoms, discharged at about 400C have been known to take fire. Th* circulation, through the teatine oil is not started until the still has settled down after th charging. DSVV 462105 WATER PCB-SD0000045471 Process la Detail, oatd 49 Dltilia11cm of Santewax fhJj Is carried out tmder about 50 bh of ^ absolute prasine . at th receiver, wing * WTism Y&ewm (#40) Tha> pre- @at oqulpwQt ms originally- sat up for the separation of erode Saatowax Into Santomx 0, M and P, which are rude ortho, atta, and para lsBa of terpbwsyl, For Santowx R only straight error distillation is required, with a single receiver (#39) Instead of the series of receiver installed in the present plant. The still ebarge 1 received at about 150C in on of two Charging Tanks (#35A and #35B). These ar@ Interconnected at a low level and really ecwstitate one vessel, They contain bating colls and one has a submerged ptsfl? (#3to), by which liquor is circulated through (#3to) an external preheater oil on the side of a firewall remote from the tanks and still. The oil is heated by gas burners and is sv^jpprted in a steel flu with firebriok lining. The material is pre heated to 230G. The Bmm pimp is used to transfer the hot liquor to the (#35) still which las a similar heating arrangeMat. The still capacity is 6-7000# of crude. The still has 10* vapour outlet (ami explosion disc) to (#36), 12 piste column This column, has (#37), a condenser consisting of a -single Jacketed tube in the fora of a sig-zag. (See page 104 & 105 below). This condenser ms used in place of the original shell and tube condenser because the latter often became blocked with frozen material. There is a reflux split box (#38), but reflux is used only in the (rough) separation of erode Saatowax into the , & p isomers. The Saatowax S distillate Is m from the receiver , to th buffer vessel (#39B) and pumped from, there, fey (#39A) to th Aroclor plant, the Saatowax R flaker, or to the BB-40 plant, as required. Th still bottom are sold as Mont&r 9, any excess production being dioc>d . a*. Bardy reported, Oct.Tf/hjt bA totel forward flow is maintained on the split flow box throughout th Santomx R distillation. This is nece ssary in order to get over sob of th higher boiling constituents which boil above th terphenyls. These m terlaIs mast be pro8 at to bring the hold point of the Santomx within our specifications *0ur original Saatomx still had no reflux at all and th new still (1943) I supposed to duplicate th product of tbs old still*9. DSW 462106 WATER PCB-SD0000045472 Process is Detail, coatd Pietmatlorn of Santcnmx, ccatd 50 . Distilled S&atom Is a reddish brown liquid eryat&lllsIng to * yellow solid at room te^ratwes * Rts distillation la controlled V "Hold point d&teraiaaticas -- there ar two such point aM th speeifioatlcm for the pro duct r^quirtgi Tapper hold point 137-l43C (changed Sept.23AT to 137-1*5C) Lower hold point 45-6oG (changed Sept*23A7 to 45-63C) A &n>l strip of takerstur mortar chart for various points oo tb S&atowax till system was sent to Mr* Cooper* Get*31/^7, Qa fcamry 6/^9* Ms*. A* M* ELleritmrg wrote? "At m t@* distilled Saatowax was allowed to solidify in dnsas, asd shipped* but It was noticed that the pro duct tended to segregate a It solidified* As a result, the outer layer f the drums contained tb high Belt ing portion of the Santowax R, and the center of the drtm was. wade of the lower Belting fractions* "in order to obtain & tmifom product, so that a whole drt wtmM not hare to be melted to get out 10 pound, the Idea of flaking the Sflntowax was proposed* A chill wheel 1 used to cool the material, and a blade serapes the tsrial off the rolls* frost which it falls into bags or Used barrels* (lot, however* that Santowsx las two "hold points In its crystallisation curve, see page 13 abort* and gives first a plastic mss at about l40C, then a waxy solid at about 500* a fact which affects the flaking process* EM) * The Itg>y js&terial results because the Santowax Is not chilled sufficiently before placing In tb ba@, and a slight fusion of the flakes results* However* the partial chilling la enough to give a tsalfora solid product* The crude Santow&x could be handled, a siMlar way If necessary, because Its characteristics are similar to thos f Santowax R. A Mg tank for storage of the molten crude 1* of cours, the easiest solution to a storage problem* Amistcm, pointed out that tie Santowax flaking could t d< ou the mma dm as the diphenyl flaking* See also the note tasder Specifications Ifc Test Methods, page 67 below* ' ,,c\M 46tf 07 WATER PCB-SD0000045473 Mowamto Chemical Company A, PLANT BEGINNING 7:00 A. M. 1X UtB I U* Diphenyl Operating Record /- i v r No. 1 SHIFT eouNo* ooo?K corM* ` iK It 9 n J'j'.c ? *4 ^ j 7^ 2V0 16 . V'i ^ l~As> Jl'Q '* v' y' Uk'-yd^Zj ' 'll ^ ^ SjlXojl. v- jS er P f'' R-t ^ P"( ig^f f_S jc iU -- ^ 77? V/4 ,y * f0_XL&O_ ** Jilt' -- r in' r: / * ,7 > rv 7*7.51n I: t\ ]) , . "'Ll /. A[-: :-\'Y '*/ 3#/*# fi: '~ . /: ; ? /. / '.iXf. LJi. No. 2 SHIFT ' iJ/r ^ T IV - ; /6 Lj : v ,y _ / . a,-'-5'" | 32# I ^ '5 7 22 ??> ^ IvJ-j y / 4 / '/ / T UNIT NO. CHIEF OPERATOR ota c lv, ,>/ < * CCmvSfrfr'OH OAJtfVB V : 1>y` f #a--)=z \J~2JL jEjll. JfZZ. _Z2!_ s:uxc chief or j7u |2 6 i 4/" \>-Tery:0-A'- ' / i'/,v. r /.'T _____ _ '^<r. __ ^ ., ^ 1*1 8111 ir. r ' i" -------- No. 3 SHIFT-* 0&9Q\<?O !"// i./ 7.1B/ fc7;^}l>W|2i MPj "i r r ! ' i' * * i * \^i I n \9-ni2y ;>yjlp5\ CHIEF OPERATOR |27i27p7'p7,, / " \0y P.7.p7uns'..i' ! ? 1" i 'i n 2 71,2.7 WATER PCB-SD0000045474 Ptphonjl Plgtill1stIon Record Dirtllliation Ho. Still Ho. 7 !? .5 'Data Started _ / Operator Start -^4 Operator Finish Starts* Charging Still at -/J //: __ 194 ^ _ehirt 3 JL_Shi ft CHARCS: B&T Tank; inched before '/ 7 inchse after gallons ohargid 7 77 Ho. 1 S.T. inches he fora Ho. 2 S.TT i*ohas?befcre No. 3 S.T. inches before f) inches after inches kfter inches after j2_ /( gallons chargel-? gallons chargel grulone chm-fo-l f _l_ No. U S.T. inches before Benzol Still " n Inches after inches after lono cha~r?'\ gall one chavgal ! Total Gallons Charged _ +0 ka Circulating at /?:' Tire on at /2~: 7 ju. AT. ' _ ............. eticij jDl\ U-TTTNGS: 1. On // r at - ^ Ji Y) 5. on 3y. at 7- -Tf ' ? 2 On ' f 5. On S' C h. On. ? 0 at /St at O ; //' 6l On 7. On 8. On at at at BENZOL: HEADS: Fan 2Z- Start#, carer at Esn /?' " or tf or gal. /mT' lb.. TAILS: Started orer ^ !?i . , Flnlahed at - /.* .1 7> Ran _ 10__________" or _____ 7___________lbs. DCHEHTL: Total in Distilliatlan HICHBOH*: Groat 'Weight Mfr Weight y//- lb. So. of Brusa lb. " of. lbs. DSW 462109 WATER PCB-SD0000045475 c Ptocobs In Detail, centd. Sumary of fieoorda of Diphenyl Still Working 53 (Taken November 1950 from the plant sheets as on the preceding page) sew Material to Still U.SeOalloo 3485 3394 3394 3485 3869 3394 3485 3485 3576 3485 3485 Benzene Fraction off U.S.G. 437 598 667 506 690 690 874 598 391 598 598 Heads tknr~ Biphenyl lb lb lb (8 itAbo) 2024 1928 964 1157 18,785 17,459 2121 1157 15,470 2217 1446 17,680 121 1157 17,238 2217 1253 17,017 2121 1350 16,133 2024 2314 2314 1253 1157 1060 16,796 15,249 19,448 2410 1350 18,785 Bottoms lb 4400 54oo 4400 5000 4600 4600 -- -- -- 4800 4200 DSW 462110 WATER PCB-SD0000045476 SPECIFICAflO Am TEST MEH30EB 54 Haw Materials Benzene la September 1947 Anniston war In a favourable position in respect of the qmlity of tbs benzene received. By a special arrangement with the s^pliers la Birmingham, Alabama, they received material usually running 5*39&0 Gr.Pt., (on the sa^l Kas i*8), and at least up to "nitration Co-ade" on all other points except possibly sulphur content. She arrangement was so good that Anniston were able to rely alaoet entirely on Birmingham control of the quality of the deliveries. The only specification ms that lulled in the description of the aat rial as "Industrial. Grade Benzene ", and the deliveries were so much above specification that the specification was inopera tive. Because of this position Anniston do not perform routine testa chi benzene deliveries made to the diphenyl plant. There are only very few test reports on file, but the following which were avaiXaBle were believed to be representative of the mate rial usually received5 Task # QATX a Ml Date Pr.Pt.^C. Sp.Or. 60P. Diet, rang 1st drop 79.7 80.2 50g 80.3 95* 80.4 dry 80.4 Colour Water whit Wash test #1 Total sulphur ^ 0.05 Acidity mg M&OH/g BgO p.p.k. Paraffins akTX 21357 80.5 80.5 w.w. #1 0.05 ? GATX 19403 Aug^rr June 0,8825 0.90c 79.5 80.2 80.4 80.4 80.4 0.r 1. C (oorr.) 79.4 80.1 80.3 80.4 80.4 v.w* #1 0.0004 700 nil The freezing point method used was that of J.I.B.Ch.Tol.lO, p.1010, (see page 56 below). For the other tests, the latest A.S.T.M. methods were used. In order to check the Anniston method of determination of the freezing point of benzene, against the Buabon method, and to mks sure that the Anniston imterlal really had such a high test, by British test methods, a saeple from rail tank GATX 21357.* NovAl, ms gent to Ruabon. It was found to have a crystallizing point of 5.4 c by the standard Rmbon method. DSW 462111 WATER PCB-SD0000045477 Specifications & Test Methods* eontd 55 Saaplea* representing mterl&l available in Britain* have ' been exaainsd at Anniston: Fr.Pt.C Sp.Qr,50F Blit, range 1st drop 5 5 95^ dry Dolour Wash test Acidity mg BaOB/g HpO p.p.m. Paraffins SanpXe 2CB279 Taken A .24A 5*16 0,886 79.69c 80,2 80.3 80,4 80,6 v.w. #9 0,0016 458 Saaplo 60768 Taken. Ally 27/48 0. 1.2 71.4 80,2 80.2 80,3 80,6 v.v. #4 i.oo4 (earr.) Asmiston's eamaants on the British sasg>le HB279 were that it ms not UP to the quality of the Ami*ton supply*, it bad a high acid wash eelour*indicating lnoca^lete aeid treatment, and the presence of uaa&fctirated or hydroxy oosg>ounds* hut that it should give good diphenyl if the fraetional distilla tion of the diphenyl were good enough. The e&sple left an dour of tar at the end. of the distillation. Anniston' conent on British aaple 60788 wear that Its aeid wash test Just at the Unit of the Anniston specification (for *Badus trial R) again indicating laeospleb acid tre&tesat of the material. BaterlaX to this a^>l@ would pro duce good diphenyl* though a little extra attention to the diphenyl distillation. Bight be needed. The effect* of i^jurlties la th benzene were discussed in Axmiston reports 1640, p.19* & 1642* page 1 t 2. For a time no rery.high standard was et* but in recent years* trouble with the stability of Arcolors used for electrical work to renewed the Interest in this subject. See page 111*" below. In a Vhort form report ** No ,2152* dated H<yreMar 17A7# Hr. A. H. EUeaburg of Aimiston reviewed the quality requir#-**nt for benzene for making Biphenyl and Chlorbenzene, He found th available evidence to be ineoaeluaiT* and reeosisended aintalnlag a limit of 500 mlnlsmm for Biphenyl &d 520 for Chlorbenzenes. Dp, 2, E. Ssrdy* Bs,23A7* advised caution a accepting a lower standard* for baazone* whleh contained paraffins* would new /ifo-i 19 WATER PCB-SD0000045478 <L Specification > Test Methods, ecmtd 56 yield itym and apparently rinyX biphenyls, Br again t chlorine derivatives ware biased for skin trouble in tlm Arocler plant. as pointed out that though the chlorinated products my be stabilized by being held at high temperatures, it is not certain, that this process will go far enough* a April 28/^9, % Ellenburg mentioned the beneficial effect tialeh high temperatures la ok vtas are taaowa to hare on the purity of the beiszena (freedom from paraffins), See also th discussion of Effects of Variation in Benzene Quality/ page HI helm* Test Methods for Benzene Ffr.Pt. As neationed above, Amlaton use the method of md.Bng.Ghea.10. , p.1010 (20 e as^)le in the "as is* condition.,, put in a test tube In an ice bath* and when the solid benzene begins to separate, the feesperature will remain constant for a time. This temperature is taken as th solidifying point. Accurate 0.05C. Other Tests Anaistoa was A.S.T.M* methods^,but on Feb. 15/^9, Anniston v- porta4 that th British (H.B.C.) for of the acid wash test wi simpler, especially in respect of the preparation of th standards. On applying th H.B.C. test to their own benzene, they &wa& it to give a colour matched by only 0,1 g diehro- mate per liter of water as against th H.B.C. standard of 1.0 g. Th same benzene gar colour #1 on th A.S.T.H. acid msh test. DSW462113 WATER PCB-SD0000045479 c Specif!cations & Test Methods * contd \ 1mA for the Pota 57 Bo specifications exist on lead used in the diphenyl lead convertor unit ether than that "chemical lead" is to ht purchased# Apparently toe effect which is^writle in to lead my hare cm toe stainless steel* is sore feared than any effect on the confersion process itself# , V# . Wade of Amiston hare the following laformtimi "A typical analysis of chemical lead as nx^fp!l& fey the St, Joseph Lead Cospaay, 250 Park Are,* Hew York* New York* west Pfet 99.9272* Cu* 0.0608 . As* sb* 0.0001 Snt Fe* 0.0001 Zm 0.0001 Od: 0,0003 0.0048 Co* Agi 0.0066 Bi: nil "Elements that should fee particularly avoided* as observed is practice at Amis ton* and as recommended fey manufacturer of stainless steels* are, in order of importance: tin, rise* bismuth* antimony* and cadmium, Tin* sine* and bissufch should not exceed 0.0002* max,* antimony and eadaltsa* G.OOOfj* bz, "Caution should fee taken in plant operation to avoid contamination by any of to above elements." Speetrogmphie analysis has been foxmd useful for cheeking toe purity of the lead for the convertors. We are warned to look out for isaptaitlem which may fee picked in any reused lead. BCL have found a source of supply of lead apparently up to the Amis ton standard except that the bismuth content is 0.001* and the lead percentage only 99*9955. Amis ton consented that they did not think 0.001* of bismuth would cause any serious trouble. DSW 462114 WATER PCB-SD0000045480 Specifications and Test Kathodecont'd 58 Finished Products Diphenyl coda 3980-500-74-CK) ~T?e5unica.l) authorised July 16/45, (Sailed fro the mil tank, la eupercedea Kar, 2/38. the e&s of tank car Mies) Production Dept. Ho. 09 Appearance yellow to pale amber solid. Colour Pr.Pt . eoual to 2.0JS aqueous FeClo smz f6fi5T.7O adn. -> Dist. range 2 *5C. max. including 255UC. Freezing Point of Diphenyl Standardised Anschutz thorsosetor 40-100C. counted vertically near shaft of a ciaall electric stirrer. Bulb about 1/4" above stirrer blade, and 3/8* from the shaft. Magnifier cl&aped to thc-rwcnieter. Kelt and nix the sample. Pour about 120 o.c. into 250-.OC Griff.in bsaksr making cure thermometer is not above 100Cc Set be&ksr u.r>.der stirrer so blade is -1" above ths beaker, and tho thermometer icsnerced to 4oC. marie or more. Run stirrer at moderate rate through test. When cry stallization begins, the teit>erat\u*e will rise quickly about 0.4C. , then become 1. onstajit for 2-5 lain. before slowly falling. Highest reading taken avoiding parallax. Diet. Kenge of Diphenyl Plant "B" xasthod slightly modified by R.Sudhoff, Bar.8/37. 200 oc Pyrex (Coming 1600) die tilling flask. Keek grapped with wet asbestos paper allowed to dry on. 200-275 range precision Txylor type thermo, engraved stem 0.2 division. 1 4 a.ru Both bulb rsnd expansion bulb to be below the side tube, 6* auxiliary therso. 0-150, attached with bulb 2/3 way down tho emergent stem, Cover both thermos oSVM 4621^ 5 WATER PCB-SD0000045481 Specifications Tcist Kathc-ds, oont';d Finished Products, cont'd Kith 3/4" glass tuts-. Correct for emergent atom, and baronetrid and' thermions trie e:::-or. Condenser as for Barrett bensol distillation., i.e., 24" x glass tube @ 75 anc,l In copper trough. W ;sr at 75-85C. Auxiliary burner to prevent freezing at exit. Drtft shield 5" I.D. x 6* high. Flask on 6" x 6" pi&cc of 1/4" transits board with 1-1/4( hole. 7op of auxiliary bulb of thersoT&ster level with bottom of side outlet. Cork stopper flask to con denser . lgh 100 g. sex?:. 1 Into flask. Heat with Keker burner till ebullition starts, then vapour' ring reaches Into ths neck, but not to the side e.rn, oool a little. Repeat 3 tl^ea to get tb.err.ocster and flask neck heated. Distil 2 drop,s/ascend into broker on & balance. Read: 1st drop 1$ J$ 5$ 50$ 90$ 95$ 96$ 97$ Dry read auxiliary therusoirs ter at *, Record weight in receiver 1 minute after removal of flams. Dry- point! observe when last drop ie ves bottom -- needs two observers. ^760 - Baron. reaching ) x 0.036 = Tj. ' f,lot di'op - average of avix.iliary readings) x 0.000153 x no. of degrees ftbovc the bath * T2- Add Tj and Tg to observed readings. 5? 0sW 462AV6 WATER PCB-SD0000045482 Ov' Specifications and Test Methods, nt'd Finished Products, contfd Diphenyl Colour Melt 120 g diphenyl In low form Griffin 150 co beaker. Compare @ about 80C. with ferric chloride samples In bottles of same diameter as beaker. Standards 25g FeCl? *6Hp0 0.625 6* COClg in 200 cc PLjO * 15 oc HOI (S.G. 1.18), make up to 2p0 cc. Make Sfcandai*da 1 1 li 2 10 cc stock per 200 cc 20 w 60 80 Standard Mos. are ^PcCl^'SH^O. Sample 0-4072 of Finished Diphenyl was sect from Anniston to Ruabon, Oct. 13/47* gSW 462117 WATER PCB-SD0000045483 Spec1fteatIona & Test Methods, confcd 61 Ifr. Barden, August 1950, collected the rollowing test results at Anniston: ^yypleal Analyses: Diphenyl Date Colour F.Pt, Mst Range 1 drop 1* 3 5 10 50 90 95 96 97 dnj 31ft 1.0 68.8 0.6 254.8 25^.9 254.9 254.9 255.0 255.1 255.1 255.2 255.3 255.4 25/7 1.0 68.85 0.7 254.7 254.8 254.9 255.0 255.0 255.2 255.2 255-2 255.3 255.3 255.4 Lot 246 20/7 1.0 68.9 .5 254.8 254.8 254.9 254.9 255.0 255.1 255.2 255.2 255.2 255.3 255.3 18A 68.9 0.6 255.0 255.0 255.1 255.1 255.1 255.3 255.3 255.4 255.5 255.6 255.6 247 18/7 # 68,9 0,8 254,7 254.9 255.0 255.0 255.1 255.2 255.3 255.4 255.4 255.4 255.5 12/5 (1950) 1.5 68.8r 1.0 254.7 254.8 254.9 255.0 255.0 255.2 255.2 255.3 255.4 255.5 255.7 Date Colour F.Pt. Diet. Range 1 drop 1 \ 10 50 90 25/4 1.5 68.8 1.2 254.8 255-0 255.0 255.0 255-1 255.2 255.4 255.6 255.6 255.8 256.0 27/2 1.0 68.8 2.5 254.9 255.0 255.0 (1950) 255.2 255.4 255.6 255.8 256.0 256.4 257.4 Test result collected in 1947 are given on the next two pages, 62 & 63. DSW 462118 WATER PCB-SD0000045484 TBOHSICAL DIPHSHTL 5HXPMHT3 Bate Car no. IHatilXe tioji* FT.? t4 lot *G. drop 1# 3# % 10# 50# 90* 95# 96# 97# Dry Colour Dist;. Ft. RJU1EO aep - j/4? KOKX 659 68.9 255.1 255.2 .2 n .3 .5 .5 .6 7 .8 255.9 1.0 .8 mohx 504 68.9 255.1 255.1 .2 ,2 3 5 .6 7 .7 .9 256.1 1.0 1.0 Sep *7/47 OATX 37304 68,9 255.0 255.0 a .1 .2 .4 A .5 .6 .7 255.8 1.0 .8 sp,,10/^7 HOHX 147 63,9 255.1 255.2 .2 c2 3 A .5 .6 ,6 u? 255.8 1.0 .7 Sep. 27/47 MOKX 653 68.9 255.0 255.1 .2 .2 .2 A .5 .6 .7 .8 255.9 1.0 .9 Sep. 19/47 HOHX 651 68.9 254.9 255.0 ,0 a a .3 5 .5 7 .8 255.9 1.0 1.0 MONX 659 68.9 254.9 255.1 ,,i ,2 .3 A .5 .5 .5 .6 255.7 1.0 .8 6V^y Ql\3\ WATER PCB-SD0000045485 C nC SJS 1 7T VO CD CD t-- * *e q h o" Q j? -P R &< o H Ofvt n >s\ CM oo o H t- G\ e LA tn mm CM cm a o tn i a rH o C5\ vo vo e m mm LO X\ iA cm cw CM s *CO t- CO . oo in in a0 63 TECHNICAL DIPHKMYL SHIPMENTS & Ot ' . ft VO 9 t t 1 tn 0p W m C?\ VO VO o t- b 04ft in e I$ c\ m o tn VO e VO 9 CM z? O $ M- X*- tn tn tn cn tn 9 4 < in CM $ -M CM cn CO Ox CM --f 0 o in r-j o CM 4 CO CD o\ H 9 $ C O rl^ P H 4 H r-HC p. y+1 O <bH a-l Su p p ^O k ?j CM CO cn 0 ru eH CM CV * JU CM r*t o 0 n tn m in A m in in CM CM OJ CM Oi CTi 0\ C\ o 99 D CO CD CO O VO VO VO CO H e H co m tn CM CO a\ *4 j4- tn tn CM w Q\ o e CD Ov VO VO t lT\ 8 t- 30 co r-t H H H . X CM H -P Pi (Sfl) O CQ o 1H 0\ a\ ri r-i b- t-ef \ tiHn CM & O, cn to DSVV 462120 WATER PCB-SD0000045486 V Specifications & Test Methods, contd 64 SJammx R The properties of Santomx R aa given in "Monsanto Chemicals and Plastics" - 27th Edition - are typical analyse#. Tentative Sales Specification Color 3*5 - 4.5 HPA Solidification Hold Temperatures * Upper 137 - 143C Lower 45 - 69C Distillation Range* At least 80# between 350 - 400C (uneorr.) This property is not determined on every lot. See also under "Properties of Materials", page 13 above. DSW 462121 WATER PCB-SD0000045487 65 Specifications and Tort Methods (cent :d ) Analysis of Santowsx R DESCRIPTION Santowax R Is a yellow solid hydrocarbon mixture of micro-crystalline structure. The main constituents are ortho-terphenyl( meta-terphenyl with smaller quan tities of diphenyl and tri-orthophenylene present. The molten product is chilled cn a flaking roll and bagged or put in paper lined barrels for shipment. LABORATORY TESTS: 1. Color: 3-5 - -.5 NPA Test Method; A portion of the sample is melted slowly over a low heat. Care should be taken not to overheat the sample. Some darkening due to decomposition 5.s possible if the sample is heated above 250C for any length of time. The molten sample is poured into a clean 15 mm test tube and the color is compared to the standard disc comparator of the National Petroleum Association. ' 2, Hold Points: Upper hold point 137-l43C Changed Sept. 25/4 to: 137-1450 Lower hold point 45-6CC 45-63 Method: A 250 cc beaker is filled about three fourths filled with the flaked. sa^>l and placed on the hot plate to melt. After the molten sample has attained a temperature of 175~200oc, the stirrer and thermometer are placed in the beaker. The material is allowed to cool while stirring until crystals appear in the liquid. Then the thermometer- is watch closely to see if the temperature holds as the sample crystallizes. This temperature where the thermometer reads constant for a few minutes is known as the upper held point. The stirrer is removed and the sample is now al lowed to cool to about 8oC. The sample is then stirred by hand with the thermometer. The chilled material on the sides of the beaker must be inti mately mixed with the molten sample in the middle at all time3. The temperature at which the ther mometer stops after it goes down and rises to 1 to 3 Is called the lower hold point. DSW 462122 WATER PCB-SD0000045488 Specifications and Test Methods (cont'6) 66 Analysis of Santowax R - Page 2 Standard therr.c^etcrs are used In this test. No correction is made for stem exposure. 3. Distillation Eange: At least 80 per cent between 350~400c (unc\ rr.) Method: ASTM D-20 (modified) The apparatus is designated in the ASTM method and consists of a flask, condenser tube, shield, receiver, and thermometer. After assembly of the apparatus is complete, the sample is melted and stirred to insure proper blend ing. One hundred grams of the sample is weighed into the flaak, the flask is put in place arid heat is applied so that the first drip comes over in from 5 to 15 minutes. The distillation shall be conducted at the "ate of 50-70 drops per minute and the distillate collected in a weighed receiver. The temperatures recorded shall be at the first drop and at each 10 degree interval between 350-4QOOC, the per cent distilled over shall also be noted. This distillation range specification is subject to change as more history on this test of the prod uct is obtained. 4. Sediment Tests There shall be no insoluble impur ities In a molten sample of the product. Method of Sampling: It will be very difficult to obtain a good sample for this test and, therefore, the best means of having a clean product is to el iminate the sources of impurities and keep a check on these sources. For the above test, a 3 or 4 pound sample could be melted at hourly intervals to Bee If impurities were present. qS'N AR2A23 WATER PCB-SD0000045489 Specifications anc- Test Tiethods (cont'd) Analysis of Santovax R - Page 3 For a fool -proof method, a mechanical means would be needed at the flaking rc1Is to remove the metal scraps which are the main contaminant at present. If the rolls were capable of cooling the product to 30C, so that a cold, brittle product could be obtained, the metal could probably be removed by a vibrating screen of 4 mesh size. A magnet might also be capable of removing the metal scraps. At present the flaker is being resurfaced and a new blade is being installed to prevent the * 4lings from coming off the rolls. 67 DSW 462124 WATER PCB-SD0000045490 c Specifications a-nd Test Methods, cont'd 68 Extermination of Sulphur in Santorax Tentative liatbod; KO g. saj^ile, 20 g. Miclcei formate, 150 cc H.B. 40 (hydrogenated Santowax) In 1000 cc boiling flask. Heat @ rate of 30-4oC per minute to 285C. Vaterof cryst. of formate cornea out up to 200. Formate begins to decompose! around 24o, and rapidly @ 270-275. Heat to 285 and cool to 20-80C. Add 100 cc 1:1 HC1 and some 'boiling chips. Reflux till Si has dissolved, (foams), with Meyer or similar apparatus attached to condenser, 50 cc anraroniacal CdCl2 (!> of CdCI^ In the bulbe. Hash CdS to bsaker or flask. Make acid to ; henolphtbaleln with concentrated HC1, and dilute to about 250 cc. Add 10 cc X/lO Iodine and 5 cc concentrated EC1 added. Leave 10 minutes. ' Titrate iodine with K/lQ thio using staroh. Calculate to $ sulphur in r&ntonax. Do blank. Determination of Chlorine in Santown* 30 g. Santowax and 1 g. sodiuia in dry Hi crucible, 80-100 cc capacity. . Cover. Heat over low flams, until Santew&x has gone, then to dull red. Remove cover and allow excess Ba to bum uuder hood. Cool, wash well with ^Q- Make up to 250 cc. Determine Cl greTimetrically in 100 ec aliquot. Do blank by dropping Ha into water. DSW 462125 WATER PCB-SD0000045491 Specifioatloaa Santowax ft Test Kathode, t ' ' ' 69 goca 0-I5OI fto Specif! oat lori. Date Sep .15A7 Sep. 22/47 let UpDor Bold Losjst Hold Colour* Bo. Ft. Go Pto C. KPA 47 144.2 60.0 3<8 46 144.2 61.0 3.8 50 142,0 60,0 3c6 52 142,5 52 142.0 60.0 56.0 3.5 3-5 53 142,0 59 c 5 3-5 Sm^I G-4073 of Sastowu R wag seat fs*o* Aaalstea to Hmbf Oet,13A7* DSW 462126 WATER PCB-SD0000045492 c Specifications and Test Method? (cent'd) Finished Products (cont'd) 70 Santowax, (crude Individual isomers} Only small amounts of the individual isomers have been made. Test methods used at Anniston are given below. . V Analysis of Santowax Q DESCRIPTION: This material consists of crystals coated with a eutectic oil. The color is pale yellow due mainly to the adher ing oil. The product is about 97-93 per cent ortho ter- phenyl with traces of diphenyl and meta terphenyl which form the oil. Tliis product is distilled, mixed in the catch tank and run into drums to crystallize before shipment. LABORATORY TESTS: . 1. Color: 1.5 NPA Method: The sample is molted with precautions not to overheat and poured into test tube. The color is compared to the standard disc comparator of Nat ional Petroleum Association. 2. Hold Point: 53C - 55C. . Method: A portion of the sample is melted to fill a 250 cc beaker one-half full. A stirrer and a thermometer (standard!red) are inserted in the beaker and the material is allowed to cool while stirring slowly. When the temperature get3 down tc 55C, add seed crystals slowly until sample begins to crystal lize. Record highest temperature reached after ther mometer starts to rise. 3. Distillation Range: 10C maximum range. This range should include 335C (corr) Method: ASTM D-20 (Modified) Sane procedure as for Santowax R. DSW 4b/127 WATER PCB-SD0000045493 71 Specifications and Test Methods (cont'd) Finished Products (cont'd) Analysis of Santowax 0 - Page 2 The temperatures recorded should be at the first drop and at each 10 per cent of distillate up to 90. Then the temperature should be. taken again at 96 per cent of distillate. Receesary stem temperatures should be taken to correct for the emergent stem. Correction should also be made for the atmospheric pressure. The distillation range teat is subject to revision when more history or. this teat of the product has been obtained. 4. Sediment Test: No insoluble impurities present in the molten sample. Method of Sampling; The material shall be fil tered through 100 mesh screen as it is loaded into drums. A sample of the molten product shall be inspected for solids . The drums also shall be inspected for cleanliness. DSW 462128 WATER PCB-SD0000045494 Specifications and Test Methods (eontd) Ptalahod Products, eontd Analysis of Santowax "k" This mtwSMl la a yellow solid of crystalline structm*. Tb purity is approximtsly 95 Pr cent jseta terphenyl with para terphenyl mkiag up the reoaindep., The pre sent method of separation yelids a meta-para utectie at 3.3 per cent para which accounts for most of the para contaminants ' At present this product is crushed to liwps mo inch or atm21@Ft and hipped in paper Mgs or paper-lined barrels. Laboratory Tests t . 1. Color: 1,5 - 3.5 XPA Method: The s&isple is melted with ear not to dis color by heat and poured into a 15-am test tube. The color of tbs molten sa^l is conpared to the standard HPA disc comparator, -*4 ; 2. First crystals: <K)C. Method: A 250 ec beaker is filled about two-thirds full of the asolten sai^le and placed under a stirrer and a standard thermometer. The material is allowed to cool with stirring until the teas>er&ture reaches about 90C. Seed crystals of the saspl are added slowly as the cooling continues e The temperature at which new crystals cmm out of the solution Is recorded as the ''first crystals" point. 3 Held Point: 83-85. Method: Stirring is continued in the abowe sample while the temperature goes down and then rises 1-3C to the hold point. The highest temperature at which the temperature regains constant for a while is re corded, ! 72 DSW 462129 WATER PCB-SD0000045495 Specifications andTest Methoda (cent'd) Finished Products (cent *d) Analysis of Santoyax Page 2 4. Sediment Tests No insoluble Impurities are present in a molten sample of the product. Method of Sampling: A sample of the crushed mater ial as it Is prepared for shipment shall be melted for this tefet. The product can be-filtered before it is remolded after removing the water. Then it can be crushed to 1/2," size for shipment - Under the present open air method of handling this material, the dirt is especially hard to keep out. ,\N 46*^ WATER PCB-SD0000045496 Specifications and Test Methods (c on t8 d) PlnlBhed Products (ccnfc'd) Analysis of Santowax P . DESCRIPTION: This material is a white solid which crystallizes in thick plates. The purity Is 95-98 per cent with small amounts of meta terphenyl and trl~orthophenylene as the contaminants. LABORATORY TESTSi 1. Color: 2.0 KPA Method: The sample is melted and poured Into a 15-mm test tube. Of the standard disc comparator the color 1b Judged h!th KPA standards. 2. Crystallization Point: 209-213C Method: The cooling in this test is started in a mineral oil bath heated to 230C. The sample, is melted and poured into a large test tube. The test tube is placed in the mineral oil bath and cooling begins. The test tube contents are stirred as seed crystals of the sample are added. When new crystals appear In the solution the thermometer which is in the test tube is read. This temperature is the cry stallization point of the para terphenyl. 3. Sediment Test: No insoluble impurities are found in molten sample of the product. Method of Sampling: A thief sample of each barrel of material shipped shall be examined for impurities. This material is also hard to keep clean under the present means of handling. DSW 462131 WATER PCB-SD0000045497 Pontrel f@eta Conversion Stage t <t> Conversion There Is * 0Btttia fro the pip between ttm lead trap and the bottom of th eelutn a the convertor* leading fee a small* water-cooled condenser. Sample# of the vapour mj b &m,mi off at any tins* condensed* and a careful measure ment of the density of the condensate mad, as a measure of the 0 conversion* The Anniston operator ikee this tost one# & day on aeh tmit* usually in the morning shift. Each tm.lt has & sailing condenser* as shot on the attached sketch, permnently connected* and there is a steel sheet "fire screen" to protect the operator and th equipment fro the radiation fro* the conversion unit (especially the lead trap). Th eperator starts th water flow through th condenser and open* th# asapliag valve enough to give a distillation rate of about 500 Bsl/tsp as Judged by eye. Ho .purging with OOg is done. Some of the condensers have a screw cap fitting with the condensate and vent tube passing through* others simply have a two-holed rubber btrag. In either case* the sasple bottle Mist mfa a good vapour-tight connection. The use of spring clips to hold the bottle against fclie stopper has been suggested. Th sample bottles are of glass* square, 3^" x 3^" x r on the straight side* with screw necks* and the operator carries 12 of the* one for each unit (clearly numbered) in a wooden rack* puts one on each unit* leaves the for about an hour* then turns off the vapour and water, removes the bottles* puts on their screw caps or blank corks* and carries th twelve of tbs to his test bench where he has a twelve-holed water bath, at about r-oa teiders,ture* and leaves them until their to^eratur is somewhere between 34 and l6c. A portion of each sa^>l in turn is poured into a glass hydro aster Jar end its tsi>ratur and density observed. Th hydremter 1 graduated 0.880 to 0.950 Sp.Gr. in 0.0005 divi sions and should have been calibrated. The te^>ratur should b# determined with an accuracy of O.20* and even at that th test is not highly accurate* but it is good enough for routine control, . Tint % conversion* corresponding to th density and tBf>erature* is read fro th attached nomograph. Th samples do not crystal- Use* but care met* of course* be taken not to allow serious loss of benzene by evaporation during the saspllng and testing. Th sasples are quit hot when first collected* and there is a distinct mmU of benrea (and BgS) from th vent of th test condsnseft while the sa^>l is being taken,, There is* of course, a slow stream ef hydrogen escaping through the bottle. n/Mr WATER PCB-SD0000045498 DSW 462133 ^vx.v.Jile bo'Ctle - :>V* Y . -fr'pjghT "bide w i H-l <C*~aw_ n<-<;L -C--O--N--D--E--N--S-E--R----F--O--R----C--O--N--V--E--R--S--I-O--N----T--E--S--TApprox, scale 1" * 1'-0" //' WATER PCB-SD0000045499 BSH&SM cosmaio?? chabt From Final Report No. 1712, "Study of the Diphenyl Process, Part III" By F. T. Kilei October 19, 1042 0,900 -t -F 0.910_______p -T j- 0.92H Speoifio Orov'ity t4 -r t 2 34 32 3 0 30 1 z 8 28 " I-6 26 T = 4 24 * 4-* 22 o 20 I e IB .6 16 Temperature C. Banograph for Calculating Conversion of Benzene frc Specific Gravity In the example shown by a broken line, specific gravity of 0,8977 at 30,0*0. shows 18.65 per cent conversion. 22 \= 21 18 ___ 17 t 16 DSVV 462134 Per Cent Conversion WATER PCB-SD0000045500 Control Test oorstd ?6 Conversion oerntd TMj conversion test 1b net done until a unit has settled dot to steady naming condition,. If the % conversion of any wit ia distinctly different frca 18, the tcapera tup of the conversion pet will be altered, 2 to 3C at & tlaa, to bring tbs conversion back to noml. Analysis of erode Diphenyl Halt 100-150 g. in a 250 diet, flask with 10" eolum, into weighed receiver to 275C. diphenyl = weight distillate x 100 weight sample Distil Test for Benzene Leaks Into the Stack Gases Se page 91 below. Distillation Stage "Bold point and crystallising points are used in the control of the distillation of diphenyl and of Santowax, though in both oases Amnia tea rim the stills largely by "dead, reckoning", plus eoliaan top temperature in the ease of diphenyl, because of the tiB required to take the sasples and ak the test, (See page 46 above), The test bench in the department is, however, equipped with the mechanically stirred crystallising point apparatus described tasder "Specification & Test Methods" cm page 58 above. See sa^l 0-4071 of Crude Diphenyl, sample 0-4074 of still Bottom fro the diphenyl still, and maple 0-4075 of Still bottom fro tha Santowsx still, sent fro Anniston to Ruabon, Oct,13/47 Sables 0-4074 & 0-4075 were lost, and repeat samples were sent 3&a. 25/49 to London, Benzene recycled from, the distillation, stage should not contain lore than a few part per cent of diphenyl. The operator can Ittdg by the colour of the benzene and by allowing a few drop to evaporate 00 hi finger, but a freezing point test would give a better criterion ' WATER PCB-SD0000045501 um OF BRAWHIPS 77 There are over 350 drawings on file at Anniston, but copies only of those thought to be of interest to MCL hare been sent to London at different tioes, as listed below. Those narked "a" in oolum 3 were sent by Mr. JTagel of Amis ton, to Hr. V.M. Cooper in London,by airmail, Oct. 10/47# a second copy going by sea mil to Mr. M. Buis In London, Oct. 13/47* GSSring SSL!____ Date sent Sent fc.0... titHfcllil. A& ^aem Conversion Chit AA-5581 Cast refractory tops for linings A 90-5584-3 90-7817 Cast steel door on shell of fur nace A Lead pot,flange,& thermowell July 21/50 cm 90-7845-5 Stacks on V&pourixar A 90-7847-8 Pot #1, details,with later revisions A 90-7937-^ Baffle for distributor A& July 21/50 OWM AA-7955 Cast steel flange for distrib. pipe A 90-8131-4 Details of coluan A 90-8143-3 Traps for eoltnm A 90-8147-3 Stainless piping for convertors A serves for references to 8147-1 & 8147-2 90-8151 Brick lining, #6 unit A 90-8153-3 Details of mounting of burners 90-8159-1 Manhole Into stacks A A 90-8166-4 Pot over July 21/5$ OWM 9C-8166-2 Pot cover,Baffle locations, units 11, 12, & 13 A WATER PCB-SD0000045502 List of drawings, comtd 78 Swing' Ho. Description Omrrersioa thlt, eoatd Date sent wuQtTrl&r to MCL to Remarks 9C-8194 9C-8205 Lnyout of pipings diphenyl trap* to &\af) tanks Layout; benzene feed tanka & pmps Hor*13/50 Hov.13/50 see letter rm EM-DOT Hot.13/50 for amend ments rm do 9C"8208"2 Layout; feed piping & waters Hot. 13/50 dot do 90 "9015 Layout emits 11, 12, & 13 A 90-9019"! Preheater pot A 9C-9019-2 Distributor July 21/5 0WM 90"9022 Convertor shell, units 11,12,& 13 A 90-9024 Thpourlzer coil details A 90-9025 Vhpourizer shell A 90-9026 Vapourizer assembly Apr.l/48 DSH Revised to Hov.lt/47 90-9054 Gm piping to burner, & bill of materials A 90-9055 Vertical condenser & split flow box A 9AA-9058 90-9069 90-9070 90-9075 Expansion flange in steam Jackets^ piping Aug.10/50 bwt Layout of benzene rtmbaek Hot . 13/50 DOT see cowaent m-im Hot.13/50 H2 piping to coolers Hot . 13/5<1 dot Benzene line, coolers to feed tanks Hot.13/^4 dot 3W 462137 WATER PCB-SD0000045503 List of drawings ji ccmtd 79 Swing So. Description Ho. 2 Diphenyl Still Late sent Sent to KCL to Remarks - 90-7870 Fractionating eoltm A 9C-7871 Layout Diphenyl still #1 A 90-7872 Condenser A 9G-7873 Still A 90-7875 Diagrammatic flow sheet Hew still* Included In "Design Data for Diphenyl St ill'7 Sept/38. Jime/46 90-7877 Kiboiler tank A 90-7886 Swire1 split flow box A 90-7888 Diphenyl' still condenser details July 29/48 DSH 90-8152 1500 gallon catch tank A 90-8192 6000 gallon catch tank A 90-8193-1 Layout of crude eateh tanks 90-8210 Layout #2 still A A 90-8211 #2 Stm heater shell A 90-8212 #2 Still heater assembly A 90-8213 #2 Still catch tanks A 90-8214 #2 Still beads and tails tank A 90-8215 #2 Still* piping from snap tank to still A 90-8223 Hotaweir A 90-8224 Rotaweir details A 90-8254 layout of piping, plan fc eleratlotij Diphenyl still A DSW 462138 WATER PCB-SD0000045504 List of drawings, oontd Vo. Description Hydrogen Compression n g_ A-Mitefew "j UJ %n ' ttiriM 9C-7360 Armngeaenta for burning Ho (obsolete), not sent to HCL, 90-7366 90-8o4o 90-8165 eoafprj wiring & control oondenser piping wiring & piping dlagraa 80 Date sent Bray to *EL to Recmts discussed in AME's letter Jhne 30A8 May 24/46 DGH A Bee note on PC-7366t 9C"8l88 9C-8279 Layout & piping Layout piping from units , A& broT. 33/50 fco<S AOkiU' N0T.I3A0 EM t DWT for amend ments HSB-14836 Griscoa Russel Cospany Condenser (Pinned) * See AME's letter June 30A8 for corrections to this drawing, also E.G.Tboenaa, Kay 2lA8, explaining that it relates to one compressor, while 9C-8lo5 refers to 2 and 9C-9095 to 3* 9C-9095 Hot seat to MCL Santowax Distillation 90 "8551"1 High boiler distillation June 1946 mm 9C-8551-2 KlaratIon A 90-8552 Highboiler distillation June 1946 eaom 90-8552-2 Pictorial Elevation A General 90-7850? 90-7851 90-8140 Diagrammatic Plow Sheets. Inclu June 13A^ ded in "Design Data, 4" Diphenyl Unit, "Aug.9/39 #6 Chit. March 25Al June 13A^ EAQjS DSW 462139 WATER PCB-SD0000045505 Hat of drawings, eontd 81 Er33f35g .WGe Das crip tIon Seiml, eoatd 9-8X90-1 (Je&eral layout, units 7*8,9,10 90-8466 Plow Shoot - Converters 9C-8550-2 Plan 90-9060 Xnstrimentatlon diagras Diphenyl (electrical! Shows Benzene feed systen Date sent "Sent" to MCL to Reimrks Jfov. 13/50 See letter B to BWT Jfov.i;1950 for eaeo Santa A A A& Hot.13/50 mr DSW 40 WATER PCB-SD0000045506 CFEHER&L HOTBS OH BQPIPMEgT LIST 82 Reference should be mdd to Anniston drawings and design data fear further details of the different pieces of equipment. The following list is Intended only to giro a general description of the equipment, and a few comments picked tip during various visits to Anniston., The equipment list is valid only for units other than #4 and #5 The design was developed at Anniston and gone modifications were introduced when units #4 and #5 were planned* These change were found to be undesirable and the design of subsequent units, including #11, 12 and 13# (the last installed ^followed the ori ginal pattern. See page 3 2 above and page 85 below. All benzene lines are s tears traced and line carrytag diphenyl or hi"boliars are steam jacketed, the Jackets being liberally provided with expansion Joints. (See Anniston drawing 9AA-9058). It is important to carry the steam Jackets right up to the flanges. The diphenyl conversion and distillation units were indoors, the store tanks and the Santowax distillation malt outdoors, with some shelter for the heating furnaces, vacuus pub$> and instrument panels. See the notes oa "Gaskets" page 24 above. The conversion. and still buildings are high, with effective roof ventilators, and are open completely on. the Saat side, up to the level of the working floor. (Pot rim level). See also pages 16- above. The floors all are of vertical steel grating and iuaaiflton are very e^hatic about the advantages of tola. Flanges on the conversion system piping are of the standard awsonia, pattern q? to 3 s pipe site, and are special east steel tossgue and grooved flanges of Monsanto design ^.bove 3". Crane eXwp gate valves up to 30GC, no valves above 300C except cast steel gate valvea on. the diphenyl still* H&teri&la of construction for various items are detailed in Anniston Research Department, Report Ho. 164-2. See also pages 22 & 41 above and 86 & 88 below for notes on the choice and performance of different stainless steel. DSW 462141 WATER PCB-SD0000045507 Equipment List, eoatd 83 #1 Benzene Storage Tanks Five horizontal steel tanks. See also pages 17 & 29 above. #2 Pump for stipplylng #3 Controlled by float In #3 which exits off the puaf> when the (5000 T30Q) task, item 3# eontains about 4,500 gallons, and re-starts It at about 4000 gallons. #3 Recycle Peed rank See also page 29 above, monte In letter EH - DOT, but see amend- She tank in use In November 1950 was a horizontal cylindrical steel vessel with bulged ends, about 7'"6" diameter by 13f"0" straight side. Capacity about 5000 TJ3G. Set in side & concrete retaining wall outdoors at some distance from the flow control room. Pipes to and from the operating building run overhead xmder a steel sheet shield with a steam tracing line. Fresh benzene in from #1 via #2 under float control; re covered benzene in continuously by gravity from the reflux spilt boxes, item #12, of the conversion units, and semicontinuously by pump from the benzene receivers, item #27, of the hydrogen compression room. Benzene in (after exami nation), bstebwise by ptmap from the benzene receiver. Item #21, of the diphenyl still. This batchwise return is dis liked, for Newport conditions because it would cause wide variations in the ratio of fresh to recovered benzene, erf it has been proposed to interpose a buffer vessel so as to smooth out the flow. Senses out, by a bottom outlet with an "upstand" in the tank to retain water and solid matter, to the feed pum>, item #4, The us of a bottom outlet helps to prevent air locking of the pumps. The line to these p^>s Is Jacketed for steam,but it had no steaa connections la November 1950. It is cemented through the retaining mil. Drain, from a sxsqp at the lowest point of the tank for removal of water. This drain requires attention several times a day and should be conveniently located so that the operator can see when the water has an run out, and the benzene Is coming. There is no special provision for s&jspling, though a sa^Jle sight be drawn through the drain valve, or taken p^oa^ne of the branches on the line from the feed DSW 462142 WATER PCB-SD0000045508 Rquipaant List, eoafcd 84 #3 Recycle Peed Tank, Contd Tented to the hydrogen system by mans of a 1%W Insulated line, (the tank outfits are usually nans at Amis too, ly fro* the stress of recycled benzene.) There Is a rbranch on the top of the tank, with a gate tb.1t through which the tank might be gauged. This Is rery rarely dots. Float controller stopping the pi^>, It an #2, whan the tank contains 4500 ISO, and restarting it when th level has fallen to 4000 QSO. Floats for high and lem level alarm. (There is no formal drawing of this arrangement). These various floats are now made of glass, stainless floats taring failed, end stainless guide rads ere recommended because sticking of the float my earns bad trouble. The domes over the float controllers are insulated and itea traced, but the tank itself is not insulated. It is, of course, electrically earthed ("grounded"), Anniston experience is unfavourable to the use of internal steam coils in benzene tanks b-scause of the risk of water getting into the benzene if th coil, fails, and of benTM zeae loss via the oil. Even if the oil is taken out over th top of the vessel, loss is possible by siphoning. #4 Feed Pimps to the Conversion Units Anniston report 1642 of Oot.15/41 describes th feed pu^ps as Weseo Bo.507 (one then for each unit) with hand-operated by-pass to set the delivery rate. Stainless starts with Tfi Resistw lapelixira and liners. 1800 HPM,, In Hoves^er 1950, one Gould centrifugal puop with an inTM stalled spare (and room for one more) was serving the whole 12 units through a row of flow controllers, one for each unit. It was of the 2-stage centrifugal type, 3^00 HPH, (but this high speed is disliked by the operators). Gland packing of fiber-reinforced rubber rings, with the gland nut aImply tightmod carefully with th band. * Delivery about 170 03G/br/Wit at 100 pslg. A steady feed rate is important because fluctuations is the rate cause variations in the pot teaperatures (Th flow of fuel gas to the preheater pots is set by band, and con sequently is act automatically readjusted to meet such . variations. Th convertor pot temperature is automatically controlled, via the fuel gas supply rate, but naturally th control lags, because of the sensible heat of th lead, the pot, and its setting). * These ring are mde for the steam of water valves, but they have been' found to serve better than other packings - i-'- - *----------- 1-------- ---------------- & (SIS** 1 1 "i TUX DSW 462143 WATER PCB-SD0000045509 gquipnant List, eotatd 85 #4 Feed Puqps to thp> Conversion Units, eontd There Is a Fisher strainer on the line frost the feed tank. Item #4j and the pumps deliver to twin filter Teasels In the flow control room. See under "Process In Datall" above, page 30. #5 Conversion Units Drawings. See list under "Diphenyl Process Drawing List" subtitle" "Conversion Halt", page 77, especially1 90-9019-1 9C-9022 In Hoveriber 1950, Anniston had 12 units, of which two were of the two-pot type with special tubular heat exchangers, to transfer heat fro the converted vapour to the in cosing benzenevapour, and the remainder were of the 3-pofc type. There wore numerous minor differences frba one unit to another, representing different stages in the design history of the process * The 3-pot units are preferred, and will be described In this report, because the design of the Newport plant is to be based on the 3-pot system. A 3-pot unit consists of three essentially similar stain less steel vessels, about 6,-0" deep by 1'-10-3/4" I.D. (esc drawings listed above), each sot in its own gas-fired furnace. The benzene vapour passes through the three in series, called respectively 1st preheater, 2nd preheater, and convertor. The 1st preheater is in the Middle of the row of three pots, with the 2nd preheater on one side of it and the convertor on the other side of it. The furnaces are of firebrick, with steel casing. Each setting 1ms eight gas burners, horizontally directed tangentially into it, four at on level and four at another, evenly spaced round the circumference, and there is a pres sure gauge (about 22 p.s.i.g.) on each burner, between the control valve and the Jet. The flue gases fro pots 2 & 3 go downwards to cross flues leading to the bottom of the setting of pot #1, then up inside that easing, and out to a flue leading to the bottom of the setting of the vapourizer, ite #6a. There is a steel door, with tabbing hole, at the bottom of each setting, for running out lead in ease of leakage fro a pot, and there are access doors in the flues where needed. DSW 462144 WATER PCB-SD0000045510 ISqv&Qimnt hist, eontd 86 #5 Conversion Unite, contd By means of daspers, the flm gases my bo by-passed aay from the vapourixer tw passing them Into a -rent stack. The te^awtuTM of tbs three pots ai* discussed raider "Proi la D@ts.ll* on pages 33 aM f>l above, and it will be soft that the #1 pot is at a auoh lower tajqpar&ture than the other two. Actually the waste heat from pots 2 and 3 is almost enough for #1, but the burners la th #1 setting hare a little work to do, and of course, would b seeded If the pot had to be re-started fro* cold. Benzene fro* the recycle feed tank, item #3, Is forced by the ptn^ps, ltea #4, against the back pressure of the whole conversion system, to the top of the v&pouriser, it* #6a It Is vapourised In passing down the colls, and the vapour bubble* through the lead in the three pots in series, then passes, via the lead trap, itea #7, to the bottom of the fractionating eoltma, item #8. Each lead pot has a dip pipe reaching nearly to the bottom of the pot, and the upper part of the pot ha circular baffles to diminish the entrainment of the lead. A groat deal of experimentation has been devoted to such problems as the design of the dip pip and of distributors, (see below), for use at its lower end, the design of the baffles, the choice of stainless steels for the differ ent parts of the equipment, and the choice of gaskets for the pot overs. Something of this can be seen from the *Hote oa the Maintenance of the Lead Pots8, on pages 4l- above. So attempt is sade here to review the whole history, but only to describe the arrangement now used, with present-day ideas for improvement = Various old patterns of pots etc are still giving good service at Anniston. The pets, and the fitting inside them, exposed to the hot lead, (but not the overs), are of stainless steel. See pages 88 & 8g below for the choice of the type of stainless steel, also page 22 above. Amis ton use steel covers for the pots. The #1 pots have flat covers, of steel plate welded on to the ria of the stainless pot. Some of these plate covers have heavy radial fins welded on for stiffness. The #2 pots have heavy oast steel domed covers, bolted on, with heavy cast steel (divided) backing flanges under the pot rims, The backing flange has four lugs, fitting Into sockets on the furnace roof and supporting the pot so that the rim is several inches above the top plate of the furnace easing. DSW 462145 WATER PCB-SD0000045511 Equipment List, oontd ST. #5 Qoaverslon Itelts, eontd The gasket is this ease la 5/l6n round soft annealed copper, with a square section asbestos gasket inside It. Bm |rd pot is similar in construction, but ha a gasket of X* braided asbestos rope. Hr. Barden took a s&apl of this in August 1950 This thicker gasket Is used be cause the edges of the flange pull together la service at the high teaperature, and they wm remain In service longer with a thick gasket. To sake the gasket,a pleoe of the asbestos rope is cut, long enough to lie Just Inside the twit circle, plus a few Joshes over-lap. The ends are overlapped, end the groove between the overlapped parts is stuffed with strands of asbestos rope, and the overlap bound with a few thin wires. Liquid glue is used to help in Baking the overlap and in holding the ring in place between the flanges during assembly. In us^ the Joint ring becomes cooplately flattened and bard. The use of restriction orifices after #3 pot, as discussed on page 34 above, has thrown Each greater pressure cm the Joint of the pot and the asbestos rope gaskets are giving such sore trouble. Vertical sheet iron fences, about 6" deep, in two halves bolted together, are being looselyfitted around the cover Joints of some of the conversion pots to deflect assy possible burst of flame due to a fail ure of a gasket. i London'8 proposal to use thicker covers and, backing flanges, and to sake them of stainless steel having a higher tem perature yield point than the plain steel ones, is liked at Ansslston, because It offers a chance of using copper gaskets on the conversion pots as well a on the preheaters. London's proposal to us slotted bolt holes is disliked as tending to favour the bending of the flanges, London also suggested supporting the pot rl cm a continu ous ring instead of on the four lugs, but this arrangement would appear to make the over bolts more difficult of access, to rob them of the cooling effect which exists under the Anniston arrangement, and to sake the raising of the pot a Httle sore difficult. At Anniston the eoa^anlon flange rnder the pot ri* is in two halves, bolted together, as mentioned above, fanning a circle, with four lug at right angles to one another. Pairs of short pieces of angle iron are welded inside the box frame which composes the furnace roof, these pairs forming guides for the lugs on the em^mnion flange. Steel packing pieces are placed first on the bottom of these guides to give the necessary elevation of the pot. then WATER PCB-SD0000045512 gqulpaent Mat, eontd 68 #5 0oarers lota Halts, eontd tbs pot lowered in and secured by steel wedges driven is alongside th@ lugs, The pots should not be rigidly conneeted to the fvrmce easing because the continuous vlbra- tiea of the pot would be eossBunieated to the brickwork of the fumaee, and tend to mice it ortsabl. It Anniston they fit fairly closely into the round holes in the furnace roofs, but in sons eases steel sheet sectors are used to bridge the gap. in any case, the Joint is imde good, either with clay, or more recently with a paste contain ing asbestos fiber (insulating coEpound 66) ,, This help to keep the pot rims a little cooler. The bolts in the pot cover Joint and in the adjoining pip flanges, are of ordinary steely at Anniston, and are never re-used, partly to save time and because they beeass stretched, but mainly because working conditions can be very uncomfortable because of the radiation of heat froa other units. Hewport, using stainless bolts, and having only one unit should be able to re-use the bolts. It is suggested to use nuts of dissimilar metal, to diminish galling. Xa cutting out the bolts on the pot over, the Anniston welder uses an oxy-acetylene torch, and cuts through the base of the nu t, flush with the upper surface of the cover, and the stub of the bolt is then knocked out downwards, the pot cover being high enough over the furnace roof to leave room for this and for the insertion of the new bolts. On the pipe Joints, the bolts are out between the flanges. The cover bolts have square heads, but hexagon nuts, and they go through the flanges, tail upwards. Ssll squares of steel (old nuts will serve), are welded under the ecn^o&aion flange, between the bolt holessto pre vent rotation of the bolt. The nuts are run on with an air"drivea spanner, for speed, and tightened x%> after the pots are hot, with a 4* long ratchet spanner. Anniston advis strongly against attempting to us a tongue and groove Joint on the pot covers bec&us of the risk of dis tortion. The attachment of the stainless pot rim (by welding) to the pot itself appears to b# a line of weakness because th lead in the pot is very heavy and is gently buying and vibrating whenever the vapour is passing. Cracks at this point are not tmknown. Anniston have increased the thickness of the rim of the pot) formerly 5/&nt flow 1D. British makers of stainless steel agree that 309 stainless teel tend to be brittle at the pot temperature, but that 330 does not. M3L are experimenting with pots fabricated, by welding, froa eentrifugally cast sections of 330 stain less, welded either with 39 or with special electrodes. ' nsW 462147 WATER PCB-SD0000045513 Equipment List, cotd 89 #5 Conversion Chits, eontd (5<s the latter from Michigan Steel Casting Co, to Annis ton, May 3X/50) 1? Anniston discussed this desiga, Aug<,!/%$, Beat tmtMotj, after fabrication, is reoomended for both 309 and 330 stainless* Inconel, Eureka, nickel, and alloys rich in nickel are said to gl.ro poor service, Anniston reported, Aug,l ft 5A9, that east thermo sells of 309 had proved to be brittle, Ceatrifugally cast dip pipes of 309 were better than rolled, or mold east, but were brittle or became brittle in s errice, Centrifug&lly east dip pipes^h&v recently (1950) given excellent ser- ^of 310 vlea. It is noted that in this method of easting the dross atain tends to form on the inside of the pipe, but no barn less appears to have resulted. Thera wells of cast 330 have steel) recently given very good service. Carbon tends to build *p in any crevices in the interior of the pots, and to exert a bursting pressure. Cast covers should be free from pinholes, blowholes and slag inclusions. Anniston warn against welding cover strips on the outside of welds on the pots. Outlet branches on the covers should not extend down into the pot, and the Joint should b# welded inside, to fill tip any crevices. Sharp edges of metal also tend to attract deposits of o&rbon. Any distributor at tha bottom of the dip pipe most be such as will not increase lsfilngement of the gas on the pot wall, because of erosion. Anniston are using a sisple open-ended pipe with a renewable liner for the last few inches at the bottom and four 5/13* hole drilled radially through the waH about 4m from the bottom. At a meeting at Anniston, Mar, l/#9, a proposal was made to try a deflector which would discharge the vapours tangeatiaUy in a horlssontal direction. This it was thought would give the lead a swirling notion, diminish vibration of the pots, increase the contact tin of the vapours, diminish tha ise of the gas bubbles, and diminish the entealament of lead. Barrow orifices must be avoided in the design of assy deflector because of the building up of earboa. This deflector had not been tried at Amistcm, but London asked that the pots to be supplied for Bewport should have a deflector. Standard dip pipes were, however, shipped in lovemberAO te avoid delay. DSW 462148 WATER PCB-SD0000045514 Equipment Mat, eoatd 90 #5 Conversion Chita, eontd Jeiai City, Atig, 10A9, aat MSL a drawing of the distributor they had develop4 for pots for propane cracking. There is iso heat Insulation used anywhere in the conversion system# except that fch vapour pipe from second preheater to the convertor is insulated os some of the units. It is desirable to avoid loss of heat anywhere along th line of flow, up to the top of the convertor pot# and at <m tins th pot lids were insulated. It was found, however# that greater distortion of the pot over and bolts resulted. Tbs inselation of the vapour pipe from th# second preheater to th conversion pot is not an easy task. la some cases, asbestos fiber# Inside a sectional (lobster back) easing is used, and. la other cases a special Johns Mmrrtlle powdered product in a dust-proof steel easing. This insulation and easing adds to the weight of the pipe, and my cause sagging, and all these long pipes# frost 2nd to 3rd pot# whether insulated or not, have support stirrup, which, however, appear to be out of us. In addition to the vapour inlet and outlet and th thermo well, each pot cover 1ms a. fourth opening. On the conver tor pots this is blanked, but on the 1st and 2nd preheaters this opening is used to connect the balancing line. These connections run in 1R pipe vertically for about 7'-0",and then Join into a horizontal header running to th# hottest of the eolwm# item #8. There is a pipe coupling on this line about 2'-0* above th pot cover, thro a branch for a pressure gauge, than a etop valve, which is normally closed. These gauges show the pressure In the space above the lead in pots 1 and 2, and the line toy be used to by-pass a pot in emergency# and to prevent lead fros being forced backward list th vapourizer. There is a pressure gauge ess a breach la th vapour line fro the convertor pot to th eolws, 4Xbo a branch for the sailing condenser des- erib#d tmder "Control Testa8 on page 75 above. There is a heavy I-beaa about 18" deep, with 6 flange*, and with a chain block . . permanently installed# running along it , one for aoh row f 3 pot, with a hinged section of the floor to permit lowering a pot or a lead trap to the ground floor. When a pot is put obt of action opporttmity is token to clear debris fro the bottom of the furnace. DSW 462149 WATER PCB-SD0000045515 ( ~S Nn.... TO SHOW EQUALIZim LIKE ON LEAD POTS S^c4t i lLo &jL Xxtc-^ -SO t r\A aStewf K f ir r n T AT. \ DSW 462150 WATER PCB-SD0000045516 ggutpaent List. ecmtd #6a Vtepmgtsera Drawing. 9C-7845-5 9C "8159-1 90-9024 90-9025 . to per conversion unit E&eh. consists of a single oil or of two Us in parallel* In a brick lined itel task through whieh the flue gases pas. Beams parses downwards through the oil countercurrent to the flue gases. The yap ourlxera firit installed at Anniitoa had two eolls In parallel* one Inside the other with a eoaaton inlet header* and a control valve on each exit, leading to a Y pipe into the first preheater. This arrangement was found inconvenient.,, and 1ms (except in the case of one unit) been abandoned in favour of a single oil. There was son doubt about the proper sharing of the flow between the two eolls* and considerable trouble with car bon blockage. Anniston report 1642* Oct.15/41* states that corrosion of the vapourizer coils nay occur by con densation of moisture from the flue gas* near the point of entry of the cool benzene. A small leakage from a vapourtzar coil into the flu my easily pass unnoticed* because the benzene will probably not ignite in the stream of flue gas, and the 1atomy cause serious losses before it is discovered. As a safeguard against heavy losses a sanple of the flue gai is aspirated every day from a point in the flue, imm&istely above the vapourUsgr oil on each unit, and la passed through a mixture^equal parts of sulphuric and nitric acid. For this purpose a " steel pipe is per manently installed in the vapourizer flu and all these pipes are carried down to a test bench on the ground floor. The sulphuric -nitric mixture is put into small rubber steppe red bubbling bottles, which, for safety* are sheathed in simple steam-pipe sockets, The bench has a sii^>le water aspirator, and it is the night opera tor's duty to test all mite. H stilly aspirates the gas through the acid for about 10 minutes, then ssslls the acid bottle. Blockage of tbs vapourlzer coil is rare (except by lead forced back from the first preheater). Traces of ispuri- tie left by evaporation of the benzene are singly carried forward in the vapour stream. Tbs flue gas mat* of course, be by-passed round the va porizer who the benzene flow is stepped. A coil should give over a year's service before needing repair. 91 DSW 462151 WATER PCB-SD0000045517 Equipment hist, eootd #6b By-Pasa Flu Drawing. 90-78*5-5. . On pr aversion unit, fitted with a dasher, ffo allow \ fits gases t by-pass the vapourleer as necessary. 92 #? LsM Trap Drawing 90-81*3-3. Ou par conversion unit. This 1* a centrifugal type separator for restoring any entrained lead. It Is a closed, welded vessel which Must be taken out at Inter" vals to allow any lead to he salted out. 0a boss of the Anniston waits., the lead trap Is a rela' tively snail steel Teasel, so placed that lead o&n drain back from it to the converter. In the newer units, the trap is larger and stands on a steel plate on the opera ting floor, which is nearly at the level cf the flanges of the lead pots. These traps take the form of flatbottomed cyclones 31 ~6R high, 2f-0* diameter, with a central pipe 6" diameter, for the gas exit , and the usual tangential inlet for gas, high up the side. It has been found best not to carry the central pipe more than about l*15 down inside the trap, otherwise its bottom end becomes choked too soon by lead and by solid debris (iron oxide, carbon, and shots of entrapped lead). In a trap, seen Jfov/50, the layer of entrained lead was 1*" deep, and there was considerable solid debris as tell. After the lead ted been melted out this vessel was cut open to permit the shortening cf the imer tube, and pportwilty tes taken to dig out the solid debris. yot oa By tying the Lead Trap The unit is shut down and allowed to cool a little, and noma diphenyl etc. may run back into the lead trap and ay take fire when the trap is opened. Each cyclone has a lifting hook welded on, opposite the gas inlet| this is for the yard crane; inside the shed the pot is lifted by a stirrup bolted to the central outlet flange. cyclone is lowered to the ground floor, picked up by the yard crane, and taken to a salt ing table in the scrap yard, and put on the table with the vapour islet downwards, (vessel oa its side), and flams of natural gag played oss the pot until the lead DSW 462152 WATER PCB-SD0000045518 (To follow p.ogo 92 ,,) Side view table, ctc. m%D FOR CLBAKXM THE LEAD TRAPS Scale V** I'-O' 6^.0et.x.sc. WATER PCB-SD0000045519 Equipment List, eontd #7 Lead Trap, eontd 93 mfl out on to the table and. down into a lead salting pot, tram which it can bo ra off at convenience into olds liJoa those used to ei^>ty the pots. The ml ting pot has a brick setting, and a proper gas burner, but the eyelon is boated iBply by open flames, confined aoaawhat by means of sheets of corrugated iron. The natural gas Ms a high oalorifie value, so tie salting is quick. The toIda aw the same as those used for esptying the lead pots, see page 39 above. goto oa Repairing Lead Trap & Colutm These units are exposed to the blast of hot vapours opposite the gas inlets (especially the lead trap since the introduction of orifice plates in the vapour pipes from the convertor), and they wear thin. The unit being shut down, and purged with COg* external patches can be welded m. A useful trick first is to weld a pipe nipple on the center of the patch and to leave it open as a vent until tbs patch is welded to the vessel, then to put in a screw plug. Such repairs are done with the vessels in their working positions, but filled with 002* The trap has to stand up to fairly heavy handling when being cleaned, apart from the high temperature during ser vice, and It should be of heavy plating. Stainless is not necessary, and thin stainless would be unsuitable. #8 Fractionating Golusps on Conversion toiti Drawing 90-8131-4* toe to each conversion tmit. Fhpour in at the bottom from lead trap #7. Benzene reflux in at the top from reflux box #12. Vapoa? out at the top to condenser #11. Underflow out at bottom via carbon, trap #9 to sua^) tanks #10. Thermo meter well at point of entry of reflux line to eoltnm, and one in the exit fro the carbon trap. , T2i@ eoluan has 12 plate, but the caps have been removed from the lowest 2 plates because they toeoaae choked with entrained lead, etc. The lead would, be above its welting point as it entered the eolisau The need for so many plates, for a cooperatively rough separation of benzene fro* diphenyl, Ms been questioned., but plant experience indicates son difficulty in maintaining a reasonably DSW462154 WATER PCB-SD0000045520 Equipment List, eontd #8 Fractionating Colmng on Conversion Uhlts, eontd low content of diphenyl in the distillate and of benzene in the tmder flow of the eoltnm. Preausably tbs plate efficiency is low because of the dilution by hydrogen and possibly there is fouling of the plate by carbon carried forward in the vapor stream. She plates have the usual drain holes to prevent block age by freezing* Design data were unavailable. Hay 14/48. fh erode diphenyl tanks are heat insulated, and any tea Jacketed lines outdoors * The colums have no heat insulation. Packed coltarns were used cm the earlier units, but they beease plugged with solid natter carried forward from the pots. 94 #9 Carboa Trap Drawing 90-8143 -3 Underflow in from ooluam. Side outlet at top to suaf> tank #10, with thermo well in the pipe bend. The outlet pipe goes down nearly to the ground level befor rising again to the susg> tanks, so forming a seal bend between the trap and the suag> tank. This seal bend and all the piping are ste&s jacketed, inner tub 2m diameter. These traps are removed from the unit for cleaning whennecessary, about every third month. An opportunity my occur when the unit is shut down for sons other purpose. The tesf>erature of the eoXtnsn trap is below the melting point of lead so tlmt the lead that settles her Is usually in finely divided solid particles. However, due to the nature of the infusible, highly carbonaceous organic materials that settle also, the lead is intermingled and agglomerated^-tot a solid mss. Thus it is necessary to burn and salt out Use trap to recover the lead. The proportion of carbon to lead Is greater in the "carbon" trap than in the "lead trap. Anniston report 1642 of Oct.lsAl states that this carbon trap needs cleaning every 3-6 months, and that, although it ha a bottom outlet plug, it 1ms to be taken out and leaned ^ burning. As seen at Anniston in Hovember 1950, these pots were simple vertleal steel cylinders about 3 r"0" deep by about 1'-6*r diameter with about a 9s flanged neck DSW 462155 WATER PCB-SD0000045521 95 #9 Parboo Trap, eotd to connof to the bottom of the eolism. The over also had mi inspection plug md two Wttng eyes to facilitate handling for mintenane. #10 Suqp Tanks for grade Biphenyl ' Horizontal, stool# insulated tanks. Underflow in, by gr&rity, from oltusn ^8 rl& earbon trap #9, Out by sub- mergod pp #104 to Diphenyl still #13. All liquor lines thoroughly mto&m jacketed. Teat to off-gas system. Stem* oil comofIcms. Tarec liquid depth Indicator. Test with explosion disc. lft. EUenburg, Msy 14A8, stated that these tanks are operated at about X25C to prerent crystallization. When seen in Borembay 1950 the rent pipes were quite hot to the touch. . #104 Submerged Pwm For transferring crude diphenyl frcaa ausp tank to diphenyl stills. On to each sub?) tank. Explosion proof motor. #11 Geodepeers oo Conversion Units Drawing 9C~955. (Me to each conrersion tmit. Tube and shell type, water through th tubes. Tapotn* is fro* colum #8 and conden sate out to Reflux Split Box #12, through a strainer with by-pa. Balancing line from top of Reflux Box #12 to condenser, with connection to hydrogen off-gas system. There is also in emergency rent to the atmosphere. 'tenistoa adrise against tho use of copper tubes, because of the sulphur iapurities in the benzene. They adrise making this condenser of a^le capacity. #12 Reflux Split Box, lowing 90-9055 DSVV 462156 Standard Botaweir, with light glasses and levelling screws. One to each oowersion unit. Forward flow returns via light glass to recycle feed tank #3. Sight glass in reflux Uae. Both lines haro deep seal beads, and there mist be sufficient head between the reflux box and the return inlet WATER PCB-SD0000045522 Equipment List, eoatd #13 Diphenyl Still rr&wlag 9C-8254, Two &r< installed. Horizontal, Insulated, steel-task. Subnargod pimp with water cooled bearings, and outlet to external gas-bested oil with bp&noh to crude Santomx receiver #20. Inlet fro #10 snap tank and "Heads and Tails* receiver #18. to me dished end is return line fro bottom of coltnm #14. Beturn line from beating ooil. Vapour outlet to bottom of ooltzm #3.4. 4 vent pipe, fro a branch on the vapour pipe to the column, carried up through tbs roof. This Tent pipe has a bursting disc between two flanges located about 6*-0 aboTe the vapour pipe. In one ease, the 6f length of pipe is jacketed (jacket espty), and in the other ease it is bare. Dsaedi&tely below the flange there is a theme well, with a therms couple giving a continuous record on the Multipoint temperature reoordar in the instrument roost. It is found that the disc# slowly become perforated, probably by sulphur eospounds, but even a sail perforation is detected by the tempera ture rise. The pipe above the flange is supported on rods with a tuna-buckle fitting by which the pipe can be lifted for easier replacement of the dise. The bursting discs are B.S.&B. dlies, type Al-Fb (lead on the concave surface) "Vinyl service . Bursting pressure 39 (in another case, 43) p.s.i.g., carried be tween two B.S.&B. type flanges. 96 #13B Heating toil nmwittgfj 90-88X1, 9C-8212. One for each still. Supported In a steel easing with firebrick lining. Oas fired. Liquid circulated by pu^p #X3A from and to still #13, Plow is countercurrent to fits gases. Half the casing hinges away on a steel track for access to the oil,. The circulating lines are steam Jacketed. Not, however, that if water is trapped in the Jackets and the hot diphenyl circulated, a very high pressure would develop in the Jackets. - DSW 462157 WATER PCB-SD0000045523 (To follow page 96) s-rty DSW-462158 SVXVKL BOX WATER PCB-SD0000045524 Equipment List, eoptd #2.4 Qoltgaa Braidng 90-7870. . 0s@ for aeh still. 20 plat# colum. Drain holm In plates. inlet at bottoa fro itiU #13* Be- flax return fro split box #16. Underflow from lottos task to still #13. Vhpour out to cmAmmer #15 via goos# nook. Anniston forserly used a packed colum, with a directfired still, but the results wore not so good ai with the present bubble cap colum, On May 12/49 Anniston expressed the opinion that the 20-plate colum, preposed by London Central Engineering Dept, wold be adequate. Special care is needed if tha reflux line to the still is not to frees. 97 #15 Condenser tewing 9C"9872. One per still. Horizontal tube and shell. Tbpour in fro top of eoltais #14. Condensate out to split box #16, Cooled by water through tubes, circulated in a closed system by ptrap #23 through heat exchanger ^2 with mke-xsp tank #24. #16 Reflux Split Boa: tewings 9C-8223 and 90-8224. . . 5 . Standard Rotaweir, with sight glasses, and levelling screws. One for aA tin. Condensate in from condenser #15. Reflux out to top of eoltnm via sight glass. Forward flew to bmxmm receiver #21 or through boa; #17 to re ceivers #18 and #19. Vent pipe* steaa Jacketed for occasional mlting out, (should have flasse arrester). The reflux ha should have steam tracing for use while th# diphenyl fraction is running. #17 Swivel Boxes for Switching Diphenyl Still Distillates tewing 90-7836 On* for each still. Condensate in free Reflux Split Box #16, and otrt, by muml adjustaant, t either ^Bm&a and Tails receiver #18, car Biphenyl receiver #19. DSW 462159 WATER PCB-SD0000045525 (To follov p&gs 97) WATER PCB-SD0000045526 Equipment Lilt, oontM fl8 *Hemda and fails* Receiver. Drawing 9C-812*. On Tor each still. Vertical teak with submerged puB?>. and mnhol. "Heads" or "Tail** fraction of distillate in free Swivel Split Flow Box #17* Steam ooil inlet and outlet. Submerged puzq? delivery line back to still. Vent lino with, lower portion steam Jacketed and carrying burst&g disc. . Inspection hole with loos hinged corer. Bottom outlet. #18a Submerged Pmp One per Heads and fails receiver. For transferring Heads and fails fraction to Stills #13. #19 Diphenyl Receiver Vertical tank fitted with submerged pusp #19A. Diphenyl fraction in from Swivel Split Flow Box #17. Finished product out via pu^> delivery line to Aroclor Plant, Store tank or Flaker. Vent with lower portion steam Jacketed and with - burgklqgj* disc, to'hole and cover. Handhole with loose hinged cover. Steam ooil inlet and outlet. #19A Submerged Ptm& On for each Diphenyl receiver #19 For transferr ing diphenyl to Arcelor Plant, Store f&nk or to Flaker, Explosion proof motor. #20 Crude g&atowax Receiver Drawing 90-7877. Vertical tank with submerged pus?* #2QA. Inlet from submerged pun> #13A of still. Crude Santowmx from outlet of submerged pum? #20 to #34B of Santowax Dis tillation Unit. Handhole and loos hinged cover. Banhol and cov*r. Steam coll inlet and outlet. ' Steam Jacketed vent and burs^tag disc. Crude Santowax to firusa through bottom outlet. Second atpam Jacketed vent with hand valve. DSW 462161 98 WATER PCB-SD0000045527 Equipment List, oontd #2<M Submerged Pa^> Oa for each crwio Santown recelvur, Pop transferring opttd Santotrax to #3^B S&ntowax still charging tank. 99 #21 Butter Storage g&ttk for recovered benzea. Vortical tank with manhole and went, Recovered benzene la frost reflux split box #16 and out to pun? #21A, Inlet and outlet for steam oil, Gauge glass. #2U reap Receiving recovered benzene from buffer storage tank, #21, end deliTerlng to recycle feed tank #3. Explosionproof aotor. #22 Saat Exchanger . Oa for each still Receives hot circulating water fro condenser #25 and delivers cooled water to pu^p #23, Cooling water through tubes. The circulating water is maintained at 30"4oQG during the benzene forerun, and about 8oC during the diphenyl * fraction, (by hand control oa the fresh cooling water through the tubes in each ease). Cocpere page $7. #23 *2Bt '. Oa for each still. Receives circulating water fro heat exchanger #22 and delivers to condensers #15. Explosion proof otor. #24 Make-iy Water Tank Cum for each still. Receives sake-up pond water as necessary to replenish water lost by evaporation oa cir culating through condenser #15, Bottom outlet to circu lating line. Overflew. Constant level device for eontrolling receipt of snake-up water. Condensed water would, of corn's, b better for this iskt-q?, DSW 462162 WATER PCB-SD0000045528 Equipment Lilt, anM 100 #2$ Cooler for ffidregen Savings 9C~8o0, Crlaooa Rtxasel 0o# HYB-2W36# Eaehtf th fora? parallel tmifes of the original cooler Ms been surrotmded by a water Jacket to Inereate th cooling surface. Receives hydrogen, for cooling, from a min serving all th converter suits# There la a rent with hand controlled valve connected to th hydrogen inlet via a benzene trap# Tha latter Is a small pot containing baffles aM drainlug to th surge tank #26. #26 Surge Tank for Rydrogen tewing 9C-8188 ' Receives eooled hydrogen and condensed benzene fro cooler #25 and benzene from the vent to the hydrogen cooler. Hydrogen delivered to inlet of compressor #29# Condensed benzene flows by gravity through hotto outlet to either of th two tanks #27# Fitted with 55" water eT*to provide pressure release if necessary. Water seal has a vent with flame arrestor. Line to instrument controlling pressure within limits of U*l6 os. Pressure gauge. Balancing line to benzene receivers #27. When the pressure drops to 11 or.. , the compressor low stage beoojses inoperative and only the high stage operates. When the pressure reaches 16 os both stages operate until the pressure falls again, to 11 oz. (per sq.ia.) * through the roof, #27 Benzene Receivers tewing 9C-81&5. On for each compressor. Receives condensed benzene from surg tank #26, feota low pressure tank #31, and high pressure tank #33 through sight glasses. Benzene out via bottom outlet to pimp #28. Balancing line to surge tank #26, Level gaugea #28 Ptnt> On for each compressor. Receiving condensed benzene fro benzene receiver #27 and delivering to recycle feed task #3. DSW 462163 WATER PCB-SD0000045529 gqtslpEisat List, oontd 101 #29 Two Stag Hydrogen Coapresaars Drawings 9C-6188, 90-7366, wiring and controls, revised version sent to Me*. Buis, J&n.l8/50. Two are installed. The first stag eonpresgee the hydro gen to 60#, and the second to 300# pressure. Provision for introducing 00g for purging purposes. The oppressors thesselvoa ar water cooled and there is a snail verti cal tubular condenser after each stage, draining to the corresponding pressure tanks, items #31 & #33* It. Hardy stated, Movaaber 17/48, that the eo^ressors haves 316 stainless shafts and valve discs. Unresist cylinder liners and valve cages, Goetz gasket, stainless steel or aluminum type, and tlmt copper and its alloy are mdesirabl. So copper or brass gaskets should be used, and generally copper and its alloys are avoided. Mr. Clegora, Hov/50, mentioned gaskets of Babbitt natal for the compressor Anniston were asked if un-lubricated cylinder with car bon rings would not be better, but they replied that finely divided oarbon, which Might cone over in the hydro gen stream, would abrade the earbon rings. Drawing 90-7366 showing the wiring and control system for a single eo^irei- sor, was sent to London, May 24/46. Th compressors are fed rather liberally with lubricating oil to cope with the possible condensation of benzene in th cylinders, but Anniston have not noticed any trouble fro* lubricating oil getting into the process stream. Mr, A. M. KllenbOTg, Jtmo 30/48, gave a general discus sion of the operation and control f tits compressors, incidentally giving 150 and 300 p.s.i.g. as the two pressures, but stated tlmt these values were not critical and. that the choice ttimed on considerations of cylinder size and quantity of gas to be handled. Progressive tmloading would be satisfactory as an alterna tive to the "trigger, cm & off" unloading control used at Anniston. Bj 1oy./50 th solenoid unloading controls had been replaced by pneumatically operated controls, partly for reasons of safety. Electrical switches would 61 any case be outside the coapressor room. The room is lUtsriimted by flood 1o^>b placed a few yards outside the window*. ncuu 462164 WATER PCB-SD0000045530 Equipment List, contd #30 Interstage Pooler On for each cos^ressor. Sluply consists of vertical, water -jacketed pipe between outlet fro first stag of ensressor and, islet to lev presaw tank #31, 0a and Taper in at the top fro* the compressor Condensate and ga out at the hottest to the low pressure tank. Ite* #31. 102 #31 Lev Pressure Teak ttwing 9G-8U38, Ota for each eomressor. Receives hydrogen at 60#, ria Interstage cooler #30 fros first stage of cospressor, and deliTers to second stage of compressor. Condensed benzene blown to benzene receiver #27. Bottom drain cock. Pressure gauge. Shs tank has a pop mire to opes at 100 p.s.i.g. and a bursting diecl(B,S&B. aluminium* with lead facing oattsa pressure sla*)-?--toLOpea at 150 p.s.I.g. Both these hare hooded rents well abov the roof of the eos?pressor room. She rent should be well away from the roof louvres of the conversion room* and the still furnace room. A connection* originally installed be tween item #31 and the gas inlet to the compressor, was removed. #32 Cooler Similar to #30* and cools the gas passing from outlet of second stage of the compressor to the high pressure tank #33. #33 High Pressure Tank Drawing 9C-8183. On for each eo^ressor. Receives hydrogen at 300# via cooler #33 fro second stage of coapressor and delivers to BB~4o department. Excess vented to atmosphere. Con densed benzene blown to condensed benzene receiver #27. Bottom drain cock. Pressure gauge. A connection, origi nally installed between Item #33 and item #31, with a reducing valve, ms removed. There is a spring-operated release valve to atmosphere, opening at 300 lb gauge pressure, also a pop valy to open WATER PCB-SD0000045531 gquipaent List, eontd . #33 High Pressure Tank,, ontd at 380 Us and a rupture 41s o to open at 580 lb. Anniston installed float type traps to discharge eondens@d beofien from the pressure tanks, items #31 & 33, but discarded to* because of leakage past the mire a. It is believed that traps made, for instance of 316 stain less steel, irito hardened Beatings, Might serve. At present, the bam:ss is discharged by means of handoperated valves, as described on page 44 above. 103 #34b Charging Tank for Santowax Still Vertical tank with submerged pusp #34D. #34b roceivea crude Santowax from crude Sailtowax receiver #20 via toe suboerged ptsp #2CM.. Return line from preheater #34c. Delivery of suimerged piap is to preheater or, for toe preheated Material, to toe still #35. There is an inter connection, low down on the side of toe tanks, between #3^A and #34b, also a 4" connection, about 8" froa the top for use in ease the bottom connection should be frozen at the start of the heating process. Inlet and outlet of heating coil. Manhole with hinged lid. #34a Charging Tank Similar to #34, but only* connections are toe intereatmcting line between the two. Vessel 34a sla^ply adds to to capacity provided by 34b, and it has no ` pxap of its owe. #34<J preheater A gas fired coil within a brick-lined steel easing. 0a side of firewall remote froa the still. Entry of erode s&ntotf&x froa to pin^p #342) is at the top of the ceil, and the flow is countercurrent to the flue gases. There are four gas burners. #34d guhaarged Pmy for circulation For circulation of erode S&ntowax through the Preheater #34c. Explosion proof motor. DSW 462166 WATER PCB-SD0000045532 Bm&pmnt Lint, atttd #35 Smt&mx Still Drawing* 90-S55Q 90-8551 90-6552 General Layouts, Earisoats! tank with 8Soj#pged pm%> to vxterml gaa heated oil #35A Preheated charge in. fro suhiaarged pwsp #3to of ekarg tank #3te* Return line fros th stm h@at#r #35A. Waderflew in from, column #36. Btlivery Ub from submerged ptxp #35B to th still heater, #35A, r, for still bottom, to the HS-%0 de partment or to feha pood, Yfepoop line to eolwm #36, with trer-sting disei Inlet and outlet for steam ooil, Th tn>eratnr spread la and. out of th Saatowax still oil is normally 15*-l8C on a Saatowax R distillation. Th pts^ ha a apaeity of 100 gpm and a 2" extra heavy pip is mod for the oil. 104 #35A Still Beater SiMlar to Preheater #34<J, hut is longer and 2b~s eight gas burner. G&s supply eontrolled to giro eorrect temperature spread between Islet and outlet of the coil. #35B Submerged Ptag For elrotdlatiag still barge through heater oils sad discharging bottoms to 'pend', iDeploiion proof motor. #35 Qolmm 12-plat eeltffla, 3 x 1/B drain holes in eaeh plate to pwmt b3,ok&g by freesiag. It is thought 1 x {' . hoi would be a better safeguard. Inlet for vapour at bottom fro* still #35# Inlet fro* reflux split box #38. Underflow from bottom took to still #35# fepour out to oodtusser #37 ' A melt simpler ooltsam sill serve if only Santow&x R is to be md. #37 Potsdameg DSW 462167 Single pip# in fora of wig-rag and Jacketed for water or taau Receive# vup* fro* top of ooltsm #35 and deliver* oodamoat to reflux iplit box #38# It is important to sure that water cannot be trapped in th jaiwfe m,TMA raised to a very high te^>erstre by th R*4^!%ssi.,5' rsnraa*. WATER PCB-SD0000045533 / BqtttPMeat List. eoatd 105 #37 Condenser, eeotd Actually; only * dribble of water la used, la parallel flew with ths vapour, and the water stream la so adjusted tim% the mfltsx split box fcespenature la around 200&C, (point #10 oo the Multipoint recorder) for Santowax R. Ail earlier condenser* of aboil and time design, using Aroelor as a eooling aediua, ms discarded la favour of this sinpler condenser, because of maintenance troubles. there ar no drawings, tout Mr. Hlenburg, Aug. 23/48, wrote the following description: "The inner tub is a standard 2* black iron pipe, Jacketed throughout its 45f of length by a 3" black Iron pip. -------toy extending a well-insulated 6" riser 8* above the top of the ooltnm, ire were able to get 45* of condenser to connect to the original location of the split box as follows: Four 10* lengths of pipe were doubled back on each other to girt a hair-pin shape condenser (a descending sig-e&g. E.K.), with a pitch of about 1" per foot. Vertical sections about 9s in length were used to connect the long sections. A final vertical section of 2' long connects the spilt flow box with the sig-zag part or the condenser. The inner pipe is Jacketed continuously to prevent any cold spots on the inner tube.------- - performance under the --- heviet load 2000 lb total condonsate/hr-- ---------Pop the ortho and Biota terphenyl fractions, where K3h lower otmdensate tesperattiros are per- atssibl-------the water rat oan to increased.--------It would b@ worth while to provide a blanked off connection for sailing the condensate even if a couplet (sailing; arrangement is not installed.R #36 Reflux Split Bex ' Standard types tout 00 reflux is used in the purification of crude Santowax to Ssatowax R. 39 Santowax B Receiver A vertical tank operating under a pressure of 50 m of erotsy absolute. Receives Santowax R from condenser #37 vis. #38 Inlet and outlet for steam coil. Connec tion to v&cwtm pun> #40, Bottom outlet to the buffer vessel, it* #39B. Vhlv for breaking vacuum. D3W 462168 WATER PCB-SD0000045534 Equjpiaeat List* oontd #39& Subnarged Puny la item #39S Delivers to the Arcelor plant* the S&ntowax R flatosr* or the BB4o plant as required. 106 #39B Saatowax Distillate Receiver Tfcrtlcal eyUndrleal rssl 5' x 5*,, Distillate In from. the receiver* ifcea #39* sad out by atabissrged pusp* It&m #39A. tforks under atnoepherie pressure, 3^s steaa soil.) #*0 T&etitn Pi^> Manufactured by be Tine. Between It# #39 end the Tectum ptasip, Amtlston have a subHast trap and a vacuum tank la the llAe|to allow settling of particles. Ho filter is esf>loyed because traces of terphenyl reaching the pta^j are either dissolved in the oil or discharged to atmosphere* and do no harm. DSW462169 WATER PCB-SD0000045535 Bgujpiagpt List, eoatd 107 laatrtgaentatioa 3m Erawing 9C"906o0 1. OoBToraioa Haiti . Each convertor wit has; (a) A L.&S, 'Mieromae5, recordingoatrolling instrument for the texjier&ttinf of th convertor pot, which operates by controlling the gas supply to th pot* This ssws Instrument, still responding to the thensooctroi ob th convertor, also controls th gas supply to #2 preheater* If automtie control should lead to towards a drop In teaper&tur of the #2 preheater, then this Is corrected her turning down burners on the converter. (h) A Poxboro "On-Off" type potentiometer tellertra*e controller for the $2 preheater to prevent the tem perature of this pot fro getting too high. All pilot lines are taken fro the gas line to th #1 preheater, which only Ms manual control of the supply. She Fcaboro controller is a safety device which will work if the converter control does not operate. The converter control should out the gas off on both Ho. 2 pot and the convertor pot if th temperature gets too high In the convertor, hut If the control fails tbs Poxboro cuts off the gas in Ho.2 pot. There Is no definite limit on this control, hut it operates at approxImt% 7^0e, (e) A L.&H. fHieroMx' 12-point recording instrument for temperatures at the following points; l*l Fhpour from outer vapotn*iser coil to #1 preheater, l2 Ffcpour from inner vapouriser coil to #1 preheater. #3 P&pewr fro #1 preheater. #4 Yapota? from #2 preheater. Wpour fro* convertor. #6 #2 preheater lead. #7 top of ooXttMB, #o condenser water outflow #9 flu gas to vapouriser dsw 462170 #10 flue gas fro vapouriser. #11 #1 preheater lead. #12 u^> line froa oolum, The points for units #4 and #5 have not `been detailed her# -- they are two-pot units of a different and lees satisfactory design, . WATER PCB-SD0000045536 Equipment List, ontd A * Qonreratda XMl'ts ooatd (d) A FoxPro flow controller for the benzene supply to &eh tmit, activated by an rifle in the fe@d Ha, Peibero Pneuaatic Pressure Tmaenltters ter beea installed. In j^oresber 1950 tixes were installed, with am spar, la a separate room which contained also the asters for the fuel g&s, and which ted a eoamrunicatiag door to the control rooa where moat of the otter instruments wore located. These indicate the now ate also transmit the ori fice press wes to the control instrxnsent. There are also located, within the Control Hoc, tend valves ate pressure gauges for each benzol line. See also page 31 shore. B Off-gas Treatment (a) A testers,ture indicating instrusent responding to thermocouples at the following points on the Hydro gen, cooler (1) Hydrogen in. (2 points). f 2) Hydrogen oat (4 points). (3) Cooling water out (4 points). (b) A e cmtrailer responding to pressure changes at the hydrogen surge tank #26 and controlling solenoid (store recently pneumatic) operated valves on the com pressors so as to mintain this pressure within the limit of 10-16 os. per &q,in. Rubber fittings must not be usal^wlaer8b exposed to the process gas.,because of the swelling which would be caused by the benzene in fete gas, 108 C. Diphenyl StUla Each stm teas (a) A L,& H. 'Mierosaax' controller similar to ttet used on the oonrertor pot, but controlling, via tte gas supply, the spread of temperature between inlet ate outlet to fete heating Coil. (b) A L.& 1, 'Microsax' multipoint recording instrument for t^peratures of #1 stiU Body, #2 Coil Inlet, this will be about the saa a point #1. #3 Outlet circulating line, #5 Top of ooluan. #5 Reflux to eotest. nsw462i7i u #6 s^otesnser Mater. J_f tpa> circulating pump should stop4 the gas stqpply to WATER PCB-SD0000045537 Byajpg-ent JAnte eoatd 109 D. Saatowo: Still (a) A L0&He fMier,oxr Controller #ieXar te that used on the eomortoF pot, but controlling, ria the gas apply tha 1 spreadf of te^emture between Inlet and outlet to the heating eoil. (fe) A 1-5? 1* `ffiapom1 multipoint recording instmswnt for fcaaperattspe oft Still body. Heater inlet. Beater outlet. Vapour leafing eolu. Top inside of eolum. Sight glass at reoeiirer, Bofctoa inside of eoltnm. Condensate In flow box. Preheater inlet. Preheater outlet * Specisas eharts fro most of these instrusents were sent to Cooper, London, in October 19^7* Anniston suggest using^glass wool trap, about 1 pint else, to protect instrument Hues from blockage by diphenyl ete, and using glycerin trap to protest Instruments operating on benzene serriee. DSW 462172 WATER PCB-SD0000045538 POST OF BQPXPMHgy Amlutem rfeimto for the instsllafelon of 3 diphenyl units (#32, IS, & 13), ,Jto 26/47, ms given oa p&g 58 of th re port hy l&vorcroffe & Bather*, September 19^7, and Is not repeated ter, nor aw ths installed oat tlmmea for otter parts of th@ plant irtileh mm glrm on page >8s, of that rtpcrt 110 DSW 462173 WATER PCB-SD0000045539 OOHMEBTS Off THE FH0CIS5 111 3m "Earlier Reports" listed on page 2 above, and ^Hbte cm Choice f Process" a page 6 abo?i gffect of 'ftoiatleti la Benzene Qtaalifer See also aoti on hmzmm under "Specifications & Teat Method*, peg 54 &tY9. Isnlatoa report 1$42, Oct,15/41* states that, at that tins, brasem with a distillation rang of 79*4 to 8l&0 ms used, bat that the freezing point had to be 50C Minima. Traces of toluene caused tbs fcrasatloa of styrene etc. which aecusmlsted in th "heeds" fraction of th diphenyl distillatibo. The amunt of this me only about 0.055$ of the diphenyl ude. Aliphatic i^niritles ww United in amount by th 50 specification, Th Material ooatained 0.06 to 0.08$' total sulphur, but this ms not thought to earn any operating difficulty, and sulphur ms found, to daisy the formation of carbon on the setal sur faces f th pots. Experimental work indicated that water in th benzene favoured the formation of carbon. (Excessive amounts. If praped into the vapourizer, my eauae a violent development of stea, endangering the Joints of the equipment.) Th report refers to work by F.E.Hubbard & R.A.Ewing, Spt.l?/4l, showing that fresh benzene gives 1.5 to 1.8$ more conversion per pass than does recycled benzene, and other reports mention eve greater differences. See for examples pages 112 & 123 below. This effect night be explained in one of the following way t (1) The fresh benzene my contain boss material which pro fits the reaction. * (2) The recycled benzene my contain sons material which SnhiMta th reaction. (3) The recycled benzene my contain sows Material which destroys an Inhibitor which is present in the fresh benzene. - Explanation (3) seems to b ruled out by the observation that in ordinary routine working, with about 80$ recycled benzene, and about 20$ fresh, tbs conversion goes quit well. As between (l) & (2) it is argued that boss grades of fresh benzene show even higher conversion rates and it has been shown by experiment that th addition of certain ehmsioals does actually speed if) th conversion. DSW 462174 WATER PCB-SD0000045540 Cotate ca the Process, ooaW Effects of ''Proaotors" in Season 112 Th report by Goaorer cited a pag 3 abor giro th follow lug remits in a laboratory unit. Pronetor Added sr~ Ion (recycled boas to) Sou (fresh benxoa) Acetic Acid Ethyl Alcohol Ethyl Ether a. Butyl Alcohol sec. Butyl Aleohol iso* Butyl Aleohol Acetone j* Conversion at 600C proSuot) 10 14.5 23.0 24.0 24.5 26.0 26.5 27.5 30.8 Effect of Sise of Bos 2.0^ Iex Propyl Aleohol 1.0 " * " 0.5 * ' " 0.2 " 0.15 * * 0.1 * " 0.0 * * * Conversion @ 750C 17.6 17.0 17.1 16.0 12.7 10.8 6.3 DSW 462175 WATER PCB-SD0000045541 Co--eats on the process, eontd ' Effect of "Prcaaetorg81 la Beozeagj, emtd U3 Promoters ter not been used at Amia ton In manufacturing work. Conorr*' a report reeoassonda that If the us of promo ter* Is routine manufacture is planned, a trial batch ought first to be carried right through to Aroolora, to mk sure the product does not contain any detrimental by-products. If ths plant is charged with fresh hmzem the conversion figure for the standard conditions will bo about 24$, but this figure will fall as the unchanged benzene is recycled, and at the end of the day my be as low as 10$. The incoming benzen, though of very high purity, appears to contain enough of an unidentified promoter to hare a narked effect on, tha rate of conversion. Tim falling off in the confersioa rate would naturally be very inconvenient in routine wtnuf&eture, so the feed of fresh benzene is made practically continuously into the re cycled benzene tank, so that there is always about 20$ of fresh benzene in the feed to the vapourizers. The reports lust quoted discuss the confers Ion reaction in isteh greater detail. Impurities likely to occur in the fresh benzene are toluene, paraffins, cyclop&reffins, and similar products, boiling arotmd B0C. pyrolysis of benzene which is contaminated with these will give diphenyl which is likely to be eontasamated with a variety of products, and unless these contamitents are removed before the diphenyl is chlorinated to give Aroclors, the Aro- clors *ade from toe diphenyl are liable to be contaminated frith Chios* cospounds in which toe chlorine is more labile than i.true Aroclors. Consequently the contaminated Areolar my be reacted on toe very stringent tests imposed by sew electrical users of ArocloWe . Tim Diphenyl mde by MCLls to be used to mice Aroclors, and Mr. f 6. Crane, Oet.lf/47, estimated that about half the Arc elor production would b as 1254 for electrical uses, so to question of stability of the Aroclors is of importance to MGL. Apparently, however, toe trouble has been limited to *PyranolsM, mixtures of Aroclors with trichlorbenzene, and it is to tri chlorbenzene which has been minly at fault. Mr. EHenburg suggested that more intensive fractionation of the diphenyl might eospeasat for to use of inferior benzene. Xr a^dy, Dc.23A7# stated that benzene contaMmted with paraffins, would yield styrene and apparently vinyl biphenyls, and that these product, on chlorination, would yield waterials DSW 462176 WATER PCB-SD0000045542 Qonosats oa th process, eootd 11* Effect of *Prootors* la Benzene, coatd liable to cause skin troubles. The chlorinated products Might b stabilised by being held at high teaperatures, hut it ms not certain that the stabilization would go far enough* Toluene a pyrolysis is said to give some styrene, and it was believed at eta tin at Anniston that chlorine derivatives of styrene were causing skin troubles aaong the workers In the Aroeler plant* See page 16 ahoy. Ua a letter dated April 2l/k9t Mr. Ellenburg listed alkylated benzenes and alkylated biphenyls as possible by-products from the used isfpur benzene, and he stated that styrene and stilbene hay been Identified In the "heads* fraction of the diphenyl still. Benzene homolegues on pyrolysis give also dibenzyl or derivetires (H.Szwarc, "Bature", Sept.20AT). Effect of Variation in Time-Tenperature of Exposure The process is normally run with th lead la the 3rd pot at not above 840C and with a benzene flow rate of 170 IT.S,Gal/hr., these eeditions faring about 18& conversion of the benzene into diphenyl, terphenyls etc* The retention time correspon ding to the given, flow rat, naturally depends on the pressures at which the pots are operated. As the process is carried on day after day, the y&petir passages become more and more restric ted by tha deposition of carbon in then, and this raise the pressure in th pots, md therefore the retention time increases. Also, orifice plate restrictions are being tried in th exits frcei tha 3rd pots. When the pressures increase, from either cause, the practice i* to reduce the teaperatures enough to Maintain th sane conversion figure of about 18^. Increasing pressures also give less eotrainssent of lead because of the lower linear velocity of the vapours, and the lower tempera tures should reduce th corrosion of the pots, but Amiston experience is showing that these advantages nay be dearly . bought, at tha aoat of increased Maintenance of th pot covers, gaskets, etc. See also under "Process la Detail8, page 3^ above. DSW 462177 WATER PCB-SD0000045543 Qowteota on the Process, contd 115 Bffect of Variation la Tima-reaperajure of Exposure, ocmM Aanlstcsa report 1642 of Oet.lsAl gives the following state amt of the effect of variation la pot te^ereturen Yaap. of lead la 1st pr@- bs&ter of load In 2nd preheater Tea of 1mA In convertor ^ Denversloa to crude diphenyl #9udt 580 TOO 50 50 580 580 725 725 720 775 BOO 800 840 840 840 825 825 800 Carton formation becoaes excessive above 84oC. 18 20 18.0 to 19.0 17.7 to 17.9 21.1 to 21.9 17.9 to 19.3 The effect of mrlafelon la pressure in the lead pets ms studied ,by Conover & Hoff of Plant ^A*, see report Oct.5/35* At &00G under certain conditions they obtained S,,2^Tconversion at 5 pole, end l4.4jg at 38 p&ig. It is stated that ratio of terphenyls to benzene in the reac tion product is about the sane as the ratio of diphenyl to teazea. At 1&& conversion, the ratio of diphenyl to terphenyls, etc., (high boilers) is about 4.5 to 1, and the amount of e&rboa formation is not too serious, but if the % conversion is pushed beyond 18^, the ratio of hlghbollera to diphenyl In creases 3also the ratio of carbon to diphenyl, so 1856 appears to be about the conoslo balance for American conditions, even though Amistoo cannot sell or use the whole output of high boilers. See ^Design lata for 4th Unit,R Aug.9/39/ for a curve of eats v. % conversion. Raising the pet tem>erature gives an increase in output of di phenyl with relatively little increase in the oonsunption of fuel gas and at times small variations in conversion rate have been mde at Amiston to get a greater output of diphenyl, at the cost of a higher proportion of wastage as hlghbollers. Anniston report 1642 cites & report by Margin, Beald & Perry, J&y I5/3I, indicating that if Mghboilers are recycled in the benzene, the amount of SB In the crude diphenyl Is not increased, but that it 1ms a higher boiling range, Anniston experience up to Sevenft>er/50 indicates that recycling of diphenyl in the tenses increases the amount of carbon formation. DsW 462178 WATER PCB-SD0000045544 Q&smsnt cm the Process, eonfed 116 fh benzene distillate from the diphenyl still is examined be fore being recycled to the cam-era ion stage, xt usually contains Tory little diphenyl, but if it contained store than about 3$ it would be fed back grsdmlly, or in an extreme ease, returned to the heads * tan* tank for rediitillation. It ms stated in September 1947 that conversion was reaching 13$ in the second preheater and 10$ in the convertor. The extent to which the reaction proceed in each of the 3 pots, naturally depends on the conditions of tes5>erature and pressure in each pot. Anniston report 1642 gives the follow ing figures for vapour leaving tbs second preheater: 2nd preheater lead tengeratur $ conversion 64oC 720-725C 7750 1.0 4,0 to 5.0 10.0 Distillation of the Crude Diphenyl , Ifcr-produots, which boil between benzene and diphenyl, build tip, only very slowly, in the continuous recycling of the "heads" fraction, and it is not difficult to run the fractionation so as to give diphenyl of the necessary quality. Ifr.EHehburg, May 12, 1949# stated that about 0,1$ to 0,2$ of the diphenyl yield was side-tracked in the form of the odl from the "heads" fraction. Amis ton report 1642 gives 0,065$ on the diphenyl as the amount of styrene, etc. formed. Wriatioa in the diphenyl distillation condition might also go soso way to offset the effects of i^tffities in the benzene used, see pages 55 & 113 above. geaxeae recovery from the grdrogea Amis ton reported moderately good result from scrubbing the hydrogen with mineral oil. An activated alumina absorber ms in stalled at Anniston, to take up benzene from the hydrogen, but it gave poor result and was discarded in favour of the presaat eauf>r@gioa system. It Is thought that the alumina ms not pro perly re-activated. See Anniston reports 214, Sept. 22/33# * 948, Aug. 21/35. Since there is a use for the compressed hydrogen, the eagresion system appears to be the best for Anniston conditions. Originally the hydrogen at Anniston ms piped to a gas min and burned, with natural gas, tinder th units, but difficulties in keeping the correct air-gas ratio in the burners soon caused a dxseontismtiao of this use of hydrogen. DSW 4S2179 WATER PCB-SD0000045545 COST MTA Xahotg Requireasat . At Anniston la Ibreiber 1950, one operator per shift'eould look after ^ to 5 trrersioa unit and on diphenyl still* ZD addition* there was om ehlef operator per shift, (but his r#sp<mslhUti@s Included Aroolor & HB-40,) and there was a general day foreman. (Carry), covering a mmbar of departMats, including Aroolor. Hr* fSUeaburg wrote Aug,l8/483about the breakdown of the various sarrl barges among tbs different products i Diphenyl Crude Diphenyl Distilled Steam, Ibe City water, eu.ft. Recovered water, eu.ft. Gas, eu.ft. Electricity KHH 0.10 0.037 0.49' 13.5 0.050 0,91 ---- 4.4o 2.2 0.008 The tmita are given per pound of product -- for JUne/48, and he eoraeats that there are seasonal variations in such figures. U7 Repair tfork The pr&ctlee sheets, pages 120 & 121 below, give a record of the frequency of various repair jobs. DSVV 462180 WATER PCB-SD0000045546 118 fC-OS/T>I raAfl TO Yi ^-H/- "j "7 0f /K'1^'. / "f/1 \ar t *i( ' fi4 ( j s. ^jJL. *tq9\J /f<r AafJtB~Lce) '7*fT f D '7*7 tvm. es f fc/r *7 M *-o 4f M *rf 3***-i > *-t o DSW 462181 1X wo ft 1 * **t 71 IX / A* 4 r7 > ru / 47 47 re 7*- 773 iO < >--* *4*/ 4> 041f*f. 11. // *M t K < ( | to f1 744* I41t 7* t* w*o K t?1 1C t N If l At * TX **T* v 1? X OT? rs /f/ 07 m7 tr / / 0r 1*ft Cl 7/ ir7 / Hi 1 rt >-7 7f u-* IS *** ie "V t>S *1 - a>( 47 /& ef /' > rr 'J XJ fO *# x '` 7xf -- - if* t 74 (X tn /! m 19 t.1 1t%jf O44f a -H -- 1xar/? .*/ T7 . M 01 - v-g 3 4 >*^13 * 04 > 9-10 . 0 &! 1 ru 47/ xom Aim J77 vrj ^T o<v 4<s /'*/ ,, v m 4 14 f ' -a^e 0(W *7 07/ o0 O/ Jtf wj." ' H7 ' 3-rT wt Off r>r t+T t?T `->*7 UO/ 'OOf ">& a of or *. ir A/f "0 ft* OCX,. * 00/ * 4 1 XttfX _ >oa 7f *f7 1*1.f *'7S 7W X> 4-**+ * 07/ *07f '*T f fc. 7 * 14/ ,Vfc Of-- *i=r fW OiT JtJ) 04 f r3X -<7 3' f *iT> *a |<ft 1 as #n (|*n * ; >' > 4 4 r>f. ] 9 H* I r- >70 * nn t* f/#i ^ C*4oWf7* . * *rf *9* 1 /*% WATER PCB-SD0000045547 R 7/ ftfa-f gWmUfTO CMMKUi. COMPAHr COST WWT >- /ia/________ *A TO feATY_______7/<fr /01 .&C * ( 4m&.(( a tr** *^jJU Av A)-*. ?f7- ) 4 4r A- A , COAX. Q w. ^ ruo^-C A * i DSW 462182 prsAW KITT rvL--a4 coax. ft< I V I 3^ *T <TC 1 7 3-T 14 Of vT VI Tt <0 U * r fli - Tf SI 7*4*.t <3/ W X"7 i) 7Xr s* /-*- 07 f ST *3 Aft < -*# *-s Xf * .f / ST * 3 57 u T f 17 50 i. f 7 <Om / - *5 4/ r -f > *7 17A. >c 7 on **S 002 Oil iei 7f"b 7< t >--D <9* 0 */ o/V 30 4 'JO| 0 t 3 ( 1.1 -p*5 OV2 ^('r ** 3 ' Tf^ Ou u r >5 "*/ ij.1 ou 7 X4 1>7> p.>| r >r rU .M ?rt 'ill O' l TW afc7 j o7 oit O^i (V TO S >MI Of w>_i*. J"v ^V( 4.1 Vr 7? - J.*f 7< <?f Wi - % "3 ~<TJ . TV "1*0 tf 07 --7 f * >7 1X4 -wf (vV /5T iS 5t Of - r XO ~T 051 1 f (0+ " V " W* '*f " . .*7* J . **a .71 . - . < ** ,&t , ~ -i/i >7 . /2^8 , ' Y'J # bTf . < rj . 1 00 ^ M47 4*7 4 i 1 00 4 I S WATER PCB-SD0000045548 i 1 .: ; 4 '1' ,'' mm 1 1 : _ - .lJL.it 1 " M&.M l '* nsnsr GollJs* 11--asi.srmS !-------- ^ : 171, Kd 3aJm> n.^6 #.m t1 i >r I*. teenilty ' i.<m . fl.on 99Q.0C0 20,000 f 5.2*7 5,000,000 10.446 Ur55ff^000 i o.cm6 i ' Lbs. M.fi. 'B Ham ficxtri ------------ <sr 1.212 ~1.UJ 78? *.552 11.7*0 J05 5i ^ ' V,' t -. * *|'- . PfodvtltttZ -* ^ Mil . Fourda T.Air5ir ^ H Q*. Qxlt la,r . 6rU^*t 0 ' '* 5fT Wkwb " x.%7rkm S5i So Mfc *9*r i mIS UL71 fia* ifatriale 0*& HwkjI - Arteal # 3aptlel " Um _ * * " Jwwi Qallsjm ...JVr U. . 0.1795. U95r< 0.1695 _ 75.890 0.9446 Chcrto-- . - B6e* - 14*. 7,9t7o6a,.cQtOltQTr^Pewr Lb r Waffr~Cltj-Cu, Ft. 115.000 .019 Wetw-fiooof'4-Cn. Ft. 58,105,000 5.oe6 Qas - Cu. Ft. 54,991,000 - 17.666 KLertSieitr -XHH '415^000 .054 Trmk - _lmn &->S Otwretlnr MoioUsucoo* i 'U u.'wF3 ~J^6E6'~ 7.672 99? Psafctn 5.594 Shltmlaa 189 24.140 100.0 05 99,57 0.7 1 2 1 1 1 1 1 Obit-flours 6.696 --------- *52 6.602 Oprstlnr Tina Bourn - Calmd/tr Unit Bout IfraP A &xir* - Shut Dobb 5.464 aburs-te-oo* Orratd 49.024 Hour* - Delar 508 Houm-ffo-t Owrsted 48.516 WU.ru i of Grwws Open Osiers i Cl* so CoooenBOlai fLar( at n Clwn Gooaoawsis (Baali 7 Clssn Distributor 2 CLmb Carton 5Vsp 9 Clsso Ld Trap fl ClMCD Onlum Cleexi TaiKadsar Coi l1 ? Qumfla DLrtrfcfeutnr Oat'r. 12 CKsncn* TufMadL Pat* 1 QutoOB LM Ttwi 4 Chann Thansnarmpl* ChBnxp Tharo-Un 5 t- 6.60 95.40 92.45 1.04 .. "1 1 1 Chanc PreMur* Cu*^im R^jAiT IUUami Tim KI#silltsnw 14 CL* #1 B Mat. SbiMlIi- So&saslr 2 ft*!** Testfarl ttw 0*11 Slams. HD ln( d* twi T-inmaa Qua #8 TW Mat. 1 1 P 4 ________ 1_ Oumfa M Pst, f& . I 1 *WLii- Oemm. tosi ^. ------------ ------ sxmu'ii RCPCRC Page - 1 4e?us WATER PCB-SD0000045549 EUaaburg, totarj 20/kSe gare th following break down of th fuel gas eons motions Areolar Distillation 0*66 Biphenyl - Grad Units 16*7 Biphenyl - Distillation 2*2 Saafcotmx R Distillation 1*5 Calorific value of th gas about 1040 Bth,F./eu,ft. at 60F and atBospherie pressure* 0SW 462184 WATER PCB-SD0000045550 ir--sqpS|P@| hrjKH r-JSOb-*9 --Tg5i^a-8FMrg r"--i ^- nuni 1 _ y*> am ' 'SUX^iS^BtWrObfUCZg W ~mqXFOauxfttr^' '.. . ri ,J ' * jm.m , *"7*5 .. * - ' % .. fMtmm V. .. - ;>. . ^nEsr PfiSsh^sixT^ V* V fY;** . - ^v' ' ~5obtsaasm ~i=T?o*ufir i 58l.O<0 .*s-,o 8 3XJMB . - .... <9. - ZpTTMI .XttJttsal MW '*'.. a si.(m nssnsiiFiM 1 *9%OS5 tm t 1 m --gTM^'~n^^ytas>w~:------- it 3 _... *r "TSJSSpB" S'<HL< Fltr# Ifeni'tSM 1 * " ~D*0&'ag4s '~K^'lran't!nm=VSX' " " *^PMnerci is --i^BiRW * " -Etestea^stf- ~tejwp lUsarB^t^ " * .-Ussrapefea . { *2n< m 121 l ' j .. . . J . i 1I I 6-1300 -a ^----- . fe .. .._ . _ . _ ._ ..._ . . _ . _ mwnasrt. was 6-U ta a DSW 462185 WATER_PCB-SD0000045551 122 A OS MO E DO ME IT This report Is snalnly a coopnation, of infermtlcm fimw frca Anniston reports awl froa discussions and, correspondence with max members of the Annis ton staff* whose willing and able help is grate fully resaeaJberM The reports ssade by Messrs Eavercroft & Mather, September 19^7* haw been incorporated* also that of lte% H. L. Harden* August 1950* and obserrations made bj the author during wisits to Anal*ten. DSW 4S2186 WATER PCB-SD0000045552 Index page 1 ion (Oadwlined figures denote tbe sore l^ortant entry under any one subject) ACSSOHLEEOM2HT...................................................................... 122 AluHlna absorber oa hydrogen (abandoned). *.................. Xi6 Aroclor, electrical standard required ....... 55,113 EEHZEHE, catalyst in, see "Benzene, effect of catalyst8 danger fro overpraping into feed tank . ... 30 danger from water in . . ..................... .... 29,83 discharge fro Hp pressure vessels .... 44, 103 effect of catalyst in ....................................5i29-,lll- effect of isfjurities in ...... -3,16,55,111- effect of premotor* in............................ .335" effect c sulphur in. ........... .Ill effect of water in, see "Bensene, water in" feed arrangements. ....................................29-,83 see also leader "Instruments* feed rate. .............. ... 31 feed rate during starting tg> . ... 37 filters............................................................... 30,31,65 handling ......... .................. . . 29-, 83 leakage into flues, method of detection described. * . . . ... 91 mentioned. . . . . 32,36,76 losses in the hydrogen stream, Anniston report mentioned ..... 3 physical properties of .................................... .... .10,U puaps. ............................................................................ 83,84 quality, effect of on Aroclor workers. . . 16,114 qmlity of, suggestion to do better frac tionation. of diphenyl to com pensate for poorer benzene 55,113,116 receiver froai diphenyl still....................... .... 99 recovery fro off gas, see under "aydrogen" recycled, reacts more slowly, see "Benzene, effect of catalyst8 recycled froa diphenyl still, examined , . .47,76 recycle feed tank, .......... . , .29,83 recycling.................................................................5, 29", HI recycling should be fairly imlfor* ...... 30 risk of flooding convertor with. ...... 30 DSW 462187 WATER PCB-SD0000045553 Benzon, specifications and test sethods, store tanka............................................... store tacks, fire arrangements , store tanka, objections to internal colls In........................... sulphur In ,........................... test records ................ ...... trap failure in Hg tryst*.. , , . , trapping of water fro....................... water in, dangers from ...... effects of . ...................... sources of ...... . Buildings ..... .................. ....... see also under "Ventilation" Bursting discs, on diphenyl stills. . . . . , on Ep ressels ........ By-Pas flue, see under "Vapourlzer* Index P 2 ... 84 . .54,111 ... 5^ 44-103 0 02985 . .29,83 29,112 ...... 29 82 , .18,96 18,102,193 CABBOH, build-up, bursting pressure of........................... . . 89 build-up, favoured by presence of water . . .111 build-Tap, favoured fay recycling diphenyl. . . .115 build-tip, in the conversion system. . . . . 34,114. burning out from pots and pipes ...... . . 41 detection of blockages. . . . , ....................... . . 41 dioxide, connection to convertor, . . . . . .19,31 dioxide, handling ............. .31,3| dioxide, not used in diphenyl still . . . .18,48 dioxide, suggested use to remove carbon .. . . . 4l dioxide, use in checking conversion system, . . 3T intentional addition to lead pots suggested . . 22 precautions in burning out (damage to equipment). . . . 41 (risk of poisoning by lead vapour) ........... ::Ssuggested removal by C02. ......... tetrachloride in fir prevention....................... trap, cleaning of ............ . trap, description of........................... . . 94 trap, operation of. ...... ..................... . . *3 Catalyst in fresh benzene, see under "Benzene, catalyst in" Charts, se# under "instruments* Chlorination of diphenyl, Mentioned ........ . . 7 see also under "Arcelor* Ghlarlmtlm of Simtmmx Cblce*ine, determination, of, in Sant wax Choice of process . ......................................... Column on convertor, arrangement of . . convertor, choking of , convertor, efficiency of. . . DSW 462188 WATER PCB-SD0000045554 Index pag 3 Colism on eoawtor, operation of,.................. osvertor, packed coIuess maultable, 9? eovertor> repair* of ............................... diphenyl still Santowax atUl 93 $ Concents cm procMi,..................................................... m Coapreisors, see xm^sr "l^drogeja, cmpressor Condenser cm conversion units, description of operation of , tm diphenyl stills, description of. ................. ^7 Operation of, , cm Santowax still Control tests. .43,*7,Z,ll6 Conversion pots, baffles........................................... ::::: gbaffles, sagging of .... . e&uses of failure of , , , . .... 41 corer ..................... . .41,42,86- covers, holts of, cut,in. . repair work . 88 covers. Joints, see under "Gaskets1' covers, warping of . ....................... cracking of well between pot 4 ri* depth of lead In ........ description of................. .... design of dip-pipes ....... 86 emptying of ... . ........................... 39 equalising lines on . ....................... flue arrangements ........ leakage of lead or vapour from, detection of .... . maintenance of...................... .... moving without emptying ..... / operation of .......... overheating of upper walls. . . . pressure gauges, see tmder "Equalizing line19 also ....... . 42 pressures In .......... repairing ............ rins thickened. ......... ..n 88 rim welds cracking . ........................... 41,88 rotation of between different settings.............................. setting of.................................. .... . 42 33,8 see also,"Conversion Pot, flue arrangement " starting of .......... . 37 stopping of . . .............................. . . .3 tonperatures of ... ...................... 33,34,51 tesspenature control methods , . , . . .107 nSW 462189 WATER PCB-SD0000045555 Index page 4 Conversion pots, temperature controllers.................. , ,34-,107 to be free fro* casings. ,............................"BET vibration of. See 'Vibration Conversion process, adjustment of teng>erature to eoapensafce for prosatire varia tions . See "Pressure increases, eospensatian for* degree of eon.vers ion in each f the 3 pots * 126 description of . .......................,,...32 effect of variables in ...... . .111" two pot system Mentioned .... 32,82,85 Conversion test, details of 75 mentioned ............... 43 Cooling fans, ............................... .19,20 Copper and alloys, failure of in Eg system, . , 24,44,101,103 not recoasaended for condensers .................. ...... 95 Corrosion, effect of impurities in lead feared..........................57 general note .......... ....................... . 22" of convertor pots...................... 4l of oarertor pots by lead blast (Anrfeton report). .......... 3 try stainless steel for traps in Eg system . . 103 Cost of equipment .................................................................. ................. 110 Cost of manufacture............................. 117- aanufacture, practice sheets, ......... ,120- manufacture, versus $ conversion. ....... ,115 Cost sheet, diphenyl. ......................................................... .118 Cost sheet, Santov&x R................................ .119 Crude diphenyl, analysis method for ........... 7 composition of, see "Plot# SheetH tanks, description of .......... 95 Crude Sanfcomx, see "Santowz, Crude" 2S32BH MIA BOOKS (Anniston), listed........................... .... . .3,4 Design data book, (London) discussed by Anniston staff. . .4 Diphenyl distillation, eootaenta on. .......... .116 control tests.................. .... . ,47,76,116 out point.................. .... . 45,46,$?, U6 cut points, variation of suggested to cotton- sat for poor benzene . . .55*113*116 description of.........................................45" fire hazard in....'.... *.17 heads fraction, saotmt eliminated ..... *28,48,116 refits ratios 45*47,52 Diphenyl, MOL do not expect to sell.................................... .... .7*48 physical properties of .................................... .... . 11,12 specifications and test methods................................58 DSVV 462190 WATER PCB-SD0000045556 Index page 5 Diphenyl still, benzene receiver of, described, , . . bottom, see "(Sru&e Santowax" 99 bursting dlso on..........................., . . . . 96 eolum, so under "Colusmi" condenser described condenser, indirect, cooling of , . . 47, % condenser, tei?> control of ..... . condenser, heat exchanger on nater of...................... condenser, crude Santowax receiver. , . description of .................................................. diphenyl receiver ...... ................... distillate switch box ......... formerly dlreot fired..................................... heads & tails receiver............................ heat cut off If ptcaf) fails. ...... . 108 heat exchanger oa condenser heating coll. ....... water . . . ....................... 4 5,9ta9 precautions in charging................................ discharging. ...... . 48 starting ........ 18,48 safety disc, see "Diphenyl Still, bursting disc". temperature control................................ :iS temperature recorder, ......... test records,............................................. 52,53 Distillation, see "Diphenyl distillation" and "Santowax distillation" Drawing list. ..................... 77 EARLIER REPORTS, see "Previous reports" Earthing of vessels ......., .................................................17,84 Effect of variables, benzene quality. .......... HI catalyst, see "Benzene, effect of catalyst in8 pressure ................................ . 34,87,114,115 pronotars. 112 recycled benzene .......... 112 recycled diphenyl, . ................................... 115 recycled high boilers. ....... 115 tiB@t*>eratur@ .......... H4 Efficiency figures, see "Cost of manufacture" Anniston report cm losses of benzene in off gas. .......... 3 Electrical use of Arodors, see "Aroclors, electrical standards" Untying of lead pots, see "conversion pots, e^>tying of" Equalizing lines oa convertors, see "Danversloo pots, equalizing lines cm8 Equipment Cost. ........................................................................ HO Equipment list.................................... ............................................ .... 83 - Equipment list, general notes oc.= ............ 8g Extinguishers, see "Fire Fighting*1 WATER PCB-SD0000045557 Index page 6 FE3TCE, round the pot lid. . . , ................................ ,18,87 Tire equipment. . , , . ................. .................................. 18- Fire precautions, Anniston report cited 16 Fire screens, mentioned . .............................. , , , , ,19,75 Flanges In pipe lines........................................................... ,,.82 Flooring .......................... .................... ......... 19,20,82 Float controllers In benzene recycle feed tank, see "Benzene feed arrangements " Flow controllers, so "Instrument*1 Flow sheet of materials............................. 25- Fraotlonatlng columns, see "Ooluans * Fuel gas, burners , ................................. ,85 calorific value of. ............................. . . 120a. calorific value,mentioned ...........93 connections 36 consmotion of. ............. 137,120a eonsmotion of, re?.a?>9d to pot tenperatures .35,115 control .................. 36,107 meters.......................... 31,30 GAS, see "Fuel gas" Gaskets .........................24 Gaskets, making of for pot covers........................................... . 87 German reports listed.................. .... 2,3,6 EB-4o, mentioned........................................................................ .... 7,18 Heads & tails fraction, build-up of by-product In, see "Diphenyl distillation, beads fraction susount eliminated0 Heads & tails fraction, ecwosition of, see . under "Flow Sheet" Baads & tails receiver, described .............................. .... 98 Beat balance. ......................................................................... .... 15 Heat exchanger on condenser water, diphenyl still , * 99 Beating coil for diphenyl still, described. . , . . v e 96 operation of, see "Diphenyl distilla tion, description" Heating coils for Santowax still .................................. 103,104 Beat of reaction. ............................................... .... ... 35 ...Beat treatment of stainless steel recommanded . , , 22 Health considerations............................................................ ... 16 See also "Welfare0 skin troubles in Arcelor...........................16,56,113: . High boilers, ratio of to diphenyl, produced. . . . , . .ns required. . . . I I Ini Hydrogen, alumina absorber for benzene abandoned. . benzene reeerrery from (Anniston reports), # 3 benzene recovery from, ocmaaenta on. . . . . . .116 carbon dioxide eootajsinatloa of, ... . .. 19,38 depression, choice of pressures at two stages. . . . . . '. . . . ,44,101 Csl cn v<U^N-7r co Q WATER PCB-SD0000045558 Index Page 7 Hydrogen, compression, flow sheet of Materials, see under "Flow Sheet* compressor, described, . .................. caa$>resBor, lubrication of , ...... 101 101 coB?jressor, operation of.................. , .44,101 coolers.................. .... ................................... . 100,102 cooling and compression....................... . .44,101 dangers....................................................... l8,l,101 formerly burnt with fuel gas . . . . , n6 oxygen determination unnecessary . ... 19,44 pressure control .................................. 44,100,101,108 receirers described, ....... . . . ioo,w surge tank................................................. a i 9 100 temperature recorder on compressor .................. 108 traps on instrument lines. .... t e ICQ traps for benzene. ........ ... .44,103 uses for........................ ... vent connections from crude diphenyl etc. tanks 19 IHTHRMEDXATE FRACTIOUS, composition of, see under "Flow Sheet * JnstrtBoents .................................... .... 107- banxeae flow controllers ......... 31,108 charts sent to MCL .............................................34,50,109 conversion pot temperature controller. . , 34,107 conversion unit tesperature recorder . . 34,107 diphenyl still .............. 45,108 diphetyl still, cooling water, no longer instrumented. ..... 47 float controllers in benzene feed vessel, "see "Benzene feed arrangements * Santowax still.................. .... .......................... .... . 50,109 Insulating eospotmd 66 for pot furnace Joint. ..... 88 Insulation* ..................................................................................... 90,94 LABOUR HBQUIHEMEHP.................................... .... ............................... . . .117 Lead, depth, of. In pots................. .... . . . 32 effects of impurities in. . . , ........................... . .22,57 emptying pots . . . 39 entrainment from pots................................................. . .38,41 forced back to vapourIs@r......................................... . .38,91 see also, ^Conversion pots, equalising lines" . . ,handling (roping off the area)................................ 20 leakage into furnaces ............ 23,42, _ detection of , . , i * . . . . 42 making up losses of ....... . .................. . .32,40 olds ..... ............................................................ 22* 40,93 DSW 462193 WATER PCB-SD0000045559 Index page 8 Lead, oxide, corrosion of pots by................... .... , , , ,22,23 poisoning, little risk of, . ........................... .... 19 pots, see "Conversion pots" quality of . . , ....................................... S7 reaelting............................................................. .... 40 pectrographie analysis of, neotieoed 57 Lead trap, cleaning o described.................... 92 mentioned 39 description of* .......92 central tube of, shortened, 92 sust be heavy steel 93 need not be stainless ,93 operation of.......................................... 43 repairing of. 93 KAXHTEHAJTCE OP LEAL POTS........................................ . . . 39**1,89 Kake-tp water tank on diphenyl still condensir^ . ays tea........................ 99 Kernel badly corroded under pot conditions, 22 Montar 9..................*..................................... .... 7,K Motors, type of. .....................................................................................1 EECEEL, and alloys rich in nickel, badly corroded under pot conditions 22 OFF GAS, see "Hydrogen" Operation Manual, (not yet written at Anniston).................* Operating records, diphenyl still. 45*52,53 conversion unit.......................... .... . 51 Orifice plates on units, details of,.................................... . 35 effect on pressure. .... 35,87 see also under "Effect of Varlablea " roaring of gas through. , 35 Outlets for products, as cable box coapound ,.*,< 7 electrical use as Aroclor. * . 55,113 as firelighters (not suitable). 77 general . .................................................. 7 in BB-40..........................................................7 hydrogen................. .... .7,116 roofing eoapotmds.................. .... . * . 7 Outline of process, ....................................................... 5 PACK3H3, diphenyl malted into drums 1 inconvenient , .48 Santowax H is now flaked .............................. .... .50 Patent position, Anniston report; cited............................... .... 9 ee high chroma alloys for lead pots. . .22 DSW 462194 WATER PCB-SD0000045560 Index P&g 9 Pip lines Jacketed................................................................ 82,83,95 See also under "Water in jackets Pipe lines traced, . . . ........................... ...................... .... . ,82 Preheater pot, see tmder "Conversion pots" Preheater, tubular, see under "Conversion process, two- pot system". Pressure increase by carbon deposition....................... , 34,114 Pressure, eca^ensation for by altering tenperatures, 34,114 Pressures throughout the conversion unit..........................34,35 checking . with C02. ... 37 Previous reports listed, . . ............................................... 2 . Process in. detail.................................. ......................... . . . . 29 - Promoters in benzene, see under "Effect of variables" Properties of Materials..............................,........................., . 10- Protective clothing, ......................... ........ 19 RATIO of high boilers to diphenyl, see under "High boilers" Record charts, see under "instruments" Records, finished product tests, see under "Specifications & Test Methods" operating, see under "Operating Records" raw material tests, see under ''Specifications & Test Methods" Recycle feed tank, see under "Benzene" Recycling diphenyl to convertors, see under "Effect of variables" high boilers to convertors, see under "Effect of variables" . Reflux split box on conversion units described...................95 on diphenyl still described. . . . . . 97 on Santowax still described, . . , , 105 Repairing column and lead trap......................................................93 convertor pot .............................................................. .... 42 Repair work figures .................................... * .... ...............................117 Reports (earlier) listed, see under "Previous Reports" Roofing coapound from chlorinated Saatowax. ...... 7 DSW 462195 SAFETY COJBEDERATIOKS ........................................................................16- hydrogen, , ................................. 18,19.101 showers..................... 19 Saaples sent to HCL listed. ................................................................21 Santowax, crude, analysis of by distillation. ..... Jo charge tanks for still ........ 103 eDisposition of, see under "Flow Sheet" disposal of. ...................................... '. . 7,48- distillation of................................................5,49- distillation yield ........................................ 7 handling of. .............................. 48- hold points of........... 13.50 physical properties of ....... . 13 receiver described .......... 98 WATER PCB-SD0000045561 -i Index page 10 S&ntowax ,cnHie,still. ..................................................... 104 column cm. 104 condenser cm. .... ....................... 49,104 designed for separation of the Isomers ....... 49 earlier design iaeaticaed....................... 49 heater described ......... 104 operation of............................. 49 preheater described. .......................... 103 receiver ............. 105 temperature controller ...... 109 tes^erature recorder ....... 109 vacuum vessel. ........................................ 106 Saatowax isomers, amounts sold. ................................................. 8 Anniston report on separation ' of cited........................... 2 outline of separation process .... 5 specifications and test methods ... 70 Saatowax O.M.&P. see "Santowax isomers" Santowax R, flaking of. ....... ........................... 5,49,67 handling of , 5 packing of.......................... 50 records of test results .......... 69 specifications and test methods...................... 64 Scale of working. ................... 8 Skin troubles attributed to poor benzene.................. 16,56,114 Specifications and tost methods ............ 54- Stainless steel pots, carburetion of surface suspected. .... 22 corrosion, see under "Corrosion* effect of Impurities in lead, see wider *Lead, effect of Inpupitlee in* effect of lead oxide on, see under "Lead, oxideH heat treatment reeaoaanded. ... 22 types of stainless steel 22-,86,88,89 Steel floor, advantages of open grids, ..... .19,^0,82 Still bottoms, see "Santowax, erode" Styrene, effects of on workers, see under "Skin troubles" Sulphur la benzene, see under "Copper Sulphas* delays the attack of benzene etc. cm pots . , 111 Sulphur, determination of, in Saatowax. ........ 68 Su^j tanks, see "Crude diphenyl tanks* i TEMPEBAOTRES, adjustment of to oonpensat for variations in pressure ..... ,34,114 T^)@rature control, detection of overptsqping of benzene to convertors...................... 30 SW 462196 WATER PCB-SD0000045562 Index page 11 Tesper&tur control In diphenyl still.................. .... . , . 45 Tis>rature controllers, see under "instruments" Tesperature, affect of variation of, see under "Effect of Variables" T^>ratur3 at various points in the conversion ' system 22,24,51 Temperature f pot, varying with the benzene rate. * . 84 lagging behind controller,, ... 84 Teipheayls, see "s&ntovax Isomers " lest Mthod,, see BControl Testssjand "Specifications and Test sssthsds" Therm! balance, see "Heat Balance" Tube process, see under ^German Reports" and under "Choice of Process" Tubular preheater, see under "conversion process, two-pot system" TOES for products, see under "Outlets* VACUUM pas?) for S&ntowue still described. ...... 106 Vacuus still, see "Santowax crude still" vessel, see "Santowax crude still vacuum vessel" Valves....................... .... 82 Vapourizer, blockage by lead, see "Equalizing Lines" and "Lead forced bade to vapourizer" blockage by solid, unlikely . . . .... 30 coil life........................... .... . . . . .... 91 described ............ . . . . 91 flue arrangesaenta...................... 32,37,86,91- leakage of benzene into, see "Benzene, leakage into flues" operation of. ............................... .... . . .32,37 overpu^piag of benzene into . . . . . 30 pressure drop through ...... . . 3* temperatures In.................................... . . 32 Ventilation ......... ................................ 16,19582 Venting of conversion unit. ......... Vibration of pots.......................................................... : WATER in benzene, tee "Benzene, mter in" see also under "Pipe lines" Welfare ....... ....................................... ....... 19 See al*o under "Health" Welding, fire hazards in. ............. .17,18 heat treatment recommended after ....... 22 on colun^a and lead trap. .......................... .... ... 93 YIELD MIA, see "Flow Sheet" DSW 462197 WATER PCB-SD0000045563