Document 3NppXZdoOENqbm49BG1YBva9J

PROCESS FOR TEE maWACTUHE CF bxfskml & mmmx CcafIl@d 'by E, tt&thsr, Jfove*br 1950 ft9. E A. Q'Jfoal, *., London. V* E. Oarrotfe, London Hr* V* D. Soott, London Mr, J. 8. B?mKh# London Mr. D. V. Shrift, London . Rmta Bosoareh FH@ (Hr. W.H, Ritchie) Mr* 0. Y. ttgftor, Howport (2) . Mr. P J 0. Burirood, Eamport (Analytical section only of the rapart) Mr. 0* 8 Dtn^i, Aimistan Vlfc8. A. K. EUetibrarg, Anniston Nr. J. V, Pennington of K.O.L., * (at Anniston, BoreiAep I9SG) 8t. Lotfi* Library 8t. Louis K.C.L. file (E.H&thar) WATER_PCB-SD0000046218 XSraODOCTOfg MQCT 1 Pr#14Mimry Informtira m* sent from Anniston to Hr, E. A. O'Neal., *%, In London, Jmm 19^6 Mr. D* S B&varercft and tee writer paid a brief visit to Amis ton in Septertw 19^7 to oolloot inforafttion needed for rmlmtloa and design work la London, and they produced the report Kote on the Process for the Manuf&oture of Diphenyl & Sm.t&mx at Ami*ton", September 19^7. A set of Anniston drawings, out of error 350 drawings on file, vu seat to Loudon, shortly afterwards, the selection being such as would give full onetractioml details relating to Anniston's preferred designs. Since then there has been & great deal of correspondence be tween M.C,L. and Anniston; ift% B. 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, n, August 1950)* and the present writer visited Anniston Ifovember 6-10, 1950, mainly to deal with certain questions raised by the K.C.L. mechanical engineers. This present report is intended to condense the information, collected as above, into a form convenient for use within Uonmnto Chemicala Limited, particularly in production work. It is hoped that it will be of use in the final stages of the construction of tee Newport plant, saw! that it will form the basis of a operating manual for use at Newport, to be supple mented and kept up to date as new information cone a forward. DSW 462056 \ WATER_PCB-SD0000046219 BMLDS REPORTS In a letter to Mr* D S. ferercrofi, Sept.11/47, Ifc% M. Buta listed tbs following a lx reports wfaleh. were already In London fileti (toa Chemlrnl Industry Report Seplw Osman Production of Diphenyl, Terpbenyla and Chlorinated Derivatives, by ayne 1,, Alexander, K.C.O., St.Louis, Oct.4.1945. Extract tram 0r*m Report, C.I.O.S. XXIX-l4'pp.56-57 Diphenyl. - Dasiga Data 4th WphaoyX Oait, D.A .Roper, with Study of Biphenyl Cotta, E.H.Buford, 0*9,39. Pinal Report on Plant Jest on Ho.6 Wphanyl felt - Part 1. Job Ho.171-41 File H0.138, 17th Sept. 1941. R.A.Ewing. Design Data for Diphenyl Still, D.A.Roper, Sept. 1939* Report Ho. 1924 Pinal Report on Separation of Diphenyl High. Boll? Into fractions or known Mixtures Part 111 ? Developing Plant Processes for Production of Santowsxes R.O.K.P. & Iff. Job Ho. 171-^1/ File Ho*2l8-B. Prepared by A.M,EHaburg. "Equipment Design, for Saatewax R Plant, May 20A3 , Job 1"-352-Report #31 by G.R.Shockley, accompanied this report. Jn September 194T, D. S. mrercpott & E. Mather wrote & report cm the Process for the Manufacture of Biphenyl & Santo- wax at Anniston. On Sept. 25A7 copy #11 of Anniston reports 1640, Pinal Report on Study of the Biphenyl Process PirtlH A Review of the Process, Job 171-41, File 138, F.E.Hubbard, Anniston, Oct.15/41,. was banded to Mr. fevercroft for London, ale a copy of Addendm* to 1712, Piml Report on Study of Biphenyl froceea. Part 3XC, Ccntlawu Let-down Proeedur, Job 171-41, PH 138. A. M. Ellenburg, Anniston, Jhn.31/45* DSW 462057 WATER_PCB-SD0000046220 IS&rllor Report*,, qontd 3 Ob 0et.l3/Vr# *lci*ofll* copie# of the following two reports were sent to Mi8. W. M. Cooper, Londons 16*12. Pinal Report on Diphenyl Operations. J.R. Moose, bctober l^Hl. C ` 1712. Final Report cm. Study of Diphenyl Process, Part lul, KiBbard, Ponmlfc Miles, Anniston, Oct.19/^2, On War<,u/fy8j, espy of report 1937t "Highly Cfalorimted Quaterpheoyla" was sent ?5*ot THTTLouIb to Rmboa. It*. BXleafcKff-g, Jtamry 20/W, rertered the following report** 214 "Bensol Losses in- Waste Hydrogen from Diphenyl Plant", J.L.Hbwerton, S opt,22/33, 445 *Reoeadatioas for the Operation of the rod Diphenyl Still", J.H.Carothers, June 23/33. 948 "Inrestigation of Benxol Losses --- at the Diphenyl Plant", Soorton Harris, Aug,21/35. Mr, KLlenimrg, Apr.28/48, cited the following reports cm tbs derma tube process? (1) I. G .ParbeaiMtta trie at Lererktajen Germany, Visit by Twnoelc & Lowderailk, (2) B,1,0.3. Fiml Report 093$ Item #1, (1947) pay & Richard*. A copy of Asmiitcm report 2211 "Interla Report on Alloy Test ing , 171-429* V.V.VMs, Ajr. 22/48, discussing the corrosion wo*ion of the lead pot* by the Yapottr blast, ms amt to London (Mp. Dwrorcroft), July l/4o. A sdorofU* copy of the Organic Dirts ion report "Diphenyl from Benzene", 117~88X, Oet.5/35, on the effects of ispurities in hmmgmp km seat to tS?* Thrift of M.O.L., tey 9/49* Th prooees description in this report In said to bar boon based largely on that of the report T)ign Data for 4th Diphenyl Gbit", by D.A.Roper. DSW 462058 WATER_PCB-SD0000046221 OTOLIBE OP PROCESS AS WORKED AT AHNI3T0H, 1950 5 BmKem vapour la passed continuously through aoltea. lead at a high temperature * causing aotm 16$T to 20$ of the benzene to bo converted, in a single pass through 3 lead hatha in series, into a aixtur of diphenyl, terphenyl, etc, with the volu tion of hydrogen, The resulting mixtion of hydrogen with the reaction produots and the unchanged benzene is passed up a fractionating column which has a condenser and reflux split box* so that the sensible heat of the rapsts's is used to give a roc^h separation of the organic cocponent* of the Mixture* The fr&etiomtion system yields a forward flew of liquid ben zene, and. an underflow of a Mixture of benzene, diphenyl, terphenyl, to., while the hydrogen passes forward, saturated with benzene* Shis hydrogen stream is cooled and co^ressed for the recovery of more benzene. The colusai underflow is fractionally distilled batatari,se at atisospheric pressure to yield distillates of benzene and of saleable diphenyl, and of coarse,intermediate fractions which are recycled to the still. The still bottoms, containing the higher boiling components of the Mixture, are called crude Santowax. *<.-- Seme of the crude Santowax is distilled ''straight-over8, under vacuum, to yield S&ntcmax R, and some is put to permanent storage because the supply exceed the demand. Crude Santowax has also been distilled under vacuum, with fractionation, giving ortho terphenyl of about 9^$ purity. Centrifuging of the distillate, or better, fractional distilla tion, gives a better product. Tim M-p fraction from distillation, has been allowed to cry stallize In pans, slmrled with water at about 85G, centri fugated and washed in the centrifuge with hot water. The centrifuge cake la then about 95$ para terphenyl. The oil liquors, separated and dried, is called See Anniston report #192*1-, Jan,8/t5 See page 50 below for a not on the flaking of Santcmaxea. AH the recovered benzene it recycled and their ia a practi cally continuous Make-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 tb processing. (See under *Coients on Process", page 111 below). DSW 462060 WATER_PCB-SD0000046222 HOTB OH CHOICE OP PROCESS Sc tli Anniston Report 1640* Oct. 15/^1, P.E. Hubbard, also Mr. A. K. KLlMib3rgli latter of April 28/49, citing B.1.0.8. te. reports on the "tube" process. The research departments at Rrnboo and Anniston agree In ho llering the tube process nay be superior to the lead pot process. Sow pilot plant work bai bees done In this direc tion at Anniston. See page U6 below for the choice of the nethod of recover ing benzene froa th# offga*. 6 DSW 462061 WATER_PCB-SD0000046223 OUTLETS FOR PRODUCTS 7 At Anniston bo of the diphoeyl Is flaked for sale, but by far the greater part is med either at Anniston or at Monsanto.*, rxilftols, for th tsanufaetec4 of Aroclors. Monsanto Chesteals Limited do not eo^eet to sell diphenyls A little also ia used at Monsantoj 111., for the aanufactm4 of o. 4 p, tmlno diphenyls* . . A mixture of rod Saatomx and diphenyl my be chlorinated to gv@ the Aroolor 2565 wed m a roofing compound. Saatewix H is used as the starting material for Aroclors 5442 & 5480, also for the hydrogemted product HB-40, which is used as an extender* in plasticizers, for example in Vinyl filM* The Saatowax R 1ms ooas little application in high tem perature greases for ?ulTe. Monsanto Limited have given lows consideration to the possi bility of usefully disposing of still residues. Dr. Scott, *uraary 29/48, considered that the residues would not be suitable for asking firelightera Er. Bardy, Kerch 4/48, passed on Mr. KLlenburg'a review of the possibility of chior insting th residues to about 60-65$ chlorine content to make a cable Joint-box oorm on ItIon v Mrs ELlenhurg thinks that chlorination at 250"2o0C to 35-4^ would be about the best procedure, but warns us that the residues are not of constant composition. It was thought at on time that M.O.L. markets would, call for a higher ratio of high boilers to diphenyl than is normally obtained in fchs Anniston process, and ease thought was given to the possibility f shipping &om of the Anniston, excess stock of high boilers to Britain, and calculations of the British in>rt duty were lade, Kr. J Y. Head's note of lurch 2/48, however, indicates it ia now improbable that such shipments will be necessary. Reference is cade to a ssastorandxm by ft*. D,, Scott of Ruaboa, dated June 2oA7# on the long term development of outlets for diphenyl. In the distillation of crude Sant wax to give Ssnfcowax R, about 15$ of th weight of the crude is left as a residue, and som of this ia sold aa "Boater 9*. ^ Sonus of th hydrogen after cooling and coo^reasioo* as out lined above, i* used for the hydrognation of Baatowax R to give HEk-4-0. Any excess of hydrogen ia vented to ataosphere after being expressed and cooled. At one tin Anniston put th excess hydrogen into the fuel gas for the furnaces, but th consequent change* in th air requirement of the burners were troublesam. DSV\/ 462062 WATER_PCB-SD0000046224 some m voR^m About 950*000# diphenyl per month# and 80*000# Smtamx H per oath* wm produced at AnaLstan during the first nine months of 19%Y In Sepbwhm? 19%9# Mae units were In operation* each rated at about 4000# diphenyl per day In Xoves&sr 1950* there ?er@ t^elr units* msdbered 2-13* la existence* the original H*1 haring boon taken tit lenport needs were estlmted by Hr# Cooper* 0et*lA7# to be 1*000*000 lb diphenyl & 240*000 lb S&ntomx per year. The aanml sales of the ortho tarpbeayl hare arer&ged only aroBttsl 4000 lb* and those of *Santowax M around 10*000 lbB There his been rery little sale for the para isomer* 8 osw 462063 WATER_PCB-SD0000046225 pATsar posgioy ' Sm Azmis tea JtwewLreh Department* Heporb Ho* 3^0, p&g 6, 9 DSIV 462064 WATER_PCB-SD0000046226 PROPSmiTO OP MATERIALS OOSqmHTO 10 Benton# Jt.Vt. tt.Pt, B.Pt. 8peeife Orerity Sp^lfle solid HqM 78 5.31a 8O0 0,883 to 0.886 155A5*5C W. g|' (1*0,T.) Ykpour Qp 0,463 "8005- * 8 Fcrsula for Sp.Ht. at eons taut pressuresTM Cp s 0,258 * (0*000875 x 0) Parry 1st Edn, 0.266 * (0,0006732 x 0) Ind.Eng.Cti.,Jlily 1935 latent Boat, B.t.O./lb: fusion eraporatioa ^IS:5 Flash Point P. 1 closed ClOYOlMKi 12 Eiploalf Unite la airt Xovsr Qpper ^ Auto-Ignition teaperature 1.4 8 iar6P. DSW 462065 Vkpour Pressures? Constants In V.Pr. Porwtla Log^o pr, sun. Hg g ^^7a6*, * B Hfimt C -5 to -30 -30 to A 5 0 to 42 %2 to 100 A *2.90* 44,222 34,172 33*295 B l:fp T.962| 7.6546 **._i------is n " *n. o/ao. WATER_PCB-SD0000046227 Properties of Materials Concerned, oentd ` 1. Bengwn (contd) Therml Oondmtlrlty^ (liquid ft gas) See sheet 3> Design _ Data for ttalts 4 ft 5* D. A. Roper, r for corves. 11 2, Dlpfeagyl Sm ^Description. f Proses* used in Dent,246\ Sept.27 Inflow,, Softmtako ft Becker, page# 49 ft ol. . S also BimIgn Data for 4th Diphenyl tbit? Ang.9/39, Specific Gravity* 0,992 @ Y50C/4Ca Th Swan Chemical Co, 'bulletin of 1930 gave thermal data en diphenyl. Viscosity of Biphenyl (from Amis ton files) F Ceatipolsee 160 170 180 190 200 220 50 300 350 400 teo 482 1,439 in4 1.034 0.901 0.752 0.574 0.45? 0.374 0.313 0.283 Specific Beat (from Amiitm files) F B.t.TT.Ab 200 Boo 700 800 900 1000 0.416 0,470 0.547 0.616 0.658 0.690 0.696 t>S\N 462066 WATER_PCB-SD0000046228 Properties of. Material* Concerned, oontd S, Pdjfaetorl (oanftd) / Another woorf give# tbs following values for liquid, ' diphenyli 2a gp.Bs&t eala./gr 100 03f0 150 0.^60 goo 0.*12 250 0.460 300 0.518 8S 0.5T5 0,610 450 0.625 WPOGP Op 0.460 25W o.< (B.A.Hopar, Design Data for tfalts 44 5) Deosity of Liquid Mphaayl (froa Anniston file*) grass./ee 75 100 0.9885 0.! " 150 0.< 200 0.1--,, 250 0.8470 300 0.8010 350 400 0.7510 0.6918 450 0.6180 Boat of Ttoorlsatlms . 65.4 g.dO/c e 258,5c. 12 OSVJA62067 WATER PCB-SD0000046229 Pr*opertli of jfatariala Concerned, oonfcd 23 Saatowx R contains about l diphenyl 1 rth tarpheeyl jaeta trphayl 21^ psa-m fa*ph^rl 22^ trIea,thophe^Xn#qii&terpbeGylB etc, (Aaaiit Mml Report 1942} !3jpp@y hold point home hold point 13T-"l4|09 45-60^. Changed ) 137-l45C Sapt, 23/47 )" 45-63C TSj density of the Santowax- my be assumed to be th warn is both th erode and distilled fora. Viscosity also is th m, Specific Gravity of Crude Saatowx; 140C 175 215 300 1,026 1,000 0.98 0,964 (eat, from curve of other points). Viscosity of Santmwa: H 155*0 225 1.4 Saybolt tBiiversal Seconds 1.5 ^ *" Moltea Bantomx flow about lik water at 25 C. (A.M.Ellobarg,a lsttsr Jfcn.6/49) Specific Beats (stimted) Solid Liquid 0.4 0.5 Latent Beats (fftlmtod) Foshs 63 B.t.W.Ah , Vaporisation l40 B.t.TJ.Ab Bolling 'Bmmi 36o-45O0. Flash Point 1 01. open ct*> 191C. OS^N 462066 Plane Feists 01 opt 01 238C. Another aseotat givem Plash Point 190C| Plane point 220C, WATER_PCB-SD0000046230 Properties of jfaterlals QoaoernM, contd 3. Bwtemx R (emM) VhlmM aearned la the design of the Santomx still at 8p,&t Bat of Irtiporisatiea Yisoosity at 2500 Ytaoesity at 350C - 0,5 , - 1W Bt.U,/lb - 5 centipoise* * - 2 oentipaLoes * * (lfc. Kiletsburg said them mlms %w too high). u 4 fmyhamlLa CSmd ortho fSantemx 0 0md@ Mta, (Santow X, Ortide para (Sasxtewax P( p msteeti Ternary @ut#ctie . "Bold Point" B.Pt, 30m 35?0 2OQ-213^0) mlxtwte 84,80 about jHcC 2050 2kOC Sm also Monsanto Technical Bulletin #P-X03, 3ank/%7 lean* for the properties of the separated crude isoaers sold. DS\N 462069 WATER PCB-SD0000046231 -I HEAT MXAWS 15 be heat talanc Is dlaouased 111 tho Anniston Design lata, til Chit, tqr D A. Eoper, Aug.9/39* Jg 6. Hi heat of reaction of benzene to diphenyl ia given aa 59.29 lbC per lb at jK00. . Trsiis.A*.Cbe.E3s, Y* 41, p.l44* (1936)* girts 61 lbC per lb. 5ffa! i calculated to b@ lei* than ^ of the heat heeded la - 3-pot unit. ^01Q osnH WATER PCB-SD0000046232 SAFETY COBSIDERATIOKS 16 (Pro* Anniston report 16^2 of October 19^-1* section "Health & Fire Eftsards*R. and fro* discussions at Anniston in 19%7 and 1950). , Health It la obviously advisable for the operators to alni*ia@ their contact with benzene vapours and with th vapour fro the hot lead* but there is no history of trouble fro either of these in th Diphenyl plant. We are warned that lead vapours my be evolved during the burning out of lead traps and carbon traps. Whan lower grade benzene wai used for Baking diphenyl in 1930-31* the operators in the Aroelor department suffered from akin eruptions (acne)* thought possibly to b due to chlorine deri vatives from styrene in th diphenyl. The disappearance of th trouble coincided with the change to better benzene. For tins the Aroelor operators bad 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 tike building. Pire Th conversion units contain hydrogen and organic vapour* at high pressures sod temperatures so any failure of gaskets or of th units themselves my lead to the asoap of a cloud of inflaamble vapour* near to th pot furnaces. The amount of organic Material present in the conversion mit at any on moment is* however* quit smll* and the flow of benzene to the units can be shut off fro outside the building, in th early days at Anniston* fires were not infrequent* but there hu been non of consequence in recent years. I^haala is laid on good worknanshlp in the construction and. miatenanoe of the tnlts. There were twelve conversion units at Anniston in JJoveaber 1950* with thir oltwnaad other auxiliary equipwmt* two of th units being in owm roc* four in another* and six in a third room. The three rooms are separated by fir walls with eoMiaileatihg door* sow of the autcmtioally closing* but held open by chains having a fusible link. There are two DSW 462071 WATER PCB-SD0000046233 Safety Conn, Idjerotlooa, contd ^ P1T0J) OOOtd diphenyl stills, each In it a own roota, those two wom taring onneeting door* Into one another* but not Into the conversion room, The still rooms contain the receiver* for the finistad diphepyT* the head* and t&ils fraction** and the still bottoms* but the benzene receiver la In a pit* behind a fire wall out side the building. The crude diphenyl from the eocrrertor Iwms flotrs to two receiver* which are outdoors* alongside the benzene receiver1, ' The win store tanka for froth benzene are In a fenced area* well away from any manufacturing buildInga* and the benzene feed tack and pumpa are in a sailer fenced area* somewhat nearer to the diphenyl plant. Benzene vessels are systematically grounded (earthed). See the note on page 83 below on the objection to internal steam coils In the benzene tanks, " The department is well supplied with extinguishers, both CO2 and CClk types* and there is a permanently piped Foamlte connection to the min benzene vessels. There Is a dznm of GO34 on a stillage on the ground floor of the conversion room for recharging extinguishers, and all the appliances are sub ject to routine Inspection. - Cloths soaked in CCljj. are used to stop off pip openings etc. during repair work and the units may be filled with C02 during welding repair, * The convertor rooms are not treated as having a dangerous atnotphera. It is not at all unusual to have escaping vapours burning round the cover of the oonvertor pot (especially now Mom of the convertors are being run at over 20 psig). If vapour leaks fro* the pot flange* it my not Ignite* especially If the seal be tween pot and furnace Is good, but it Is better to ignite the vapour rather than to have diphenyl subliming about the buildlag*and lodging 00, roof members* etc, Welding Is dm In the building* said of course* seme of the vapour pipes are red hot. Baked flame* are used to deal with blocked pipes la the convert ion system. The diphenyl it111 rooms do* of emc^so* contain large amounts of eos&ustible mterlal because of the batch nature of the operatic**, The heating coll furnaces for toe two stills are side by side in a room of their mm* cut off fro* all ether roosa. Those of the still receiver which are indoor# have vent pipes* carried out through the roof of the building, and the outdoor nSW /ifiOATO WATER PCB-SD0000046234 o Safety Conslderationa* ooatd 18 Itof! W&M - b@nxn reeeiyer baa Ita rent pipe carried well up Into the air# Each. tlU body has a burst tog dine to a pip leading up through, the roof* (so page 9^ bale*?) . 4v ' Ami*ton are a Httl restricted to doing welding repairs to their Saatowax distillation system beeause of its proximity to tbs BB-40 plant* whtoh itsos hydrogen under high pressure. The for the hydregea at mcix stag* of oppression hav'Al-?b bursting dlsei* to pipe Tenting abor the roof of the oppressor rcwm. Car is needed* of course* to restarting the gas-fired furnace*. There is a powerful draught up the furnaces and the pilot Jets my easily be blown out. Its UtoahOTg* Aug.XS/W* stated that Class I* Oroqp D motors are specified for pushing diphenyl and Sentowx, Be also stated that th@ bottom Iren the diphenyl stills* If discharged at aromd %00C* my take fir. At one tiisa it ms the praotie to purge the stills with COg before reoharging* but this Is not now thought neeess&ry* and all that is done is to allow the still* to cool to about 200C or lower before rebarging. hmn the rude diphenyl* hot fro the store tanks* is prasped into tbs hot still* there my be a great rush of Yapous? through the condensing system,. Sto@ the introduction of the restriction orifice* after the ooarertar pots* these pots hare been running at about 20 psig, so that there is a greater risk of blowing out the gasket cm the enrorter ooweer. Bom of the onYertora Imre been fitted with a loos sheet iron ring fnee about 6" deep* ronad the oorer Joint* to defleet any possible burst of flam. ym Fighting Equipment te*. Harden* August 1950* reported as follows i f,A^pl C0 and fmm oxtingnlahert are provided, Annis ton has two standard focus extinguishers on each floor of the onfwtor section and serer&l'ln the distinc tion @#tic Oil the groinid floor* available for mo throughout the diphenyl aroclor shed was a large bandart foaia pplian,ee The beaxei* tanks are permanently piped* to top of each tank and into the atap* for foaa which it strolled from a mitral point", DSW 462073 WATER_PCB-SD0000046235 Safety Considerations, eontd 19 Fire Fighting Equipgent, eontd Each convertor tmit has about a 56 lb cylinder of COg permnmtlj connected to a fair leading into the benzene feed line idler It runs below the operating floor before rising to the top of the vapourixer. These cylinders are supported against the stanchions on the ground floor* Ho provision is tads for warming the*. A drum of OCI4 is kept cm a stillage on the ground floor for easy recharging of the extinguishers. There are numerous safety showers, each with the usual yellow painted ring cm the floor below thorn* Hydrogen She eanverelon units contain hydrogen, and so do the crude diphenyl store tanks, because they are vented into the hydro gen min. Tito vent pipes from the crude diphenyl tank to the hydrogen min are usually very hot. Air must of course be purged from th system before any hydrogen is taken to the easpre ss ore, and usually OOg is used for this purpose (400 eu.ft. for a convertor unit), also to replace hydrogen before a unit la opened for repairs. Thar is no tor* in allowing the COg to go through to the hydrogen compressors, in fact there is th advantage of recovering its benzene content. It is no longer thought necessary to do oxygen detorminations on the hydrogen stereo*. The crude diphenyl receivers are vented, into the hydrogen collecting system, and there is a risk that if they are pulped @s^>ty, the hydrogen my escape into the diphenyl still system. Welfare As already mentioned, only ordinary eosmon sense care is taken against poisoning by lead or benzene, and no special clothing is supplied beyond face males and leather gloves for man dealing with molten lead. Sii^l "firscreens" of sheet iron on pipe frame ar used to shield the ana and the equipent during the collection of the samples for the & conversion, test. See page 75 below. It9. Harden reported, August 1950s "High tmq>eraturs are fairly general throughout th departaont particularly above th* convertor. AH floors are f the vertical strip lattice con struction to i^srov ventilation, and large portable WATER PCB-SD0000046236 Safety OamidaratIona . centd 20 Welfare, eonid ; llett-olng fans are used to blow up through thee floors whenever a sail has to work i4>stalr. BormXly all operations aro controlled from the growl floorj all possible controls and instrument* being lornted there. The writer regards attentions to this detail as essential if eonsei@ntioa min tenane of equipment Is to be obtained." Repair and mlntemace work a the conversion units at Annis ton Is mad more difficult by the radiation of heat from the surrounding units,, specially in the room which ontains six units* The lead traps, in particular, offer a big radiating surface. ' Tht diphenyl building, with good ventilators in the roof, is very high, and the open-work steel floors permit a strong updraught of fresh air to flow through the rooms from the ground floor, whloh In every ease Is eo^letely open on the east side. Wmo molten lead is being baled about on the opera ting floor, the ground floor below is roped off. See page 39 below. DSW 462075 WATER PCB-SD0000046237 c 21 SAMPLBS SEBT FROM ASHCTOM TO IMMO CHEMICALS LIMITED The following sables ww sent fm Asajjjtcm, Hoy13A7j 0-4070 0-4071 0-4072 0-4073 0-4074 0-4075 Benzol Crude diphenyl finished diphenyl Saatewax R";' . ' " Still bottom from diphenyl tin Still bottom from S&ntomx still (also 10 lb Montar Ho, 9 requested Jun 22/48) btst only tb first tiro reached Ruabon, so tbs last four war nMtd Jtauary 25/%9^ to London, (and wore received there Feb.21/49). Tim foilwing sables alio wore seat to M.C.L., on the dates stated? . <3te8 22/48 Saatoms R Mer./\9 Benzene as used at Anniston. DSW 462076 WATER PCB-SD0000046238 c cmmim 22 / Bmsme nod Biphenyl under the working conditions ar not corrosive, but it had boon found advisable to use atainloss steel for the lead pot* and connecting vapour pipes'. Amistoo Interim report 2211, dated April 22/48, describes pot failures by "washing erosion* of the ire Ida and the pot bottoms, failure of the welds, external erosion by lead, and by other causes, and alao reeoMand the me of 310 stainless welding reds, or of 309 rod with subsequent annealing of the pots at 2050F, Copy #11 of this report ms seat to Hr, D. 8. Eavercroft in London, JWy 1/48, See page 57 below for a discussion of the harmful effects which foreign lenaai* in the lead night Imre on the stainless steel of the pots. In January 1949 it was reported the Anniston experience up to that date showed 309 type stainless teel to give better ser vice than 316 type. She Texas City Re gearoh Report Ho, 52 "Special Report on Lead Pot Corrosion", 2,Fitsgerald, Feb, 17/50, (copy seen at Annis ton, !f0v,/5O), deals with the corrosion or lead pots used to crack propane at 800OC to ethylene (formerly for pyrolysis of ethylbenzene to styrene). It reviews the informtion 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 tests showed that lead oxide was highly cor rosive to the stainless steel used, . Sables of different stainless steels iiaaersed in the lead pots gave inooMlmirm results, but Hastelloy and Has cross appeared to have high real*tan#. Pure nickel, monel, and nickelehrosim alloys with 80$ nickel dissolved in the lead in a few hour, W,V.lfed, Amis too, Apr,22/43, reported poor resistance with 68 nickel - 18 chromium alloy. C&rbumtioo. of the metal was suspected, with the formation of brittle coating easily removed by the pounding action of the lead, A patent search revealed that the resistance of high chroma alloy ms Imawn, ' The report ended with a reeoBBaetid&ticm to rtm all the pots at a lew rat# to diminish turbulence rather than to rtm. a few pots at high rat. It ws reocraianded too to put earbeo in the pots at tb outset, to reduce lead oxides, but this recoaaeodatioa has not been adopted at Amistoa, D-SW 462077 WATER PCB-SD0000046239 CorroaiQnfl oonM 23 Lm4 ia kstwn to scape -boh itiaes through the oorsr Joints on the pots at Amlatocu It Uxj fora load oxide otits Ida the pot, &M this lead axldo m; * attack tbs outer surface of ' the pot There is no point in taring to detect lead in the stack gates because there ii always amm lead lying about in the furnaces* DSW 462078 WATER PCB-SD0000046240 GASKETS Anniston report 1642, Oct.l5/4l> recommends Oarlock 721 gas kets for temperatures up to 500C, and Goetx corrugated steel-asbestos gaskets above 500C. For the cover of the second preheater a 5A6" round soft copper gasket la 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 below), but if the distortion of the flanges could be provented, the 5/16" copper gasket would bo better. Copper and Its alloys hive given .poor service In the hydrogen system, apparently because of HgS. Copper gaskets In the compressors have completely failed, and Babbitt metal has been proposed. DSW 462079 WATER PCB-SD0000046241 U FLOW SHSOT 25 The attached flaw sheets of Materials, pages 26 & 27, are taken from Anniston Research Department,,. Report ho* 1642, October 15# 19*1. The same report gires the following: datai- 0,1796 TLSoCfsll benrene eenstraed per 1 lb distilled diphenyl produced (eosp&re cost records giren on page 128- below# f the present report} * Tb sht"down time on the cower slon systesM areraged orer a period of 8 months See also page 28 DSW 462080 WATER PCB-SD0000046242 O i phenyl Process f-lo-w Shee.f 26 cut Q Hi "mo a 7~- 2 b' c rjp -- c- t< VoL ft 3 eu Yah or it i n q t - P S ec. . o #/*P 7q = 3 4-0 d.vg C Vapor Yo{ = qs Out Ye{ 1 ^7Sft/%K & 3Vo 'Cf /SC . Prehiaier ~r= $<fo "^/ejy C - ? See. P- 3g *//** Co * 7^ - ss<5 "c op * L P ,^, . = *73 0 C y HB - T> # H o-~ ^ ^ P6 - ? A1 T.o S pher e Pa ere -3.0 H Cu fit = *? * A- At me <r 7 ~ s s~ er 5 ctSes p 3o<?w/i 4 * u-rO rrV\ / \Tr*t,.~-st l,` -J I I ft~c ( ConcT' ?nS-:r 1" " ' , sr/pp 1 O fs ( T~ f-'~ POti.'ip 7/ S."o " ACv " e/ C^fP, -uttnft- ZO p ~ u f,5 %Snv <V-B - Z.C,6fT H* 9 VOt: P>6 - ?ff To Cc nv-ertor T ~ SHCS /v f ~ 7 se TT */V afh^t-ctt . T373.o "C )p = (iuojl 3tr F-5`7 Cor r Ko/ r /S3<5<3 oj. f{B - /m - 3-# Gaet-bo n F ^ ^ P6 * rtf OP tT4r6o/j - r* tf P - P- 5' # ///, z- 7l/<?/ ro P ~ TV a d3 Co 77b ~ DP -" A8 - <7^ V'/i.' " CcxrDcrx PP <4 ^ j/ 44.0 4 5'0 ?/ C 77 ' 7' % - 3 fcS DSW 462081 WATER PCB-SD0000046243 27 C Flow SK e c-t -for hgno( (m^) ses -r ro wi Col 6 in h . Ho. <- A+ fi 'rt OSW 462082 WATER PCB-SD0000046244 IIT U M OF 3 0 IC UTERMEDXATE LIQTORS a--- *--^3-----m Ur( 1 *o 2 23 .C S? Mg mS J! n .mi A & -5 a & i a! o H8o s .1 iH s mjj^ a ml fi mjj ... s 4J .......... <0 n & g, Htsf I .......... . 8 & "w & g - u. 6 o o <H *eH . *2 I n I " O G4aoOl2rl_ . "h m_ . IA 3 4* *O _' A '? J** * st m H H 8 & -v* a m0 j* OS O ri & e ,2grl !Ia t ft. B <4sl Z*5^* fWim. g*s4 s 2 J K 8 &Qfi.rrJtl iaOS Oe(4 -. _ 1 28 jZi4 cin A ts 0 I $ini <? mn oH vA - l as, i; to o &a 45Hrl4flH4 DSW 462083 WATER PCB-SD0000046245 PROCESS IN DETAIL 29 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. Mater is used to prim the pinqp, and of course it must be separated afterwards by draining from the store tanks,tar from the recycle tank. From the Storage Tanks the benzene is putped by (#2) to (#3) Recycle Feed Tank, Eero recycled material is constantly mode 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, (See under "Comments on Process* pages311 & 312 below). A float within the Recycle Feed Tank automatically operates the pimp, item #2. There ere also two floats within the tank for high and low level alarms. There is a history of a little trouble due to the sticking of those varioua floats; see notes on I tea #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 pimps, item #4, is taken from the bottom by a Jacketed line {.Jacket, however, is not used), cemented through thv 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 the tank has a srnro, with a drain valve for tapping off the water, etc. Regular and frequent operation of this valve is a very iasportant part of the operation of the plant because a shot of water, pushed through to the vapouris er, may flash off almost explosively, and might break some Joint in the pressure system. Water gets in from Its use. In priming 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 about hourly intervals, under hand, control of the punp, item #28. (3) The benzene distills.fee from, the benzene receiver. Item #21, of the diphenyl still. This distillate cws for ward In batches at Anniston, via the pimp, item #21a, but Mr. EUemburg's letter, J&n.20A8, Indicated that a similar procedure at Newport might cause too great a DSW 462084 WATER PCB-SD0000046246 Process In Detail!, oontd .Beazen# BmdllBgj ecntd 30 yariatioa In the ratio of fresh, benzene to recycled benzene* b@eaua# the flow of fresh wmM be ?ew wish mailer at Seaport than at AmlBtanj box the diphenyl still hatehee probably not wash smUtr. Mr# nimaburg attests interposing a buffer tank between the rooeirtr* item #21* and th reoyol feed tank* Item #3* so that th stream of recycled internal from #21 can be smoothed out. ' At Amiston* th operator waits u&tH th float alarm on item #3 is Viaging oa low "^before puling in benzene fro, the diphenyl distillation on th hydrogen oppression* then he steps when the al&m "rings on high". Thar is a ease cm record la which the recycle feed tank was orerpm^ed* and the excess benzene backed nap the distillate line and into th eocyertor reflux split boxes of th conver sion emits* mp4 soaped down th oltams into the crude diphenyl store tank# Elis ovex'pts^iag was detected by the fall in ternperatur of th coIubsi underflow streams. There are two (2-afcag Gould) (#4) centrifugal jranp for feed ing benzol at approximately 100# pressure from the recycle feed tank to the oarersion tmits* and one or both my be in opera tion depending cm the number of tmita operating at the tim. Share ii a Fisher strainer before the ptmpa* and there are two filter pots* after th pu^>* in the Control room - only cm in ep^aticn at & tine* to allow for cleaning. These two filter pots are vertical cylindrical vessels about 6s l#D, by 9" deep with boltd~oa covers* fit of ours for wanking press we around 100 pslg. They hare baskets ins id to hpport cotton filterolotha but in, SormiMP/^Q the loth bad rotted and had not been ropU-oed. It is thought that glass loth wight MFTt. There are lordstrom 3-way cooks on th inlet and outlet lines for easy switching of th pots, and there is a pressure gauge on each line* to indicate th filter resistance. Th min purpose of filtration is to protect th flow controllers Solid matter earrying forward to th vapouriscr would b@ siaply cmnried through in th wpow stream* and probably eoA in the lead trap or the esrboe trap of th converter. It is said that a little dust (fr th pots) eooss forward in th recycled beneon, and there is pipe seal from the benzene lines. DSW 462085 WATER PCB-SD0000046247 Process'In Data'll, ontd Benzene Handling, ontd 31 Th filter potm deliver to a header, a erring a row f 13 Foxhom recording flow controller, on for each unit, plus on spar#, th* piping being to arranged that the spare controller an, b ewitetmd in to replace anj of the others. These con trollers are in a special room which, la entered from outdoors and which has a cowmmleatlng door to the Min control room, otherwise it is eospleteiy shut ff froa th rest of the plant. Apart from the bens*m Tim controller this roo* contain only the mtors for the fuel gaa to the furnace*, land a controller for water to the BD1 absorber for th Arocler plant). Mr, J. 0. Glegorn, th department manager, mentioned that Rota meters were formerly used, set la a glass box draining to out doors, to talc away any beasen leakage. There was a certain advantage in haring th risible flow, and he would like sight boxes (fit for 120 psig) in th present flow line. Th* benzene delivery lines from th controllers are cemented through the wall between this room and the convertor rooms., at about th level of th convertor pot lids, a separate line to each conversion unit* Bach line dips to a stop valve within easy reach of the ground floor, inside the convertor room, and then rises to th top of the vapourizer .imifc. Baaedlately after the stop valve there is an inlet for CO^ from a cylinder chained to on of th stanchions of the building. No provision is . md for warming the C02 cylinders, though the ground floor, bting @o*pX@tely open to the air on on aide, is not very war*. Th sarml flow of benzene is 170 TOG per conversion unit per hour. DSW 462086 WATER PCB-SD0000046248 Process la Detail, eontd 32 Conversion Tbare ware 12 conversion units, item #5, at Anniston In Kovem- ber 1950, two of them (units 4 & 5) being somewhat different from thm rest In that they had a tubular preheater, then two lead pots, whereas the other ten unit* each had the preferred noml arrangement of three lead pots and no tubular pre heater, (See page 85 below for the reasons for choosing the three pot arrangement), E&eh of the 10 normal units consists of a (#6a) Vapourlzr, (#5A, 5B, & 5C), three lead pots la series, (called respectively 1st preheater, 2nd preheater,and convertor), (#7), lead trap, ($) fractionating eoltsaa, with (#11) condenser and (#12) reflux spilt box. The underflow from the column passes through Item (#9), carbon trap, and then by gravity through stewjacketed lines to the rude diphenyl receivers. Item (#10), The vapourtzer consists of a coH (formerly two .coils In parallel) within a stack through which the exhaust gases froa the pot furnaces are passed countercurrent to the benzene flow. There le also (#6B), another stack for the purpose of by-passing the furnace gases. If necessary, away from the vapourlzer coll. The tenperature of the vapour leaving the vapourlzer Is about 250C, but see below, pages 33*34,If the vapourlzer has two coils in parallel, an attempt mist be Bade to share the flow between them by manipulation of the valves at the exits from the individual oils. See the notes below, under Item #6A, page 91, relating to tbs possible loss of benzene vapour by perforation of a vapourlzer coil. Each c Olivers ion pot Is of stainless steel about 22-3/4" I ,p. by about o'-0"deep, and contains molten lead. The following figures are given for the depth of load in each pot? Depth of Lead? Anniston report i^OctO^ 1st Preheater pot 2nd Preheater pot Convertor pot Height of Distributer^ Inlet above bottom - of pot given as J V-0" V-o" 3,~6r 10" H,L,Harden, Aug/fo. Zoontlrad Nor/^bjr 2,~l" dry dip 2* -6" dry dip 2 *-11" dry dip out of 51 -U-3/3 " internal depth There Is little entrainment frott the first preheater to the nsecond, and not saeh from the second preheater to the convertor, but considerable entrainnsnt from the convertor pot to the lead trap, so the depths of lead are liable to vary a little. If It Is not desired to open a pot, the los of lead may be made vp with molten lead poured in through the neck which carries the thermo well. DSW 4fionu7 WATER PCB-SD0000046249 CONNECTION FROM VAPQURIZER TO FIRST LEAD POT WATER PCB-SD0000046250 Process in Detail, eontd 33 Conversion, eoatd Each, pot cover carries (1) a dip pipe to carry the vapours down Into the laoltan lead, (2) a tfaarao well, and (3), a gas outlet# There are horizontal baffles or apl&ah plates to disdniah the entralnMat of lead, The first aM eeoad pre heaters also hare a connection, to an equalizing lima with a top vdkfe# These equalizing lines connect into the bottoms of the convertor oltros, Item #8, and are normally closed. They provide a esrreaient location for pressure gauges (on branches below the stop valves), and could be used to by-pass a pot in emergency* and they an be used to diminish the chance of foreleg lead bs.k upstream during an interruption of the benzene flow# The lead pots hang, by their rims. In a row, aeh la a gasfired, fire-briak: lined furnace, the first preheater being between the other two pots# Anniston report 1642 of Oct15/50 gives the following apprcccl" ate figure* for temperatures In the conversion system; Vapouris or XuBTi^eo11 type) 1st Preheater Benzene in 250 Flue gas in TOOG . out 34oC (137 reported AugA7 out 190C . ' . Combustion gases Lead teeperature Y&pottr exit 6^Q-'J000 570-oOOC (380C,AugAT) * 550-580C 2nd Preheater Lead teEperature 720-740C Vscpoxo' exit o50-670c Convertor Lead te^> controlled at 840 5<L (but see "Oosaaenta on Process",pages 111- below) Vhpour exit 710-720c. Ccluun Top Bottom 80C - aoastlnea higher--ip to 970 135-250C - normally about 200C The furnace casings had a tenper&ture of about 100C as Judged by hand, Hovsmber 195 DSVW 462083 WATER_PCB-SD0000046251 Process in Datail 0 oontd goaverslon, emM 3* 16% Bard#n reported the following tan^erafcurea In August 1950? Tfclt Xo, 8 lo n 12 TtefKMPtBttP 350-200 Xo.l Prsfasst Wo lb,2 Preheat J2Q Top (khimm 7*5 85 Hm gas Xslst I Flos ga# Outlet Bas&s flm 175 330 180 150 120 530 *50 *95 *80 Ms 90 83 80 a* V/ ^ 0 . fesL 235 322 316 230 170 0,3,G, per hour 300 350 55^600 7*0 7*0 820 790 85 90 burnt out 190 250 13 310 5*0 200 Earlier reoords are gives in a copy of the plant record, sheet page 51.bsloir ?te la a Multipoint te^eretw recorder for each ecavers Ion unit and a reocrder-eentroller for ttem conversion pot temperature, A maqplM strip of the Multipoint chart was sent to MrvW.M. Cooper. 0et*3l/*7. Tbs pressure drop through the double coll vspourlzer, at 170 03G bemsb0*mxj was.. 8-10 pal* Prtssur of vapour entering 1st proheator Pressure of vapour leaving 1st preheater Pressure of vapour leaving 2nd preheater Pressure of wpw leaving ecnvertcr 50-60 psig 38-*5 psig 15-25 psig 4-7 pslg Cho'prossurss V817 a little as tbs depth of lead changes by satr&liuasnt of lead frtm the pot, M as carbon builds tp in the gas passage, f*be gsttgoa waver a little because of the bubb ling ad mrfaginc of the lead In the pots* Oarboii builds up arcmd the baffles and In the pot exit lines dating operation, causing a aim Increase in bade pressure* TMm increases the retention tins of the vapour In the system, and muses the oavenioa reaction t> continue a little beyond the point thought best, so the operator lowers his pot teaperat*es a little to esf>ensate, See Effect of Variables, page H* below. Bsosatly, the back pressure on son of th wait has been purposely Increased by th* Insertion of rifle plates In tbs lines from the eotxverfeor to tbs eolisms, in the hops of WATER PCB-SD0000046252 Process in Detail, eontd Conversion* eontd 35 attaining the saae degree of reaction with usefully lower pot te^mruturee* so that the pot*, would last longer* (Ths vapour* m tfaaa mlts mn be board roaring Into tb lead trip)* This is oxperiasfffltalj, and exparioaeo is showing that the increased pressure on the convertor gasket any muse trouble# which outweigh the possible advantages, Mr* Ellea- burg1 letter of tec*2,4/49 states that two orifice plate of stainless steel 1/" thick are used, ms with a 1*31 orifice between lead trip and w&pow pip and the other with a 1,14" orifice* between vapour pipe and oolwra* This arrangement gives the required pressure drop without using too bbb.11 an orifice* !Pfaa pressure gauge ea the vapour pipe thus reads the pressure between the two orifices* * Mr, EUeaburg gives the following comparison of conditions with and without the orifice plates? Gauge pressures Location of pressure gat^e *0.10 unit old conditions So.12 imit with orifice plates After #1 preheater After #2 preheater After Converter After 1st orifice plate After &&A orifiee plate 1 r- (column) -- ` ----- 29 psig 18 --- 3 46 psig - 33 21 13 3 Converter temperature* in the ^pressurized pet were around 785-79000 for X7*5pj eoofflrsim. The lower tm>eratures nay save a little fuel gas as wen as lengthening the life of the pots* and in the early runs* the deposition of carbon in the gas passages appeared to have been greatly diminished. In ibveAer 1950 preastffes tb first orifice plate* to 20 psig were observed after The followiac operating condition# were reported in September 1947? "The bmsene pu*f> deliver at pressures of to 100 psig* and the benzene reaches the first lead pot at . about 50-60 paig (fall in presstn* through the con trol iitrtB#@tti) * the second pot at about 38-45 Pig* and the third pot at about 15-25 psig* and leave the third pot at about 4-7 psig# the drop in pressure in each pot being duo nalnly to the hydrostatic head of aoltsu lad,. nc\Af dcona-i WATER PCB-SD0000046253 Proeosa In, Dotoll, oontd Oottverglon, oontd Batwal gas la used to boat iha convertor* aM stills aM thar Is a separata gas aeter for each unit. Thes* asters are teetailed la the room mentioned above, page 31* which also contains the hemeno flew controllers, fhar^ 1m a step cook on the gas min. immediately inside the room, with a long handle % which it could ho operated from outdoors, Th min than Ms a branch to each xmlt, each branch haring its own step fairs* then a pressure reducer. The line then tranches agate* otse branch aerring the burners a the #1 preheater, under purely mnl control* and serving the pilot burners 00 all the unite, and the other branch erring the control ralrss for So.2 preheater and the convertor. f$e@ page 107 below). The flue gases from the #2 preheater and from the onvertor go downwards to cross flues leading to the bottoa of the setting of #1 pr@hw.ter, so that that wilt gets a good deal of its heat fro* the flue gases. The #1 preheater setting has gas burners of its 01m to supply any additional heat needed and for use la starting from cold. The tesper&tures of the lead in the two preheater pots are controlled hr hand operation of the gas valves, but there is a high temperature alarm which would cut off the gas os #2 if the temperature should run away, say, by leakage of benzene vapour into the furnace, See also under instrujaentation, page 107 below. Typical operation records arc given on page 51 below. 36 qSVM 462092 WATER PCB-SD0000046254 .i Process Sn Detail, o<mtd 37 got# oo Starting'a Oonvoraloo tftiit H. L, rdea* Align* t l$50j reported as followsi "Th start-^ was witnessed of a diphenyl imit froa cold; after leaning and Minor repairs , The following Instructions apply to as Aonistcs salt using natural g&a, Other fuels my TOo#fitate alight nodlfioations, ^ut on on bwraar of each isiit, Throttle back until war eomigh to keep alight, The use of the pilot light will assist in keeping the burners alight. Flu gas is to go up the by pass stack to avoid burning-qp the vaporiser oil. All vesta on the convertor should b open in the early stages of warming i^, Aa the setting warm u& the other burners are lit one by em* till all are alight and burning steadily* Burners are ad justed (by hand or automatically by controller) to obtain fcha desired takers.tores, Only the convertor temperature appears eritioal. Vhen. tereturea are approximately correct* start 02 through vaporiser* the preheat vessels and convertor to the eoltsm and out by the column vent. Divert flue gas from by-pass to vapouris er to wars up the lattexy and close vents on the preheaters. Pressure os the preheaters should then build yp and enable leaks to be discovered. Development of d ,20 pslg on Hol and , 10 pslg on Bb.2 takes about f - bottle of COg and it is assumed that the pressure build-qp is-a sufficient guarantee that the air has been adequately purged, There should of course be no pressure to speak of in the convertor if the column is properly vented. Than* provided tesseratures (inclu ding vaporiser) are about right* tit off G02 out in benzol feed at a low rat (60 TOO- per hour). As soon as the lead * trap begins to Make* Indicating that benzol feed has reached it* lose th* colt*, vent* put water on the condenser and open vmlvta to reflux split box* benzol rtm-back and biphenyl iln to ertad tank. The latter line mist be hot before start ing tmtil tuffieimxt feed of crude diphenyl is available to prevent th* line from asking "Cautiously increase tbs beazeno feed by approximately 10 TOG per hour every half "hour or so. The governing factors in effect i^thiji Increase are mlntenanc# of preheat tmuper&tur (which tends to fall a the benzene feed increases) and th avoid&nee of high convertor te^>@ratwres, . "Th preheater nst on no account be aUetred t eccl to anything approaching th malting point of th lead, mxlmm tet^eratur of th* convertor should be 830-8^0^0 (800O If operating under pressure). Th* bonzeo feed should also be looked frequently until oofiAsao ia established because any echanieal or electrical here will cause a suck back of lead into the vaporis eoU," ns\N 462093 WATER PCB-SD0000046255 IVoces In Detail, ontd 38 ffote on Stopping Coorera ton tfolt It is of course iEportant to prevent ingress of air to th wait* and to take are that th load is not farced `backwards through the aystea by allowing the pressure to fall at the inlot sod of the system, When the gas burner have been cut off, the hmx&nm feed is stopped,' and GOg is forced into the benzene inlet line to the Tapourizer until liquid ceases to condense in the convertor condenser* A full bottle (about 5$ lb) of CO2 1 *d During this period the tmcondensed gas stream, oosisting of hydrogen and some GOg, will hare been going forward to the hydrogen ospresaioa system, to prevent the loss of its content of benzene, sad the COg-hydrogen mix ture mj be Tented to waste after ogression and eooling. When th distillation eases, the system is closed off fTeta the hydrogen collecting header, and from the crude diphenyl tank,* and the run-hack line to the benzene recycle feed tank, and rented through th pipe which passes from the top of the reflux split box to a point above the roof* The costere ion unit my then be opened tip for inspection and repair. DSW 462094 WATER PCB-SD0000046256 Process la Detail. eoatd 39 gota on Emptying a Lead. Pot Hhoa a pot haa to be en>tied, the usual shut -down routin* is applied, the system allowed to cool a little, the pipe joint# and cover Joint broken, the space on ih* ground floor below roped off for safety, then the eover, with its dip-pipe . tlunu well hoisted out by Beans of a etim^ bolted to the central flange. The lead in the pot is, of course, stHl jboX- ten, and & little drips off the dip-pipe. The cover is laid cm the floor in a convenient place. The surface of the lead in the pot is usually covered with floating solid debris, and this 1b dredged out by means of the long-handled perforated ladlt (see sketch #1) and knocked out in the well of the box frame <sa the furnace cover. It is convenient to remove the lead trap, to make room to work, and in most eases the trap win contain lead which has to be melted out as described later, page 92 and will contain solid carbon, iron oxide, etc. The lead molds are made of channel Iron, about 2" deep overall and up to 36" long, 6W wide, with sloping ends welded in. Tea of these molds are then placed, five on each side, near the top of the pot, and two coloured men take turns to dip out the molten lead by means of the imperforated ladles, (see sketch 2) and pots' it carefully into each sold la turn until all are full. This is rather hot work, especially in Sumer, and the ladles of lead are rather heavy, but the Job is not too bad. The operator uses the edge of the pot as a fulcrum to lift the ladle, and steps backwards & little, dragging the idle upward tmtH he can get a sufficient purchase on the handle to lift the ladle over to the row of molds. He wears & face msk, and leather gloves, but no other protective clothing. The lead mj spit a little if there is moisture in the Solis, and casual passers-by have to take care not to step into the Bolds. Th ladle handle is occasionally wiped with a wet rag to cool it. When ten molds are full, the two men. take a breather for about 15 minute# tmtH the lead has frozen over (tested by poking with a rod), then the molds are dragged a few yards away, and inverted to dts^> the ingots. Double handled tongs are used. The mold# are then refilled in exactly the same way, and so on until the pot is practically eapty, about 60 ingots in all. The pot is than hoisted out of the setting by means of a sling chain, bolted to the eot^anion flange, care being taken that the bolt# holding the halve# of the flange are still effective, and the pot is rum along until it earns a over the hinged part of the floor, so that it osn bo lowered to the groimd floor. C^re is taken to close the hinged part immediately the operation is ended. DSW 462095 WATER PCB-SD0000046257 Handle b of 1" piping 3/16' aetal, r holes Sketch Ko.l DSW 462096 Sketch Mo.2 WATER PCB-SD0000046258 c Fmw in Detail# eoatd *0 Bote m l&n>tyliig a Lead Pot, eooM - So#ti8 a pot la wjtM with the lead still in it# for exa^le# if the distributer asseaMy wlU not break: looro because of mrhm incrustation^ or if io\md pot la to bo red froa cm sotting to another# but inch aaoa are quite rare* The load would be allowed to solidify before the pot was Mondi The twml procedure Is to tele out the lead as described abort ' The lead ingots wmliy Iwtb tbs oXds quite easily# and they art stacked tmar the unit until th new pot M In place# then they art packed# on end# in th pot# and melted down# and any lead needed for Is added,' The.eorer with the dip pipe and thermo well can# of course# be lowered into position only while th lead is molten. DSW 462097 WATER PCB-SD0000046259 c Process ia Dotal!, oootd - goto on the Maintenance of the Lead Pots (See also tbs notes cm itea #5, pages ' below) * 121 The practice shoot* , pages 12Q, Mjelow, giro bow figures for the frequency of repair*, 1 The first preheater with Its welded-on over, low vapour roloeitlea and relatively low tesseratore can mm for years without attention, The second preheater, and More particularly, th oarertor, suffer fro deposition of carbon ia the vapour passages f the cover, damage to the dip pipe, thermowell, and baffles by high temperature and by the mechanical and. possibly corrosive effect of the lead, failure of the pot wall, usually by corrosion-erosion fro inside, at or below the level of the lead, era eking of the weld between the pot and its tSm (this weld carries the weight of the pot and contents and there is continued gentle bumping of the lead, and vibration of the pot), failure of the over gasket or warping of the cover flanges, and fro entralnsMst of lead in the vapour stream. If lead comes in eontact with the outside of the pot, fro* a gasket leak or from a perforation of the pot wall, it my cause Barked erosion, apparently from the solvent effect of lead oxide on the stainless steel, but this is not a mior came of failure. If there is a partial blockage in the vapour outlet, it my show up as a darker patch on the glowing pipe. The pipe leav ing the convertor needs cleaning about each 3 weeks and that fresa the second preheater about one every 8 weeks, Carbon my also build t^> inside the cover, x-oimd the vapour exit, or ia the orifieea of the baffle plates around the distributor. The baffle plates slowly sag, apparently purely from high temperature, A convertor pot usually maw 5 to 9 weeks before needing overhaul. The earbon nay be bwnt out of a pipe by heating with an oxyaoetyleoe torch, then taming off the acetylene, but oars must be taken hot to overheat the metal when the carbon burns in the oxygen utreaii, and the welder should take are not to breath too much of the vapour. There has been mom discussion of possible overheating of the pot walls above the level of the lead, but apparently the splash ing of the lead on t tb mils does a little cooling, and of eeta4* tbs furnace draught i downward# in the eases of the 0S*d preheater and the aarertar, Jtr, Barden, August 1950, suggested to Anniston that a stream of eOg, passed through the hot converter, might reaov the carbon deposit by converting it to carben. nonoxide, Anniston have DSW 462098 WATER PCB-SD0000046260 Process In BstaH) eontd Kota on the Maintenance of the Lead Pots, cemtd 42 ttdo a few trial of this, % passing two cylinder* full of COp through a unit coca a weak. and though the unit finally eboked with earboa* it was believed that the choking had bean delayed by the use of COs Although the pressure Inside the convertor Is relatively. low, the joint of the convertor cover gives a great deal of trouble, because the tesperatur 1b near the yield point of the aetal. The edges of the cover gradually bend downwards and the edges of the eospanlon (backing) flange under the pot lid bead upwards until they neet, and the gasket bo longer holds. The gaskets on the convertors are node up from round braided asbes tos rope lm in diameter. See page 87 below. Leakage of lead from a defective pot will probably be detected first as a drip of lead from the furnace casing, (Note that it my drip fro the wrong casing by penetration through cracks in the furnace setting, and care should be taken to examine the undersides of all throe pots before deciding which actually is leaking). The pressure gauges on the pots my help to Indi cate which pot Is losing its lead. Leakage of vapour into the furnaces any show up as black smoke in the stack, or as an Increase in furnace temperature. See also the stack test dis cussed under Item. 6ks page 91 below. If a pot Is sound in some parts and defective in others, it my be made good by welding, for exaej>Xe, a new bottom amy be welded in," A pot which baa seen service in, the #3 position lay be shifted to the lighter duty of $1 position and so on. See notes under Corrosion"* page 22 above, for an account of the corrosion of the pots. DSW 462099 WATER PCB-SD0000046261 Proofs in Detail, oontd 43- . The fcirtitt4 of vapours and hydrogen leaving the convertor pot passes through the centrifugal lead trap, item #7, tcher mat of the entrained lead separates, and Into the bottom of the fractionating solum, Item #8, The mAerflm of the coIumi leave* via f#9) a carbon trap, through steam Jacketed line* to on of (#10) two sub tanks, These tanks are vented to the "off-gas* line from the top of the colums. At the top of the column there Is a (#11) Condenser and (#12) reflux split box, with an equalising vapom* line between the two, The reflux split box Is adjusted to give a benzene forward flow containing at the aost a few parts percent of diphenyl, and to give an laiderflow of crude diphenyl containing a low a ben zene content aa can be attained. The Anniston report 1642, Oet.15/^1, states that the crude diphenyl flow contains about 4 to 8# of benzene. Diphenyl still records seen in Hovesber 1950 indicated that about 17# of the crude diphenyl was recover ed am benzene fraction. See page 53 below. Hr. A. K, EHenburg, Hdr, 12/47* wrote? m The reflux flow is used to control the temperature of the mderflow fro the eoluasi at about 20CK>C. The reflux ratio varies according to the tea^eratur of the condensed benzene, --;--------(which) varies according to the length of ttms the condenser has been in service, A* the film build* tip on the water side of the condenser* the cooling efficiency drops off, and ope of the hot reflux must be used to obtain the same anrnmt of cooling. These ratios vary from JO/^O to 90/10----- The vapour line from the convertor to the bottom of the eolum has a branch for sailing the vapours for the purpose of Making the conversion test, (See below under "Conversion Test*, pag 75,) and another branch carrying a pressure gauge. The conversion teat la performed once a day on each unit, usually in the morning shift. DSW 462100 WATER PCB-SD0000046262 ' Prop8 la Detail,, contd Treatment of Off-gas Sbi off-g&a fro* the convertor column*., consists of hydrogen, saturated with becsea, and It goes via (#25), & finned cooler with water Jacket, to (#26) & surge tank, from which It goes to either of two coaprosaor# (#29) The oompreasorB work In two stages, 60 pal and 300 p&ig*, and the spresaed gas from the first stag goes downward* through a vertical interstage cooler (#30) to & lw pressure tank (#31) oaadense4 Scaxea Is deposited, theft the hydro gen goes on to the second stage of eoi^resaioa, After the ootid stage th gas goes downwards through the second cooler (#32) Into the high pressure tank (#33 i where It deposits ore 'bmx&m* The surge tank (#26) has & 55m water seal to a hooded rent pipe through the roof of the ooppressor room, and there la an autoTM Katie control instrument which mintains the pressure la the urge tank between II and 16 os, per aq,In, aboYe atmospheric* by reacting a the unloading valves of the compressors. The benzmw which collects in the surge tank gravitates to tha bemesa receiver* (#27) and that which collected in the pressure m fomerly discharged hr float traps, .also into (#27), but th# trap seating* failed by corrosion, see page 1 03 below, and tha transferrenee is now done at about hourly intervals by swans of hand-operated valves* The pressure vessels have gauge glasses, and the discharge lines have sight glasses. Corrosion of copper and alloys in the hydrogen ccspreasion system Is rather Barked ss& I attributed to the effect of HgS. See page 101 below. Oxygen determinations were made on the hydrogen at fir*t, but are no longer thought necessary. After any shut-down, the hydrogen is vented to atmosphere and the system purged with 400 ettoft* of 00g.- At Plant "b" there la a hot wire combustible gas recorder permnmtlj installed in the hydrogen stream going from the chlorine ceUi to co^iressar for the hydrogenation plant, wired up to stop the omweesors if acre than & trace of oxygen is present in the hydrogen stream* Mr. ELleaburg, June 30/W, wrote 1 DSW462ioi ", ---------As you knoif, oiff Worthington eomxreaser has tiro stages cad operates at 150 palg aad 300 pslg at the dis charge of the low and high stage respectively. These presets?* are not critical and the choice of pressure* depends tram. the size of the cylinder ohaabss? a* well as the amount of'gas to b# handled----", gee bb!p itaa #29 below (page 101) for him forther remarks. WATER_PCB-SD0000046263 Procea la Detail, coatd ^5 Diphenyl DlitlULfttlon Crod diphenyl in punned through stea* traced lines from the up tanka to either of two horizontal diphenyl batch stills (#13) Each still la fitted with (#13B), an external gwhmt&d coil, on the side of a fire wall remote fro the till, through which the charge I circulated by sessna of (#12A), a subasrged centrifugal pta*i. The "spread" or ten- ' peratur difference between Inlet and outlet of the coll 1 automatically controlled through the gas supply to the burners* and Is automatically recorded. The controller is set for a spread of 20C, but when seen in Bovember 1950 it was manning at about 16 to 18 spread, i,,e. the heat Input of the buraers ms falling short of the control limit. See under "instrumen tation", page 108 below, for details of the control instruments. A typical still charge (Sept/Hj) was 3400 ISO crude diphenyl plus 450 WQ recylod "heads ft tall" fraction, and the a till cycle took about 18 hour. The vapours pass to (#l4) a 20 plate colinm with (#15) conden ser, and (#16) reflux box working at ateespheric pressure. Out are taken based on F.P. determination, (but see Mr. Barden's coneats below). . The reflux Is changed during the distillation and the follow ing Is typical of operation (in SeptemberAT) * At Start Benzene Fraction. (tf> to 80C at top of column) Heads Fraction Mpheayl Fraction Tails Fraction Reflux / Product 100 0 25 75 50 50 30 20 IS Mr. Barden, August 1950, however, reported! "The total reflux .period seems to be practically, confined to the still charging operation. The still and eolvma are usually still hot fro the preceding batch and the Incoming charge starts distilling Immediately. Total reflux operation at this stage rapidly cool* the column. It can happen that tht* Initial distillation i too rapid for the split box to deal with it. In such a. owe It is usual to relieve the box by sending a portion to the heads and tails reeeiver for return to the still. It Is essential to avoid sending any of this initial dlstiXXate to the bear to recovery system lines it la liable tp be contaminated with diphenyl and so lead to excess production of high boiler*. The charge used at the time of the visit ms 38OO Q5Q of crude diphenyl and heed* fiiid WATER PCB-SD0000046264 Process In Detail, contd Biphenyl Distillation, omxtd H6 "tails fro* previous mm (about 4,200 red total). *8cm exeesi pressure I pt to <fevelop at start of distillation* presumably by plugging of oad@a$r by tudensat# If this is observed, a -rent is available for temporary relief* This pressure build-up was not apparent to th@ writer but t2 operator elained that 2m eeuld teH by the flow in the split box. "Oireulatlen through the oil is started before light ing burners* As the system is usually hot, the tanM an be put fall on quite quickly, The burner are controlled by the "spread* between inlet and outlet te^wsretur This Is aormlly set to 2O0, but Is re duced to 10-15G when distilling head to InIIae carry ever of good diphenyl. ' "Officially, the change-over fro heads to good diphenyl should b based on (S'.Pt. (684o). In practice it is usml to change-over arbitrarily after on hour1 dis tillation because the tine spent in testing staples Means unnecessary diversion of product to heads for redlstillation. The arbitrary time factor obviously depend on distillation rat and my not apply cm another installation. "Similarly, the tail fraotion la cut out as soon as tesiparatur (i#d epmlmn hart) Indie&taa need, as delay in f.p. deteriimtioM result In eontas&natlon of good diphenyl. FOTtbswior, it 1ms been found that f.pt. can be 0*E, but boiling range out of specification if the cutting out of tails is delayed. ISenoral rulMt- ' Wm top of eoluan tenpemtur to out into heads, We ilJ and coil inlet teac@re.tur to out into diphenyl. W@ coil inlet im>@r,twr@ (3^5"355) to out into tails. W# top of eoluBn to^wature to out off tails. * 5h@ fare m is beorene, which is mm off to (#21) a ea&U buffer tank (ituat#d near th# stop tanks), fpom. which it is periodi cally ptnf>#d totb* recycle food tame. ' DSW 462103 WATER PCB-SD0000046265 Process in Detail,, eotitd 47 Mphetqrl Distillation, eontd Each 8 till has tbrea other recelrom t . (#18) B&sAm and ffaUs^ tdaieh. are pimped bade Into tbs still, hy moan of a aetaspgM pw, for the next batch. (#19) Biphenyl Receiver. K*oa here the finished produet my be pu^>#d by b&&b of a submerged ptn^p to storage tanks, to the Arocleec plant, to tank ears, or to a mb.11 flaker. (#20) Bottoms Receiver. Crude Saatowax Is ptmped here at the end of tne distillation, taing the submerged pusp of the tlXl8 This Material my be ptiaped to the Santowax till or drawn off into drums for permanent tarage. Excess material my be pushed into a pood* The distillate flows through (#17) bbsII open box from, which it my be saapled and diverted to either the diphenyl or the ''Head* end Tails" receiver* The benzene fore rmninp by-pass this box, Each of the* three receivers is fitted with a steam coil and submerged pts^? A typical operating record is given on page52 below, and a mrmsmry of records on. page 53 . This record includes figures for the reflux ratios need. A sasple dart from the Multipoint temperature recorder was sent to Mr. If, M, Cooper, In London, Oct.31/47* Anniston recycle the cooling water la their eondens@s?j at atmos pheric pressure, cooling it in a separate hmt exchanger. This is to prevent scaling of the condenser by futurities from the pond water. They rely simply on hand control of the cooling water to the boat exchanger to give sufficient condensation without causing freezing of diphenyl in the condenser. The te^arature of the recycled water need not ordinarily- be above the freezing point of diphenyl, but it is allowed to rise to 80"85C during the collection of the "tails" fraction. Instru mented eoota*ol of the cooling water was abandoned in favor of hand control. The benzene distillate Is examined before being pu^ed to the recycle feed tank, to aobi mm it does not contain more than 2-3J5 at aort of diphenyl. The operator* Judge by a greenish colour which appear if there* mmh diphenyl, and toy evapora ting a few drop between th Ungera, but a freezing point test would be the safer criterion. The diphenyl my have rlished over at the etarfc of tht dllstillation, as described on page 45 above, or my have Co* over through inefficient fraction ? Insufficient reflux). WATER PCB-SD0000046266 DSW 462104 Process in Detail. eontd m Diphenyl Distillation* confcd Tim build t* In the heads fraction, of mt ariala other than hmx&rm and diphenyl 1m very alow (only about 0.065^ on the diphenyl according to Anniston report 164*4 but a* the frac tion la recycled to on batch after another, mtjrmw and otiwr eontaatlnaata do alowly accissulate in it* (see under "Flow Shoot** pag# 28 above* for typical values; aeo also page 116 below)* and the.out between benssen and diphenyl becomes leas sharp* Occasionally therefore a heads fraction ut* ttom about 900 to 2QQG aammting to about 10 gallon* * is side-tracked* allowed to cool to deposit diphenyl* which 1 drained off and returned to the aya tea* and the liquid con taminants discarded. Kr, EUenburg* JUn, 14/49* la answer to & suggestion fro London, agreed that the heads fraction sight b accumulated tmtil there ms enough to charge a still* instead of being recycled each tine* but he advised against that course on the grounds that & larger store task would be needed* and that the Anniston Bathed is general^ Bare conveni ent. Any impurities boiling lust above diphenyl will go into the tails fraction* but this fraction is simply recycled so that the im>urifcies finally go out in the crude Saatowax, Mr. Slleaburg advises against handling or shipping diphenyl in dross because of the difficulty of re-melting. Anniston flake any diphenyl not handled in tank can or by pipe line. London* Feb/49* did not expect to sell any diphenyl, The diphenyl still bottoms (Crude Santowax) are kept molten in steam-heated tanks If they ar to be processed further. The excess production of bottom at Anniston Is put Into old drum* and more of it tea been pumped away into an excavation. If the stored Material is needed again* it is put into a melting Pot and then moved by pinning. At on time when smaller (direct fired) stills were used* Anniston purged the diphenyl still system with COg between batches* but discontinued this as being tsmeoessary with the present stills. The still.is simply allowed to cool a little after being discharged* then a little care taken in puspiag in the new (hot) charge of erode diphenyl. Still bottoms* discharged at about 400C have been known to take fire. The circulation, through the heating eoH is not started until the still tea settled down after the charging. DSW 462105 WATER PCB-SD0000046267 Process in Detail,, mtd 49 Distillation of Santowax This is carried, out mder about 50 ** of Bg absolute pressure . at the reeeiwer* using a DsYlne Yhetmm Ptaap (#40), The pro at &quljmmt was originally set ^p for the separation of erode S&ntomx into Satrfcomx 0* K and P* which are crude ortho* net.* and para, isomers of tes^pbeayl. For S&ntowax R only straight over distillation is required* with a single roooirar (#39) instead of the series of receivers Installed in tbs present plant* Th still charge is reoeiwed at about 150C in one of two Charging Tank* (#35A and #35B), These ar interconnected at a low leTel and really constitute on Teasel* They contain heating coils and one has a submerged puagj (#3to)* fey which liquor is circulated through (#3^3) aa external preheater coil oa the side of a firewall remote from the tanks and still* The coil is heated by gas burners and Is suppprted in a steel flu with firebrick lining* The material is pre heated to 230G The same punp is used to transfer the hot liquor to the (#35) still which has a similar heating arrange ment, The still capacity is 6-7000# of crude; The still has a 10* vapour outlet (and explosion disc) to (#36)* 12 plate oolmm. This colmm. has (#37)* a condenser consisting of a -single Jacketed tube in the form of a zig-zag. (See pages lot & 105 below), This condenser was used in place of the original shell and tube condenser because the latter often became blocked with frozen material * There la a reflux split box (#38)* but reflux is used only la the' (rough) separation, of crude Saafowix into the * a & p isomers. The Santomx R distillate is m frets the receiver (#39) to the buffer weasel (#39B) aM pa^ed from there* by (#39A) to the Aroelor plant* the Santomx R flaker* or to the RB-+0 plant, as required* The still bottoms are sold as Montar 9f any excess production being dm^p#d , Er,, Eardy reported* Oct * lYffyJ : *A totel forward flow is mintained on the split flew box throughout the Santowax R distillation.* This is nece ssary in order to get over some of the higher boiling constituents which boil abowe the terpbenyls* These mterials mist be present to bring the hold point of the Santowax within w specifications * *0ur original Saatov&x still tod no reflux at all and the new still (19^3) 1* supposed, to duplicate the product of tbs old still* DSW 462106 WATER PCB-SD0000046268 Process la Detail, coatd BiatlXiatlcm of gantwax, oontd 50 . Distilled Saatow Is a reddish town liquid crystallising to a yellow olld &t ?o<sa te*s>eraturea 5h AlatHlatioa la aontrolled bj "Hold paint determinations -- there are two Ueh point* aai tbs speoifioatlm for th pro dust requirtmi %pr hold point 13T-1^3C (changed Sept. 23A7 to 137-l*5c) Lower hold point 45-6oC (changed 3apt.23A7 to 45-630) A sa*pl strip of to^eratur recorder chart for various points on the Saatowax still syatm was seat to Hr. Cooper, Oct31/t7, On Janoary 6/k9 Mr. A. M. ELlenburg wot#: "At me tine, distilled Santowsx was allowed to solidify in drum, &s*d shipped, bat it was noticed that the pro duct tended to segregate as it solidified. As a result, the outer layer of the drums contained the high Belt ing portion of the Santowax R, and the center of th dm* was. *ade tfj of the lower Belting fractions, "in order to obtain a uniform product, so that a whole drw would Bot bar* to he salted to get out 10 pounds, the Idea of flaking th Santowax was proposed. A chili wheel is used to cool the material, and a blade scrapes the mterial off th rolls, front which it falls into hags or lined barrels, (Hot#, however, that Santowsx has two "hold" points in its eryitalliiatioa curve,see page 13 above, and gift#a first a plastic mss at about l40C, then a waxy solid at about 5O0, a fact which affects the flaking process. Elf.) 'Shi lx*py material results because the Santowax is not chilled sufficiently before placing in th bagj, and a slight fusion f the flakes results. However, the partial chilling is enough to give a uniform solid product. The rod Saatowax could be handled a similar way if necessary, because its characteristics are similar to those f Saatomx Me A big tank for storage of the molten erode Sms of course, th easiest solution to a storage prbl@*R Amis ten, Janl%A9, pointed out that the Santewax flaking could be done on the sane drua as the diphaoyl flaking. See also the note under Specifications & Test Methods, page 6j below, ' 46^ 07 WATER PCB-SD0000046269 --J-T c 5i1 dtN* < rv 2" iff X- M %j 1 11 \ V" r\' M K-jv ih \' .\ > : \U^c * ,V : i ,<3 'V UV *0 ^ y * g YT v U^ *n \ V V 0 uh. . ^ orX .. -j v r> ;- -* ^cb3C E > , Os o. r ** N 7;iV i .| s - ____ . *' - ^ 1 - W v Tr <V fk. !k:j tN gtvl--^----tv*- , - " Snboi. ^ - , ?LL^s>.___l_cL tv__i _N_ctv_.__'_^t-V , CS >- r< >, r_ , ft . 'n . r- v * W r-^ rT * " <ri "3k . * r\ 'O 'ri ;-a *K K-^ s Uv 462AQa WATER PCB-SD0000046270 Diphenyl Dlrtllllatloa Beoord DirtilHatlon Ko< Still Ho. cams: 7 &'S' -Data Start* Operator Start Operator Tlnlah Starts* Charging Still at / ///i 'dT/?yt, __** 2_ _Shift 3 _Shlft HtT Tank; inched before -7 V inchea after J-S ' gallons ohArgid 7 3/6 No. 1 S,T, Inchea before . ^"7 Inches after gallons charged,.? / U-- No, 2 S,TT lnohsatbefcre No, 3 S.T. inchea before inches kfter inchea after /( gall one charged g.ojlona chargo-l No. U S.T. inches before Benrol Still " " inchea after lono ciia~r?.\ inchea after gallons charge i Total Callona Charged 4*.o b a ! i ' Circulating at /7.5 fire on at /i/ xl- Fir.i ? Tv S' TTTNCS", i. on // r t 5. On *t 7- ^ ^ ? 2 On : f at /2; , 6l On 3. On S ? At 3 q. 7, On at k. On ?0 at 8. On at BENZOL: HEADS; TAILS; Ban J11_________________ or __^jC1_ gal. Starts* orar at . tfA M Jlall>d at y A -H Ban _________Z___ f_ or /Z.IS' ' /VStarted orer s.1^/7 j&< ^7 .V/ . , rinlahed at if. 7 7>,' Ban __J0______________________" or 7____________JLb. DIPHSHTL: Total in DiatilHatlcn of.ifl ib. ETCS' BOILB: Crow Weight Mr Weight 7//-' _lb, 3. of Dr-wa* lb. DSW 462109 WATER_PCB-SD0000046271 ( Prooegg An Detail, confcd SiMmry of Roeards of Diphenyl Still Working 53 (Taken November 1950 from th plant sheets as on the preceding page) Sew Material to Still U'.S.Q&Hoq 3*85 339* 339* 3*85 3869 339* 3*85 3*85 3576 3*85 3*85 Benzene Fraction offU.S.Q. *37 598 667 506 690 690 87* 598 391 598 598 Heads Tails lb lb (8 Ib/tEO) 202* 96* 1928 2121 2217 1157 1157 1**6 2121 .1157 2217 2121 1253 1350 202* 1253 231* 231* 2*10 1157 1060 1350 Diphenyl Bottoms lb lb 18,785 17i*59 15,*70 17,680 17,238 17,017 16,133 16,796 15,2*9 19,**8 18,785 **-00 5*00 **00 5000 *600 *600 -- -- -- *800 *200 DSW 462110 WATER PCB-SD0000046272 SPECIFICATIOBS AMD TEST METBOEB 54 Raw Material* Benzene In Septenber 1947 Anniston were in a favourable position in respect of the qmlity of the benzene received,, By a special arrangemnt with the suppliers in Birmingham, Alabama* they reeelred material usually running 5390 Cr.Pt., (on the sample "as i*), and at least up to "Hitration Corade" on all other points except possibly sulphur content. The arrangement was so good that Anniston were able to rely almost entirely on Birmingham control of the qmlity of the deliveries. The only specification was that lulled in the description of the mtari&l as industrial Grade Benzene", and the deliveries were so stueh above specification that the specification was inopera tive, Became of this position Anniston do not perform routine testa on benzene deliveries made to the diphenyl plant. There are only very few test reports on file, but the following which were available were believed to be representative of the mate rial usually received! Tank # GATX 3, A6l Date Fr.Ft.C 8pGr,@ 60F. Dist. rung 1st drop 79*7 5?S 80.2 50% 80.3 95* 80.4 dry 80.4 Colour Water white ash test #1 Total sulphur * 0.05 Acidity wg H&OB/g HgO p.p,*. Paraffins GATX 21357 80.4 80.5 80.5 tr.w, #1 0.05 ? Aug^FT 0,8825 0.9OC 79*5 80.2 80.4 80.4 80.4 GATX 19403 June 17/48 D *rO 0.886 l.C (corr.) 79.4 80.1 80.3 80.4 80.4 w.w, #1 0,0004 700 nil The freezing point method used was that of Jtl.E.Ch.Vol.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 Ruabon method, and to nak sure that the Anniston Material really had such & high test, by British test methods, a eanple from rail tank GATX 21357* Hov/47, was sent to Ru&bon. It was found to have a crystallizing point of 5.4 G by the standard Rmbon method. QSW 462111 WATER PCB-SD0000046273 8peifToa,tloag fc Twt Methods, contd 55 SajqpXesj representing material available in. Britain., bavs ' been axa*ned at Aimiatmi F*.Pt.C Sp.Gr#5oP Diit, range 1st drop 5$ 50$ 95$ dry Colour Wash. test Acidity ag BaOH/g HgO p,p.x. Paraffins Sample 2279 Takn **,24/48 5.16 0,886 79.6C 60,2 80,3 80 A 80 #6 v.v. #9 0,0016 4-58 * Sanple 60768 Taken Jbly 27A 0,^3 1,2 71.4 80.2 80,2 80,3 80,6 w.w. #4 0.004 621 nil (oarr, Aimiston* eoesMntB on the British a^>l HB279 wer that it u not up to th@ quality of the Annie ten supply,? it had & high acid wash colour, Indicating inoo^>lt acid, treatment, and the presence of uaa&turated or hydroxy oc&pounda, but that It should give good diphenyl if the fractional distilla tion of the diphenyl ware good enough. The saspl left an dour of tar at th* end of the distillation, Anniston fs easmsat on British gsi^le 60768 were that its &ed wash test was Just at th limit of the Anniston specification (for "iMua trial BasasR) again indicating Inooa^let acid tre&tesnt of th material, Baterlal t this sample would pro-" dune good dlphmsyl, though a little extra attention to th diphenyl distiUaticm might he needed# Th effect of iasmrifcles in th bensem were discussed in Anniston reports 1640, p.19, & 1642, pages 1 k 2# For a time no very.high standard ms set, but in recent yean, trouble with the stability of Arcolors used for electrical work Ms renewed the interest in this subject. See pages HI- below. In a "hart form report *, No,2152, dated Hoveirtr 17A7* &* A. M, KUenburg of Axmlntm. reviewed th quality require ments for beaxeti for soJdog Biphenyl and Chlorbenzenes, He toxmd th available evidence to be inconclusive, and reconnonded maintaining a Halt of 5#0C misxlmm for Biphenyl and 5,2C for Chlorbenzenes, J>. 2, B, Mrdy, Dec#23A7, advised caution in accepting a lower standard, for benrane, which contained paraffins, would nsw 1 ? WATER PCB-SD0000046274 c Spec ifleatIona k Teat B&thodg , contd 56 yield s^reoe and apparently rtnyl biphenyls * Bare again tbs chlorine darlratlres war blamed for skin trouble In the Arcelor plaat* Ho pointed out tint though the chlorinated products my b stabilized by being held at high tea5>eratrei. It is not certain that this process will go far enough* 0 April 28A9# ttt% EUenburg mentioned the beneficial effect Kileh high inp#raitiar@ii la ok Ten ar town to bay on tbs p*a*Ity of th# benzene (freedom fro* paraffins)* See also tb@ discus8loo. of Effects of Variation In Benzene Quality/ peg 111 below. ' Test Methods for Betgene yr.Pt* . A mentioned abor, Amlaton use the method of Ind.Bng.Cbem.lO., p1010 (20 o aa^Ie la the *&a 1*w condition, put In a test tube la an lee bath* and when the solid benzene begins to separate, the teaperatw8 will remain constant fnr a time* This tesseratur is taken as the solidifying point. Accurate 1 0.050, Other Test Anniston tme A.S.T.M. method,but on Feb* 15/^9, Anniston r~ pcried that the British (I,B*G) for* of the aeld msh test ms ilipler, especially in respect of the preparation of the standards* On applying the test to their own benzene, they f<nmd It to give a colour matched by only 0*1 g dichro mic per liter of water as against tb H.B.O, standard of 10 g The same benzene gare colour 0. on the A,ST*M* aeld wash test* DSW462113 WATER PCB-SD0000046275 Specifications & Tost Methods j contd \ Jjmd for the Pota Ho specifications exist oo load used in the dlphei^fl 1m<J convertor imite other than that "chemical load1' 1b to k ptcrohaaed, Apparently the effect which l^tn'ltlei In the lead Bay hare on the stainless steel, la sore' feared than any effect on the eoareraIon process Itself, Hr. V, V. Wade of Anniston hare the following informtioat "A analyst* of chemical lead a* *upplied by the St, Joseph Lead Cosp&ay, 250 Park Are,, Hew York, New York, mss Fbs 99*9272$ Cus 0,o6o8 Asi Sbs 0,0001 Sas Fes 0.0001 Zns 0,0001 Odt 0,0003 His Cos 0.0048 Ags 0.0066 Bis nil ^Kleaanti that should be particularly avoided, as observed la practice at Amis ton, and as recoasaandod by aanufacturer of stainless steels, are. In order of l^>ortancs tin, zinc, toismsth, antimony, and cadmium. Tin, nine, and bisjntfch should not exceed 0.0002$mx, aatlawny and eadaitat, 0.0005$ *lx. '' "Caution should be taken in plant operation, to avoid octaalmtion by any of the above elements, 57 Speetregrephie analysts has been found useful for checking the purity of the lead for the convertors, W are warned to look out for i^wities which nay be picked up in any reused lead. MOL hare found a sourc of supply of lead apparently up to the Amis ton standard except that the bismuth content is 0,001$ awl the lead, percentage only 99*9955, Anniston eoaet#d that they did not think 0,001$ of bismuth would cause any serious trouble. DSW 462114 WATER PCB-SD0000046276 Specifications and Teet Kathode, cont'd 58 Finish! Products Diphenyl coda 3980-5OO-74-Op t^ooSnloa.1) authorized July 16/45, (Saapled frost the mil tank, in supercedes Iter, 2/38. the eae of tank oar *alao) Production Dept. Ho. 09 Appearanc yellow to pale amber solid. Colour equal to 2.0j aqueous PaClo Ei&x; Pr.Pt. 6$. 7 adn. Dlst. range 2.5C. asot. including 255UC. Freezing Point of Diphenyl Standardised Anschutz theiuaosetor 40-100C. mounted vertically naar shaft of a email electric atirrr= Bulb about 1/4 " above stirrer blade, and 3/8* trots, the shaft. Magnifier clamped to thonnezie ter. Kelt and nix the cample, Pour about 120 o.c. Into 250qco Griffin bsalcsr making cure thermometer le not above lOOu. Set beaks-r under stirrer so blade 1 -1" above the beaker, and tho thermometer immerccd to 4oC. mark or more. Hun stirrer at moderate rata through tost- When cry stallization begins, the temperature will rise quickly about 0.4C., then become constant for 2-5 min. before slowly falling. Highest reading taken avoiding parallax. Dlst, Renge of Diphenyl Plant "B" method slightly modified by R.Sudhoff, Kar,8/37. 200 cc Pyrex (Coming 1600) distilling flask, Seek gr&pped with wet asbestos paper allowed to dry on, 200-275 rang precision Taylor type thermo, engraved stem 0.2 division. 1 * 4 am Both bulb and expansion bulb to be below the side tube, 6s auxiliary thermo. 0-150, attached with bulb 2/3 way down the oxergont stem, Cover both thernoo 0SV^ 4621^ WATER PCB-SD0000046277 Specifications and Teat Fethc-dHj_ oont d Finished Products, cont'd Kith 3/4" glass tub. Correct for emergent a ton, and baronetrii and' theniionctrio e>:.-rar* Condenser as for Barrstt benzol distillation., i.., 24" x i-* glass tube @ 75 sr^l in copper trough. V' ;r at 75-o5C. Auxiliary burner to prevent freezing at exit. Drift shield 5" I.D. x 6" high. Flask on 6" x 6" place of 1/4" transit board Kith 1-1/4' hole. 7op of auxiliary bulb of thencometer level with bottom of side outlet. Cork stopper flask to con denser. Weigh 100 g. s&apl* into flask:. Heat with K*ker burner till ebullition stortc. then vapour' ring re&chsn into the neck, but not to the side am, cool a little. Hap eat 3 ttrsea to gat fcb.err.ons ter and flask neck heated. Pistil 2 drope/asccad into broker on a balance. Read! . 1st drop 1$ J$ 5$ 50$ 90$ ## 95$ 96$ 97$ Dry * read auxiliary thermoz^ster at *. Record weight in receiver 1 minute after removal of flame. Dry- point: observe when last drop 2 a-' ves bottom -- needs two observers. (760 - Baroffl. reading } x 0.036 = ' (1st di'op - average of auxiliary r-sa dings) x 0.000153 x no. of degrees ftbove the bath * Tg Add Tj and Tg to observed readings. OSW 462AA6 WATER PCB-SD0000046278 ou Specifications and Test Methods, ont'd Finished Products, contrd Diphenyl Colour Kelt 120 g diphenyl in low form Griffin 150 co beaker. Compare @ about SoC. with ferric chloride samples in bottles of asm diameter as beaker. Standards 25g FeCl^-S^O 0.625 g OOCI2 6H~0 in 200 cc HgO a 15 cc HCI (S.tf, 1.18), make up to 250 cc. Rake Standards 1 H 2 10 cc stock per 200 cc 20 io 80 Standard Kos . are J^PeCl^'SH^O . Sas^l 0*4072 of Finished Diphenyl was sent from Anniston to Rmbon, 0ot.13.A7* DSVV 462117 WATER PCB-SD0000046279 ( Specifications & Test Methods, contd 61 tfr. Barden, Axigust 1950, collected the following test results At Anniston* "Typical Analyses* Diphenyl late Colour F.Pt. Blit. Rang 1 drop 1# 3 5 10 50 90 95 96 97 dry 31/T 1.0 68.8 0.6 254.8 254.9 254.9 254.9 255.0 255.1 255.1 255.2 255.2 255.3 255.4 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/V 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 le o8.9 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 18A 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 68.8-r 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. Slat. Range 1 drop 1 5 97 dry 25A 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 2.5 254.9 255.0 255.0 255.1 255-2 255.4 255.6 255.8 256.0 256.4 257*4 (1950) Test results collected In 1947 are given on the next two pages, 62 & 63* DSW 462118 WATER PCB-SD0000046280 TECHNICAL JDXPHOTL 3HXPXffT3 <mHp* 0bj 3c (X) 04 sH P * c-> o9\ 00 <-i co0 &HO OO 0 0 0a 0Q 0 Oa 0a i~! fH <H H H r-t a pSS-Pp-<- ONa tiPn CJ <H VO mCM CO tmn w CD*. ttnn CM o4\ ttCnnJ OeN ttnn (V ctmn cv SG\ GO ONs b~ h'J COa co0 vo0 $Cv t-- t'0- VOe VO0 t-a t~a tn o\ VO t-6 tr. VOc VO-i cn0 m6 G\ m VO tn* tn 9 tna m IA CT0\ to JCt & 6 <* e (O0 C"J m CO * CJO tn CJ0 4 r & CJ0 CJ C CW CJ1 fTM!r CJe vv CJ cvfl Cvi CJ O0 tH c 6 Tc-<Vt. CJ OJ rH-c 0c cv 0 O9 ft in ttrv< ILCTAJ. tmr. cv ttAn CJ iicnnw ttnn cw itnn p 7r--"rJ4 (3i> pOi H 0 D anS ft0 tn mOJ r-t in tCnJ 0 in tCnJ F~i tn tCnJ 0 ttCnnM c\ tOnJ 0. tCnJ 19 fX, s 0 Q5\ 00 MO ca\ CO VO oe\ cx> VO O0x Ox ox CO CO VO VO G4\ CO 0 st 0 mCh VO J*0 m Ocn -et*--rt 00 vmo Htn vo Ctn\ vo K tj 0d H 0 35 Kfc 0 X KEH < 0 h 0 3C b 2 b 0 9S bK 2 *t- ro 0 n. <gh 5` ,-n t*Cc~c *tt'rOr-5<i .< rtJ-a CHe\ n0 ea ePn p0 w S' 62 WATER PCB-SD0000046281 4 gf ( D C| ^ VO9 t-4 00 CD4 tre- g o H o O 0 HH Oo ss HH o tn c 6 ** r-f o O o fQc bi 'o\ 9 o\ 4 Ch VO 9 VO0 .n m tn m m m P (u in tn in LA n u\ cm CM CM Cw cv CM 63 & X t- CO CO 4* tn tn 0 TECHNICAL DIPHENYL SHIPMENTS & Ch 1 vo a t- h44 -=f* un e V. mCh \00 VO9 t--4 CM tn e J o\ LAo tA VO * VO CM -=f9* O tn w =*4 tn in4 in CO in CM iH CM 0 CM ro CO 0 Ch CM V, in :} CM CO CO Ch r-i 0 4 03 , c o P fH 4 fH 3* bS <H H S P h*j M CM .n n CM CM 0 eH H 4 in m a P P-i o fe ch 03\ X GO -a VO s - in X r-t 8 -( k$~ N CM H c 4> f*t dO 5n CO CO 4 CM cv CM H 94 m in m tn CM CM C9h Ch VCOD 0VO0 tco HH CO 0 iH e H CO9 in tn CM co Ch *stn in CM CM Ch o VCOD VCOh o Ch ` HCh H ri t~- t- Jt J4" \in H CM4 ft eg* w tn SW 462120 WATER PCB-SD0000046282 Specifications fc Teat Methods, eontd sAjmmx R The properties of Santo^ax H aa given In ''Monsanto Oheaieala and Plasties'1 - 27th Edition - are typical analyse. 6k Tentative Sales Specification Color 3*5 - 4.5 HPA Solidification. Hold Temperatures; U^P or Lower 137 - 143C 45 - 6sc Distillation Range; At least 80^ between 350 - 400C fxmeorr.) This property la not deterained on every lot. See also under "Properties of Materials", page 13 above. DSW 462121 WATER PCB-SD0000046283 65 Specifications and Tc-gfc Methods (ccvit :d) Analysis of Santovrax R DESCRIPTION Santowax R is a yellow solid hydrocarbon mixture of micro-crystalline structure. The main constituents are ortho-t.erphenyl, meta-terphenyl with smaller quan tities of diphenyl and tri-orthophenylene present. The molten product is chilled on a flaking roll and bagged or put in paper lined barrels for shipment. LABORATORY TESTS: 1. Color: 3-5 - 4-5 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 Is possible if the sample is heated above 250C for any length of time.- The molten sample la poured into a clean 15 mm test tube and the color is compared to the standard disc comparator of the National Petroleum Association. ' Changed 8pt.25/4 2. Hold Points: Upper hold point 137-l43C toj 137-145 Lower hold point 45-60C 55-63 Method: A 250 cc beaker Is filled about three fourths filled with the flaked. saapl and placed on the hot plate to melt, After the molten sample has attained a temperature of 175-200C, 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 80C. 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 times. 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-SD0000046284 Specifications and Test Methods (cont'd) 66 Analysis of Santcwajc R - Page 2 Standard therrx^etcrs are used In this test. No correction Is made for eten 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 flask, the flask is put in place and heat is applied so that the first drip comes over in from 5 to 15 minutes. The distillation shall be conducted at the "flte 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 350-40000, the per cent distilled over shall also be noted. ThiB distillation range specification is subject to change as aor-e history on this test of the prod uct is obtained. 4. Sediment Test: 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 see if Impurities were present. 0s\N WATER PCB-SD0000046285 Specifications anc- Test Methods (ecnt-'d) Analysis of Santovax R - Pape 3 For a fool-proof mvthod, a reachandeal means would be needed at the flaking r* Us 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 - * lings from coming off the rolls. 67 DSW 462124 WATER PCB-SD0000046286 c Specifications and Test Methods, cont'd 68 Extermination of Sulphur In Santowax Tentative Ilathod; 40 g. sample, 20 g. Nickel formate, 150 cc H.B. k0 (hydrogenated Santowax) in 1000 cc boiling flask. Heat 6 rat of 30-4oQC per minute to 285C. Vater- of cryat. of formate coaea out up to 200. Formte ' begins to deoon^poss around 240, and rapidly f? 270-275. Heat to 285 and cool to 20-80C. Add 100 cc 1:1 HC1 and seme boiling chips. Ueflux till II has dissolved, (foams), with Meyer or similar apparatus attached to condenser, 50 cc amrnoniacal CdClp (1^ of CdCl2 In'the bulbs. Hash CdS to bsoker or flask. Make acid to ; henolphtbalein. with concentrated HC1, and dilute to about 250 cc. Add 10 cc X/lO Iodine and 5 cc concentrated HCl added. Leave 10 minutes. Titrate iodine with K/l0 thio using stai'oh. Calculate to ^ sulphur in fantonax. Do blank. Determination of Chlorine in Santovrax 30 g. Santowax and 1 g. sodium in dry Ki crucible, 80-100 cc capacity. , Cover. Heat over low flame, until Santowax has gone, than to dull red. Remove cover and allow excess Ba to burn under hood. Cool, wash well with H2Q. Hake up to 250 cc. Determine Cl gravimetr1cally in 100 cc aliquot. Do blank by dropping Ma into water. DSW 462125 WATER PCB-SD0000046287 Specifications twd Tost Kathode , i , : ' 69 SmitomiX H woda oI301 Bo Specification B&ts Lot Upper Hold. IiO*or Hold Colour Bo. Pt. Co Pfco C. KPA Sep.l5A7 47 144.2 6o.o 3<8 46 144.2 6l.o 3-8 Sop. 22/47 50 142.0 60oO 36 51 142,5 60.0 3.5 52 142.0 56.0 3-5 53 142,0 59.5 35 Saa?>l G"4073 of Saatomx 1 vai wmt fro* Aaaltoa to fitnbea, 0t813A7 OSW 462126 WATER PCB-SD0000046288 Specifications and Test Methods (cont'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 belovr. . V Analysis of Santowsx 0 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 97-98 per cent ortho terphenyl with traces of diphenyl and meta terphenyl which form the oil. Tills product is distilled, mixed in the catch tank and i-un into drums to crystallise 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. . Kethod: 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 8lowly. When the temperature gets down to 550, 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) Same procedure as for Santovax R. DSW 4to2127 WATER PCB-SD0000046289 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. ffecessary 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 on this test of the product has been obtained. 4. Sediment Test: Fo insoluble impurities present in the molten sample. Method of Sampling: The material shall be fil tered through 100 mesh screen as it la 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-SD0000046290 * Specifications aad Test Methods (oontd) Finished Products, oontd Analysis of Santowax "M* This material Jjs a yellw solid of crystalline structure* The purity Is approximately 95 per cent iseta terpheayl with para terpheuyl making up the remainder,. The pre seat Method of separation y@Hds a meta-para euteetie at 3*3 per cent para which accounts for tnoafc of the para contaminants. ;' At preemit this product la crushed to Itm^s on inch or smaller, and hipped la paper bags or paper*-lined barrels. Laboratory Testa; ' . 1. Color: 1.5 - 3*5 HPA Method: The sas^le is melted with care not to die- color by heat ad poured Into 15-Bffl test tube, The color of the isoltea sas^>l@ la eoapar'ed to tbs standard HPA disc comparator, 2. First crystals: 90C. Methods A 230 cc beaker la filled about two-thirds full of the isoltea aas^pl and placed under a stirrer and a standard thermometer. The material is allowed to cool with stirring until the temperature reaches about 90C Seed crystals of the sasple are added slowly as the cooling continues , The ta^erntme at irfaieh new crystals com# oat of the solution is recorded as the "first crystals" point. 3. Hold Point: 83~85. .' * } ` Method: Stirring is continued in the above sanple while the teaperature goes down and then rises 1-3C to the hold point. The highest temperature at which the temperature resins constant for a while is re corded, '! ^2 . DSW 462129 WATER PCB-SD0000046291 - <\1 Specifications and Test Methods (cent'd) Finished. Products (cent 'd) Analysis of Santoyax "M"- 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 to melted for this tefet. The product' can be-filtered before It Is remolded after removing the water. Then it can be cmashed to 1/2." size for shipment. Under the present open- air method of handling this material, the dirt is especially hard to keep out. 46^ os^ WATER PCB-SD0000046292 Speciflcafclons and Test Methods (cont'd) Finished Products (confc'd) Analysis of Santowax P . DESCRIPTION; This material Is a white solid which crystallizes in think plates. The purity is 95-98 per cent with small amounts of meta terphenyl and trl-orthophenylene as the contaminants. LABORATORY TESTS; 1. Color: 2.0 ftPA Method: The sample is melted and poured into a 15-mm test tube. Of the standard disc comparator the color is Judged with KPA standards. 2. Crystallization Point; 209-213C Method: The cooling in this test is started in a mineral oil bsth 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 terp'nenyl. 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 aleo hard to keep clean under the present means of handling. . DSW 462131 WATER PCB-SD0000046293 Penfa'ol Teats 75 . Oom&rnim Stage t $6 Conversion ' Thar* Lb a connection from the pipe between the lead trap and to bottom of th eolmm on the convertor, leading to a imIIj water-cooled condensr# Saapleti of th vapour my be dr&tm off at assy time, ondensed, and & careful waswe- Msst of tbs density of tbs tmd@nsa.ta mA% as a masur of th # conversion. Th Amistoss operator makes this test tmm a day mi sels unit, usually la the morning shift. Each unit has a sampling eondaiuer, as shown on the attached sketch, perwwntly connected, and there is a steel sheet "fir sereen" to protest the operator and th equipment from the radiation from the conversion unit (especially th lead trap). Th operator starts the water flow through the condenser and opeafl the sailing valve enough to giro & distillation rate of about 500 sfL/hr as Judged by eye. Ho .purging with 00g is done. Som of th condensers hare a screw cap fitting with th cmdaasate and went tube passing through, others singly have a two-holed rubber bung. In either case, the sample bottle Bust mb a good vapour-tight connection. The use of spring Ups to hold the bottle against the stopper has been suggested. Th saaple bottles are of glass, square, 3^" x 3$n X 7" i the straight side, with screw necks, and the operator arries IS of the, one for each unit (elearly numbered) in a wooden rack, puts one on each unit, leaves the for about an hour, than turns off the vapour and water, remove the bottleo, puts cm their screw caps or blank corks, and carries fch@ twelve of tba* to his test bench where he bai a twelve-holed water bath, at about roo temperature, and leaves the until their temperature Is somewhere between 3t and 16C. A portii of each sanpi in turn is poured into a glass hydro Meter Jar and its temperature and density observed. The hydroiwter la graduated 0.880 to 0.950 Sp.Gr. in 0.0005 divi sion* awl should have been calibrated. The temperature should be determined with an accuracy of O.20, awl even at that th test is net highly acetarate, but it is good enough for routine otstrcl. . Th* $ conversion, corresponding to th density and teaperature, im read from th attached nomograph. The samples do not crystal lise, but oar suit, of corn's, be taken net to.allow serious 1 of benzene by evaporation during th aaapling and testing. The samples are quite hot when first collected, and there is a distinct mill of bsnreoe (and HgS) from the vent of the test while the'saaqil is being taken. There is, of course, a si stream of hydrogen escaping through th bottle. fNOUl WATER PCB-SD0000046294 r HA /'A ,o * 'O o^ * & <9` MY a> t '-Or6 v a< . "$ J> C" 11 1 w 0.890 BESXBSE COBfrasiCW CSAJKT From Final Report Ho. 1712, "Study of the Diphenyl Process, Part III' By t. T. Kilai October 19, 1942 0,900 -F !_ 0,910. I t- f- 0.92X1 Specific Grarity t 34 ~_2 32 '3 '0 30 1 ' .. z 8 8 - I-6 26 T r 4 24 4~z 22 2-JL o 20 4.8 X Jig I. IB 16 Temperature c. Homograph for Calculating ConferaIon of Boniene from Specific Qrarity In the example shorn by a broken line, specific grarity of 0.8977 at 30,0*0. shows 18,65 per cent conTersioa, h 1 20 19 18 ____ 17 16 DSiy 462134 Per Cant Conversion WATER_PCB-SD0000046296 Control Testa eentd 76 $ Conversion. oomtd This $ conversion test is not done until a unit has settled down to steady naming condition** If the ^ conversion of any unit la dlaiinetly different from 18$, the teapersture of the eonvertsieti pot will be altered* 2 to 3C at a time* to bring the conversion back to normal* Analysis of Prude Diphenyl Malt 100-150 g,, in a 250 diet, flask with 10B ooIimi, into weighed receiver to 275C < diphenyl e weight distillate x 100 weight saapl Distil Test for Benzene Leaks into the Stack Gases See page 91 below* Distillation Stage "Bold" point and crystallising points are used in the control f the distillation of diphenyl and of Santowax, though in both canes Aimiatoa rim the stills largely by "dead reckoning", plus column top teecwatureo in the case of diphenyl* because of the ti8> required to take the samples and sake the test* (See page <16 above)# The test bench in the department is, however* equipped with the mechanically stirred crystallising point apparatus described under "Specifications & Teat Methods" on page 58 above, - See sample G-%071 of crude Biphenyl, saapl 0-4074 of Still Bottona froa the diphenyl still* and maple 0-4075 of Still botto* fro* the Santowsx still, sent fix* Anniston, to Ruabon, Oct * 13A? Samples 0-4074 & o4075 were lost, and repeat sables were sent Jha*25A9 to London* Bamen# recycled from the distillation stag should not contain sore than, a. fm part* per cent of diphenyl, The operator can Judge by the colour of the benzene and by allowing a few drops to evaporate on his fingers, but a freezing point teat would give & bettr eritericie., ' WATER PCB-SD0000046297 JJST OF DRAWHiOS 77 Th&r<6 are over 350 drawings on file at Anniston* but copies only of thos thought to bo of interest to MCL bar boon sent to London at different times* da listed below. Those narked. mAn In ooltmn 3 vore sent by 14% Sage! of Amlaton* to Hr. V.H. Cooper In London*by airmail* Oot. 10/47* a second copy going by sea mH to Mr. H Buis In London, Oct. 13/47 IrawiSg' 2i______ -DasumULtlsa. Date seat Sent -hO--UtlLXilL. Conversion Ttolt AA-5581 Cast refractory tops for linings A 90-5584-3 Cast steel door on shell of fur^ naoe A 90-7817 Lead pet* flange* & thermowell July 21/50 OWN 90-7845-5 Stacks on vapourise or A 90-7847-8 Pot #1* details,with later revisions A 90-7937-4 Baffle for distributor A& July 2l/50 OWM AA-7955 9C-8131-4 Cast steel flange for dlstrib, pipe Details of column A A 90-8143-3 Traps for column 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 90-8166-4 Pot cover 90-8166-2 Pot cover*Baffle locations* units 11* 12, & 13 A A July 21/51 0WH WATER PCB-SD0000046298 List of drawings , cootd 78 tSwcIng' So. Description gonrerglon Quit, eoatd E>abe sent Sim? to MCL to Remarks 9C-819* Layout of piping, diphenyl trap* to BUBfp tanks 9C-8205 Layout j b^zene feed tanka & pusps 9C-8208-2 Layout 1 feed piping & nstars 90-9015 Layout units 11, 12, & 13 90-9019-1 Preheater pot 9C-9019-2 Distributor 90-9022 Convertor shell, units 11,12,& 13 90-902* Vhpourizer coil details ITot?13/50 see letter mi EM-DWT Hov.13/5o for aaendmanta Nov.13/5o ms do Nor. 13/50 ms do A. A July 21/54 owe A A 90-9025 90-9026 Vfepourlser shell Vapouriser assembly A Apr.l/*8 D3H Revised to Nov.lV*7 90-905* Oaa piping to burners, & bill of materials 90-9055 Vertical condenser & split flow box 9AA-9058 90-9069 90-9070 90-9075 Expansion flange in steam Jacket^ piping Aug.10/50 DWT layout of benzene nmbaek Vox.13/50 ms see comment ss-dwt NOV.I3A0 TTn piping to coolers j Nov. 13/5< ms Benzene line, coolers to feed tanks Nov. 13/54 mr CSW 462137 WATER PCB-SD0000046299 Llat of drawinga, eontd 79 ttwiag Wo* Deseription So.2 Mphonyl Still Late sent Sent to MOL to Remarks - 90-7870 Fr&etiomting coltmai A 90-7871 Layout Diphenyl still #1 A 90-7872 Condenser A 90-7873 SfciU A 90-7875 Diagraraatie flow sheet. Hew still. Included in "Design Data for Diphenyl Still0, Sept/38 Jime/46 90-7877 Eiboiler tank A 90-7886 SwiTel 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 catch tanks A 90-8210 Layout #2 still A 90-8211 #2 St in heater shell A 90-8212 #2 Still heater assembly A 90-8213 $2 Still catch tanka A 90-8214 #2 Still heads and tails tank A 90-8215 #2 Still? piping fro su^? tank to still A 90-8223 Rotaweir A 90-8224 Retains Ir details A 90-8254 Layout of piping, plan & elsratiorij Diphenyl still A . DSW 462138 WATER PCB-SD0000046300 .I List of drawings, eontd SemBjSg' Vo. Beaerlptioa ea Compression 9C-1360 Arrangements for burning Ho (obsolete), not sent to HDLj 90-7366 90-8o4o 90-6165 Bq coiipr; wiring & control Hg condenser piping wiring & piping diagram 80 5!T"Senf to MOL to R&mAa discussed in AME's letter JUne 30A8 May 24A8 dsh A Bee note on 90-7366t 90-8188 Layout & piping 90-8279 Layout piping from units HYB-14836 Griseom Russel Company Condenser (Pinned) , A& Wor. 13/50 tmii jjatr ioT' Not.13/50 EM t DOT for amend" merits * Bee AME's letter Jhne 30/48 for corrections to this drawing_ . also E.Gf.Thoenas, May 21/48, explaining that it relates to one ooapressor, vtiiXe 90-8165 refers to 2 and 90--9095 to 3 90-9095 Hot seat to MOL Santowsa DistiUatioa 9C-8551-1 High boiler distillation 9C-8551-2 EXeratlom June 1946 EAOT A 90-8552 Highboiler distillation 90-8552-2 Pictorial Elevation June 1946 MOM A General 90-7850? 90-7851] 90-8140 Diagrammatic Plow Sheets. Inclu June 13/K ded in '`Design Bata, 4" Diphenyl Unit, "Aug.9/39 #6 Unit. March 25/4l June 13/4 MOjl DSW 462139 WATER PCB-SD0000046301 Xlat of drawings, ontd 81 Swing .Ke* Baser ip t ion General, eontd 90-8190-1 General layout, units 7*8#9*10 90-8486 Plow Shoot - Convertors 90-8550-2 Plan 90-9060 Jnstrtmenta.tion diagram. Diphenyl (electricalX Shows Benzene Teed system Date sent Sent to MCL to 1---R---e--m---a--r-t--B ------- Kov. 13/50 See letter 1 to DWT Hot,: 1950 for BJSE senta A A A& Hot. 13/^0 rw DSW 40 WATER PCB-SD0000046302 qeheral iotbs oh bquxpmkht list 82 Reference should be mde to Anniston drawings and design data for details of the different pieces of equipasat The ' following list is Intended only to give a general description f toe equipnent, and a few eomenta picked up dicing various rla its to Anniston. The equipment list is mild only for units other than #4 and #5. Thm design was developed at Anniston and eomo modifications were introduced whan units #4 and #5 were planned. These changes ww found to be tssdesirable and the design of subsequent units, Including #11, 12 and 13, (the last lastalied)/eXlowed the ori ginal pattern. See page 32 above and page 85 below. All benzene lines ere steam traced and Hues carrying diphenyl or hi-bo11era are steam Jacketed, the Jackets being liberally provided with expansion Joints. (See Anniston drawing 9AA-9058). Xt is isportant 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 unit outdoors, with some shelter for the heating furnaces, vacuum pump and instrument panels. See the notes on "Gasketsw page 24 above. The eonvarsloo. and still buildings are high, with effective roof ventilators, and are open completely on the East 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 Amtston are very esphatle about the advantages of this. Flanges on the conversion system piping are of the standard amoaia pattern up to 3* pipe size, and are special cast steel tongue and grooved flanges of Monsanto design ^.bove 3*. Crane oXaiip gat valves up to 300C, no valves above 300C except cast steel gate valves on, the diphenyl still. Iteteri&Ls of construction for various Item are detailed in Anniston Research Department, Report Ho, 1642. S#e alto pages 22 & 41 above and 86 & 88 below for notes on the choice and performance of different stainless steel*. DSW 462141 WATER PCB-SD0000046303 B^mpaant List, ooatd 83 #1 Bmz&tm Storage Tanks Five horizontal steel tanka. See also pages ly & 29 above. #2 Pu^ for etyplylag #3 Controlled. by float In #3 which cuts off the pum> when the (5000 TOG) tank, item 3. contains about 4,500 gallons, and re-starts It at about 4000 gallons. #3 Recycle Peed rank See also page 29 above. Erawing 90-8205, but see amend ments in letter EM - DOT, Hoy.13/50. She tank In use In Hovember 1950 was a horizontal cylindrical steel ressel with bulged ends, about 7*-6" diameter by 13f-0R straight side. Capacity about 5000 TOG. Set In side a eoaerst retaining wall outdoors at boob distance from the flow control room. Pipes to and from the operating building run overhead under 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 split boxes, item #12, of the conversion units, and semicontinuously by pump from the benzene receivers, item #27, of the hydrogen co^ression room. Benzene in (after exami nation), batehwise by pua?> from the benzene receiver, item #21, of the diphenyl still. This batchwia return is dis liked, for Hewpert conditions because it would cause wide variations in the ratio of fresh to recovered benzene, and it has been proposed to interpose a buffer vessel so as to smooth out the flow. Benzene out, by a bottom outlet with an "up stand" in the tank to retain water and solid matter, to the feed ptsq?, item #4. The us of a bottom outlet helps to prevent air locking of the ptn^>s, The line to these pu^ss is Jacketed for steam,but it had no steaa connections in Hoveitoer 1950 It is contented through the retaining mil, Emin, from a simp 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 an see when the water las all run out, and the benzene is coming. There is no special provia ion for sampling, though, a sample might be drawn through the drain valve, or taken . . pam ^olg of the branches m the line from the feed pimp^ DSW 462142 WATER PCB-SD0000046304 \ Bqtdpattnt hist, contd 84 #3 Recycle Peed Tank, contd Vented to the hydrogen system by Beans of a Insulated line, (tbe tack oontents are usually war* at Anniston, ly fro* the atrea* of recycled benzene*) There 1b a rbranch on the top of the tank, with a gate valve through which the tank Might be gauged* This 1b very rarely doo** Float controller stopping the pia^>, Item #2, when the tank contains 4500 tSO, and restarting it when the level .ban fallen to 4000 030* Floats for high and low level alar** (There 1b no formal drawing of this arrangement)* These various floats are now mde of glass, stainless floats taring failed, and stainless guide rods are reeofflsoaded because sticking of the float my cause tad trouble. The domes ever the float controllers are Insulated and a tea* traced, but the tank itself is not insulated. It la, of course, electrically earthed (pgrounded*), Anniston experience is tmfa.voura.ble to the use of internal sties eeUfl la benzene tanks because of tbe risk of water getting Into the benzene if the coil', falls, and of ben zene loss via tbe coll* Even If the coll is taken out over the top of the vessel, loos is possible by siphoning. #4 Feed Pimps to the Conversion Units Anniston report 1642 of Oot *15/41 describes the feed pump a as Weseo Mo.507 (on then for each unit) with band-operated by-pass to set the delivery rate. Stainless shafts with ill Resist* iapeXXorfl and liners, 1800 RPM. In November 1950, one Gould centrifugal pw^p with an in stalled spare (and room for one more; ms serving the whole 12 units through a row of flow controllers, me for each unit. It was of the 2-stage centrifugal type, 3400 HPM, (but this high speed is disliked by the operators). Gland packing of fiber-reinforced, rubber rings, with the gland nut sliply tightened carefully with the tend. * Delivery about 170 OSQ/hr/Wit at 100 ptig. A steady feed rate is important because fluetuaticca in the rate cause variations in the pot tenperatures (Tb flow of fuel gas to the preheater pots la set by band, and con sequently is not airtonatically readjusted to neet such variations. The convertor pot temperature is automatically controlled, via the fuel gas supply rate, but naturally the control lags, became of the sensible heat of the lead, the pot, and its setting). * These ring* are aide for the stem of water valves, but t*heVy_ h. a.v--e----b1e--e--n----'-f-o--u--n.d.. to serve_1 b_e%t*t.er t-tan. othJe. rHpWaAcllklninXgCs WATER PCB-SD0000046305 DSW 462143 Bqxtlpmant List, eoetd 85 #4 Feed Puqpa to the Conversion Units, coatd There Is a Fisher strainer on the line from the feed tank. Item and the pimps deliver to twin filter Teasels In the flow control room. See under "Process In hatall" above, page 30. #5 Costera Ion Units Ifrewlngo. See list under "Diphenyl Process Drawing List" subtitle" "Conversion Unit", page 77, especially 1 90-9019-1 9C-9022 AA-7955 In Hoveiriber 1950, Anniston had IS units, of which two were of the two-pot type with special tubular heat exchangers, to transfer heat from the converted vapours to tit in coming benzene tap ur, and the reminder were of the 3-pot type. There were numerous minor differences froa 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 cm the 3"pot system. A 3-pot unit consists of three essentially similar stain less steel vessels, about 6,-On deep by 1'-10-3AH I*D drawings listed above), each set in its own gas-fired ce, Tha 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 f it and the convertor on the other side of it. The furnaces are of firebrick, with steel easing. Each setting has eight gas burners, horizontally directed tangentially into it, four at one 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 from pots 2 & 3 go downwards to cross flues leading to the bottom of the setting of pot #1, then tip inside that casing, and out to a flue leading to the bottom of the setting of the vapourl- z&Tj item $6a There is a steel door, with stabbing hole, at the bottom of each setting, for naming out lead in case of leakage froa a pot, and there are access doors in the flues where needed. ' DSW 462144 WATER PCB-SD0000046306 Bggjpnent hist, ant4 86 #5 Conversion Chits, conM By Beans of daapars, th flm g&sea say be by-parsed away from the vapourlxer by passing them Into a rent stack. The t@sparatw of tha tore pots are discussed tmder ^Process In Detail* on page 33 and 51 above, aad it will be sen that th #1 pot is at a sraeh lower teai>@ra.iur@ than the other two. Actually the waste heat fro* pots 2 aad 3 is almost enough for #1, but the burners in the #1 setting bar a little work to do, and of course* would b needed if the pot had to be re-started fro* cold. Benzene from the recycle feed tank, item #3, is forced by the pu^>a, item #4* against the back presstir# of the whole conversion system, to the top of toe vapourixer, item ,, It 1s vapourised in passing down the coils, and toe vapour bubbles through the lead In the three pots in series, than passes, via the lead trap, item #7, to tha bottom of the fractionating column, item #8. Each lead pot has a dip pipe reaching nearly to the bottom of th pot, and to wpper part of the pot has circular baffles to diminish tha entrainment of the lead. A great deal of aperimentatiaa has been devoted to such problems as th design of the dip pijs and of distributors, (see below), for use at its lower end, the design of toe baffles, toe choice f stainless steels for the differ ent parts of the equipment, and the choice of gaskets for the pot covers. Soeathing of this can b# seen from the "Hots on the Maintenance of toe Lead Pots", mi pages hi- above. Ho attempt is sada here to review the whole history, but only to describe the arrangement now used, with present-day ideas for improvement. Tteioua old patterns of pots etc are still giving good service at Amis ton. The pots, and the fitting inside them, exposed to the hot lead,but not the covers), are of stainless steel. See pages 88 & 8y below for tha choice of the type of stainless steel, also page 22 above. Anniston us steel covers for tha pots. Th #1 pots have flat covers, of steel plate welded on to the ria of th stainless pot. Some of these plate covers lav heavy radial fin* welded on for stiffness. Th #2 pots lave heavy east steel domed covers, bolted on, with heavy cast steel (divided) backing flanges under to pot rims. Th Making flange has four lugs, fitting into sockets on the furnace roof and supporting the pot so that th rim is several inches above th top plats of th furnace casing. DSW 462145 WATER PCB-SD0000046307 Equipment List, contd 8T #5 Conversion Dtaita, eonfed The gasket la this ease 1* 5/l6" roimd soft annealed copper, with a square section asbestos gasket inside It. The 3rd pot Is similar in construction, but has a gasket of 1" braided asbestos rope. Mr. Barden took a sample of this in August 19550 This thicker gasket is used be cause ih edges of the flanges pull together in Berries at the high temperature, and they can. remain in serried longer with a thick gasket. To nako the gasket,a pieoe of the asbestos rope is etrt, long enough to He Just inside the bolt circle, plus a fewJhobes over-lap. The ends are overlapped, end the groove between the overlapped parts Is stuffed with strands of asbestos rope, and the overlap botmd with a few thin wires. Liquid glu Is used to help in making the overlap and in holding the ring In place between the flanges during assembly. In usq, the Joint ring becomes completely flattened and hard. Tire use of restriction orifices after #3 pot, as discussed on page 3^ above, has thrown much greater pressure cm the Joint of the pot and the asbestos rope gaskets are giving much sore trouble. Vertical sheet iron fences, about 6" deep, in two halves bolted together, are being loosely fitted around the cover Joints of some of the conversion pots to deflect any possible burst of flame due to a fail ure of a gasket. ' London's proposal to use thicker covers and backing flanges, and to mk them of stainless steel having a higher tem perature yield point than the plain steel one, is liked at Anniston, because it offers a chance of using copper gaskets on the conversion pots as well as on the preheater London's proposal to use slotted bolt holes la disliked as tending to favour the bending of the flanges. London also suggested supporting the pot rim on a continu ous ring instead of on the four lugs, but this arrangement would appear to sake the over bolts more difficult of access, to rob them of the cooling effect which exists tasder the Anniston arrangement, and to sake the raising of the pot a little or@ difficult. At Anniston the eostpartion flange under the pot Pin is in two halves, bolted together, as mentioned above, fonting a circle, with four lugs 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 pair forming guides for the lugs on the companion flange. Steel packing pieces are placed first on the bottom of these guides to give the necessary elevation of tbs pot. then WATER PCB-SD0000046308 Equipment List, oontd 88 #5 Ooutvertilon TBalta # oontd tbs pot lred in and a cowed by steel wedges driven in . alongside tbs lugs. The pota should not be rigidly con nected to the tvrm.ee easing because the continuous vibra tion of tb@ pot* would be eofiemaiioated to the brickwork of th fwrasee, and tend to mto it crumblee It Amdstoa they fit fairly closely into the round, boles in the furaao roofs, but in sons cases steel sheet sectors are used to bridge the gap. in any ease, the Joint is mde good, either with clay, or more recently with a paste contain ing asbestos fiber (insulating cos^ound 60). This help to keep the pot ries a little cooler. The bolts in the pot cover Joint and in the adjoining pipe flanges, are of ordinary steel*at Anniston, and are never re-used, partly to save tine and because they become . stretched, but to inly because working conditions can be very uncoifort&bl because of the radiation of heat fro*, other unit*. Hewport, using stainless bolts, and having only on unit should be able to re-use the bolts. It is suggested to us nuts of dissimilar metal, to diminish galling. la cutting out the bolts cm the pot over, the Anniston welder uses an oxy-acetylene torch, and cuts through the base of the mi 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 n&w 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. Small square of steel (old nuts will serve), are welded under the eo^jaaion flange, between the bolt hole#* to pre vent rotation of the bolt. The nuts are run on with aa air-driven spanner, for speed, and tightened up after the pots are hot, with a 4' long ratchet spanner. Anniston advise strongly against attesting to us a tongue and groove Joint on the pot covers because of the risk of dis tortion. The attachment of the stainless pot ri* (by welding) to the pot itself appears to be & line of weakness because the lead in the pot is very heavy and is gently buoying and vibrating whenever the vapour is passing. Cracks at this point are not unknown. Anniston have increased the thickness of the rim of the pot) formerly 5/5 now 1D British nalcera of stainless steel agree that 309 stainless steel tends to be brittle at the pot ten^peratixp, but that 330 does not. M3L are experimenting with pots fabricated, by welding, fro eentrifugally cast section* of 330 stain less, welded either with 309 or with special electrodes. ' DSW 462147 WATER PCB-SD0000046309 Equipment Lint, ootid 89 #5 Conversion tfalts# contd (Sm the letter from Michigan Steal Casting Co, to Annis ton# Hay 3X/50) & Annlaton discussed this design# Aug, ifhS. Heat treatment# after fabrication# 1m reeosneuded for both 309 and. 330 stainless. Inconel# Emeka# nickel# aad allays rich in nickel are said to give poor 0ernes. Amis ton reported# Aug,! & 5/%9* that east thermo wells of 309 had proved to be brittle. Centrifuge,lly cast dip pipes of 309 were better than rolled# or Bold east# but were brittle or became brittle in service. Centrlfugally oast dip pipes^h&r recently (1950) given excellent ser- ^of 310 vlee. It is noted that in. this method of easting the dross stain- tends to form cm the inside of the pipe# but no term less appears to have resulted.. Thermo wells of east 330 have steel} recently given very good serriee. Carbon tends to bmlld tp 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 wars against welding cover strips on the outside of welds on th pots. Outlet branches on the overs should not extend down into the pot, and the joint should b welded inside# to fill up any crevices. Sharp edges of metal also tend to attract deposits of carbon. Any distributor at the bottom of the dip pip mist be such a will not increase liningeamrfc of the gas on th pot wall# because of erosion. Amis too are using a sin?l open-ended pipe with a renewable liner for the last few inches at tne bottom and four 5/8* holes drilled radially through th waH about 4" from the bottom. At a meeting at Amis ton# 1fap,l/t9# & proposal was made to try a deflector which would discharge the vapours tan gentially in a horizontal direction. This it was thought would give th lead a swirling motion, diminish vibration of the pots# increase the contact tin of th vapours# diminish the s of the gas bubbles# and diminish th ntminaent of lead. Barrow orifices must be avoided in th design of any deflector because of the building up of carbon, . This deflector had not been tried at Anniston# but London asked that the pots to be supplied for Bewport should lav a deflector. Standard dip pipes were# however# shipped in Hoveib@r/50 to avoid delay. DSW 462148 WATER PCB-SD0000046310 Bqtrfpaaat List, oontd 90 #5 Conversion Tfelts, oontd tew City, Aug.lO/3^, seat MOL a drawing of the distributor they had developed for pots for propane cracking, Thera is m heat insulation used anywhere in the coww ion system, except that the Tapour pipe from second preheater to the converter is insulated es so@> of the units, It is desirable to avoid loss of host anywhere along the line of flow, up to the top of the convertor pot, and at one tlse the pot lids were insulated. It was found, however, that greater distortion of the pot covers and bolt* resulted. The insulation of the vapour pipe from the second preheater to the conversion pot is not an easy task. In. mom cases, asbestos fiber, inside a sectional (lobster back) easing is used, and. In other cases a special Johns MonsriUe powdered product in a dust-proof steel casing. This insulation and easing adds to the weight of the pipe, and ay oause sagging, and all those long pipes, from 2nd to 3rd pot, whether insulated or not, hare support stirrt^s, which, however, appear to be out of use. In addition to the vapour inlet and outlet and the thorn well, each pot eover 1ms a fourth opening. On the ccavertor pots this is blanked, but on the 1st and 2nd preheaters this opening is used to connect the balancing line. These ewaeetioas ran in 1* pipe vertically for about 7'-0"*and than Join into a horizontal header running to the bottom of the eolwm, it* #8 There is a pipe coupling cm fchla line about 2 S-0R above the pot eover, thro a branch for a presutsre gauge, than a atop 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 from being forced backwards tot the vapourixer, There is a pressure gauge on a broach 3a the vapour line from the convertor pot to the olwm, &Xbo a branch for the s&apling condenser des cribed tmder "Control Tests on p&ge 75 above. There la a heavy l-beaa about 18 deep, with 6" flanges, and with a chain block . . permanently installed, running along It , one for each row of 3 pots, with a hinged section of the floor to permit lowering a pot or a lead trap to the grosmd floor. Wmn a pot is put ebfc of action opportmity is taken, to clear debrl* fro* the bottom of the furnace. DSW 462149 WATER PCB-SD0000046311 txu a j-K&gss* y\jj TO SHOW OTLLIZXKG- LINE OH LEAD POTS 1 C F 3 4 w DSW 462150 WATER_PCB-SD0000046312 Equipment.List, caitd ' #6A Yhpourlsera mwLmn. 90-7^5-5 9C-8159-1 9C-9024 90"9025 . One per conversion unit. Each consists of a a Ingle oil er of two 0011a In parallel, in a brisk lined steel teak through which the flue gases pass* Betmospasses downwards through the oils countercurrent to the flue gases* The Tap ourIsera first Installed at Anniston tod tiro oils in parallel, one inside the other with s eoaston inlet header, and a control mlw on each exit, leading to a Y pip into the first preheater. This arrangement was found inoosrenient, and has (except in the case of one unit') been abandoned in fa-roar of a single oil. There was some doubt about the proper storing of the flow between the two colls, and considerable trouble with car bon blockage. Anniston report 1642, Oot,15Al* states that corrosion of the vapotartzer oils my occur by con densation of moisture from the flue gas, near the point of entry of the cool benzene. A small leakage from a -rapourizer oil into the flue any easily pass unnoticed, because the benzene will probably not ignite in the stream of flue gas, and the leakmy cause serious losses before it is diseorered. As & safeguard against hoary losses a sanple of the flue gas is aspirated orrery day from a point in the flue, iM&Sdi- ately above the yapourlxgp coil cm each emit, and is passed through a mixture,^equal parts of sulphuric and nitric acid. For this purpose a steel pip is per manently installed la the rapourizer flue and all these pipes ar carried down to a test bench on the grotmd floor. The sulphuric-nitric mixture is put into small rubber stoppered bubbling bottles, which, for safety, are sheathed la simple steaM-pipe sockets. The bench has a *isf>le water aspirator, and it Is the night opera tor f duty to test all unite. He eiaply aspirates the gas through the acid for about 10 minutes, then sjbsLXs the aeid bottle. Blockage of tbs yapoinIxer coll la rare (except by lead forced back from the first preheater). Traces of lisp-urities left by evaporation of the benzene are sinfily carried forward in the yapour stream. The flue gas must, of course, be by-passed round the mpourizer when the benzene flow is stopped. A coll should give over a year's service before needing repair. 91 DSW 462151 WATER PCB-SD0000046313 Equipment Llit, ocmtd By-Paaa Flue Drawing. 90-7845-5. . 0m jw nfersloa unit* fitted with a daaper, To allow \ flu ga@m to by-paas the vaporiser as necessary. 92 #7 ImA Trap Drawing 9C-8143-3. Oft par conversion unit. This Is a centrifugal type separator tar removing any entrained lead. It Is a closed* welded vessel which must be taken out at Inter vals to allow any lead to he malted out, to some of the Anniston wilts* the lead trap Is & rela' tlvely small steel vessel* so placed that lead an drain back from It to the convertor. In the newer units* the trap is larger and stands on a steel plate oa 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 3 * -6R high* 2f-0* diameter* with a central pip 6m 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 14* down inside the trap* otherwise its bottom end becomes ehoked too soon by lead and by solid debris (iron oxide* earboa* and shots of entrapped lead)* In a trap* seen ifov*A>0* the layer of entrained lead was l4B deep* and there was considerable solid debris as well* After the lead had bom melted out this vessel mg out open to permit the shortening of the law tube* and opportunity has taken to dig out the solid debris. lot oa &ptying the Lead Trap The unit Is shut down and allowed to cool a little* and Beams diphenyl te. my run back into the lead trap and my take fire when the trap ii opened, . Each cyclone has a lifting hook welded on* opposite the ga inlet| this is for the yard crane; inside the shed the pot is lifted by a stirrup bolted to the central outlet flange. T3 cyclone is lowered to the ground floor* picked up by the yard crane* and taken to a Bait ing table In the scrap yard* and put on the table with the vapour inlet downwards* (vessel an its side)* and flam* of national gas played cm the pot until the lead DSW 462152 WATER PCB-SD0000046314 (To follow page 92) TABLEj. ETC. mm for czmmm THE LEAD TRAPS ScoU V- r-o* 2't.Cfec.. a.' S(de viffw Picon Equipment Llat, eoatd 93 #7 Lwl Trap, eontd ms out cm to the table and down Into a lead melting pot, from which it can be m off at convenience into nolda lit those used to enpty the pots . The Belting pot tee a bride setting, and a proper gas burner, but the cyclone is heated ilnply by open flames, confined aae- wtat by moans of sheets of corrugated iron. The natural gas tea a high calorific value, so tie melting is quick. ' The boIda are the same aa those used for @sptying the lead pots, see page 39 above. goto on Repairing Lead Trap fc Colum These units are exposed to the blast of hot vapours opposite the gas inlets (especially the lead trap since the introduction of crifies plates in the vapour pipes fro* the convertor), and they wear thin. The tmit being shut down, and purged with COg, external patches can be welded on. A useful trick first is to weld a pipe nipple on the center of the patch and to leave it open as a rent until the 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 tee to stand tp to fairly heavy handling when being cleaned, apart from the high tenperature during ser vice, and it should be of heavy plating. Stainless is not necessary, and thin stainless would be unsuitable. #8 Fractionating OolinaMi on Conversion ttedta Ikwirsg 9G-8131-4. On to each conversion tmit, Vhpour in at the bottom from lead trp #7* Benzene reflta in at the top from reflux box #12. Vapour out at the top to condenser #31. Ttoderfloir out at bottom via carbon trap #9 to sump tanks #10. Thermo meter well at point of entry of reflux line to eoltnm, and one in the exit from the carbon trap. , The eolusm ha 12 plates, but the caps have been removed from the lowest 2 plates because they became choked with entrained lead, etc. The lead would be above its melting point aa it entered the coluam. The need for so may plates, for a cooperatively rough separation of benzene from diphenyl, Mm been questioned, but plant experience indicate* iom difficulty in maintaining a reasonably DSW 462154 WATER PCB-SD0000046316 Equipment List, eootd 9* #8 Fractionst-fag Columns ea Gowerslon Halts, contd low content of diphenyl in th# distillate and of bmizem in tha under flow of the olum, Preaisiably the plate efficiency a low because of the dilutica by hydrogen and possibly there ii fouling of the plate by carbon carried forward in the tupor stream. The plates hay the usual drain holes to prevent block age % freezing. Design data were unavailable, Hay iK/HQ* The crude diphenyl tanks are heat insulated, and any team Jacketed lines outdoors The eoltnm hare no heat Insulation* Packed eoltnms were used on the earlier units, but they became pitigged with solid matter carried forward from \ the pot*. #9 Carbon Trap Craving 90"8l433. Underflow is from column. Side outlet at top to susg) tank #10, with thermo well in the pipe bend. The outlet pipe goes down nearly to the ground level before rising again to the susp tanks, so forming a seal bend between the trap and the Br^> tank. This seal bend and all the piping ar steam Jacketed# inner tube 2 diameter. These traps arc removed from the unit for cleaning when ever necessary, about every third month. An opportunity ay oootr when tb tmit 1m shut down for bom other purpose. The teiq>eratuor of tha column trap is below the melting point of lead no that the lead that settles her is usually in finely divided solid particles. However, due to the nature of the infniibl, highly arbooaceotis organic materials that settle also, the lead is intermingled and agglomerated^- late a solid mas. Thus it is necessary to burn and malt out the trap to recover the lead. The proportion of carbon to lead is greater in the "carbon" trap titan in the "lead* trap. Anniston report 16H2 of Q0t,15Al states that this carbon trap needs leaning every 3-5 months, and that, although It Mm a. bottom outlet plug, it has to be taken out and 'cleaned by burning. As seen at Anniston in Hoveaber 1930, these pots were aim la vertical steel cylinders about 3**0" deep by about 19-6" dlemotm? with about a 9" flanged neck DSW 462155 WATER PCB-SD0000046317 Sculpmeat Mat, oocttd #9 Carboo Trap, oootd to connect to tho bottom of th eolin*a Th6 over also had an inspection plug and tm Itlug eyea to facilitate handling for imintenaneo . 95 #10 Suag> Tanka for grade Biphenyl -' Horizontal* steal* Insulated tanks. Underflow In* toy gravity* from edttun #8 via cartoon trap #9, Out toy sub merged ptasp #XQA to Blpbenyl Still #13 111 liquor lines thoroughly steam Jacketed. Teat to off-gas system. St&@M oil eoaneetions. Vare liquid depth Indicator, Vent with explosion dine. Mr. KLlenburg* May 14A8* stated that these tanks are operated at about 125C to prevent crystallization. Whoa seen in Koveabar 1950 the vent pipes were quite hot to the touch. - #!0A Subasygod Ptap For transferring crude diphenyl froa ausp tank to diphenyl stills. On to each susp tank. Explosion proof motor. #11 Condensers on Conversion Staffs Erawing 90-9055. On to each oaversion mlt. Tube and shell type* water through tb tubes. Wpour in from eolwm #8 and conden sate out to Reflux Split Box #12* through a strainer with toy-pas*. Balancing line froa top of Reflux Box #12 to condenser* with connection to hydrogen off-gas system. There 1* also an emergency vent to the atmosphere. toolston advise against the use of copper tubes* because of the sulphur S^uritles In the benzene. They advise mking this oodeuaer of a^pl capacity. #12 fleflur Split Bor. Efrawlng 9C-9^55. DSVV 462156 Standard Botawetr* with sight glasses and levelling screws. One to each conversion unit. Forward flow returns via tight glass to recycle feed tank #3. Bight glass in reflux Um. Both lines have deep seal bends* Apd there mist be sufficient head between the reflux box and the return inlet WATER PCB-SD0000046318 Equipment Met, eoatd #13 Diphenyl Still DrawHig 90-825#. fm sm Installed. Horizontal, insulatod, aiee>X- tank. Subnerged puap with water cooled bearings, and outlet to external gas-heated oil with branch to erode Sanbo rns receiver #20. Inlet fro #10 sun> tank and "Heads and Jans* receiver #18. On one dished end is return line fros bottom of cole* #1#. Return line fro* heating oil. Vapour otttlet to bottom of colton #14, 4" vent pipe, from a branch on the vapour pipe to the ooltwa, carried up through the roof. This vent pipe has a bursting disc between two flanges located about 6*-0* above the vapour pipe. In one case, the 6f length f pipe is Jacketed (Jacket espty), and in the other ease it is bare. Dsaediately below the flange there is a thermo well, with a therm miple giving a continuous record on the Multipoint tefiperatur recorder in the instrument room. It is found that the discs slowly become perforated, probably by sulphur ooapetusds, but even a small perforation is detected by the tesperattsre rise. The pipe above the flange is supported on rods with a turn-buckle fitting by which the pipe can be lifted for easier replacement of the disc. The bursting discs are B.S.&B. dike, type Al-Pb (lead on the oaoave surface) "Vinyl service . Bursting pressure 39 (in another case, #3) p.s.i.g., carried be tween two B.S.&B. type flanges. 95 #X3B Heating Poll Brewings 90-8211, 9C-8212. On for each still. Supported in a steel casing with firebrick lining. Gas fired. Liquid circulated by pu^> #33A from and to still #13, Plow is countercurrent to flu gases. Half the casing hinges away on a steel track for access to the coll,. Th@ circulating lines are steasa Jacketed, Note, 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-SD0000046319 jj..K.(jl----Jijt"I-nfc{KcTiO- n ofwrung Front View or T& l-tcervets DSW-46215S SWIVEL BOX WATER PCB-SD0000046320 Equipment List, eoptd flH ColtBBQ Drawing 90-7070. . On for each tin, 20 plat eolum, Drain holes la plates. Tfcpour inlet at bottom from still #13, Ht- flm return frost split box #16, todwflw ft*oa bottom bask to still #13, TSpoup out to condenser #15 via goose nwk. Anniston formerly used a padeed eolum* with a direct fired still* bat the results were not so good ai with the present babble e&p oltnm, On May 12/49 Anniston expressed the opinion that the 20"plat eolum* proposed by London Central Engineering Dept, would b adequate. Special car is needed if the reflux line to the still is not to frees. 97 #15 Condenser Drawing 90-9072, One per still. Horizontal tube and shell. Wpour in from top of oolema #L4. Condensate out to split box #16, Cooled by water through tubes, circulated in a closed system by pusp #23 through heat exchanger ^2 with sake-up tank #24. #16 Reflux Split Box Drawing* 90-0223 and 90-0224, Standard Eotaweir, with sight glasses, and levelling screws. One for eadh atHI. Condensate in from condenser #15, Reflux out to top f oolum via sight glaas. Forward now to beorene receiver #21 or through box #17 to re ceivers #18 and #19, Tent pipe* ateam jacketed for occasional melting out* (should have flaa arrester). The reflux box should have steam tracing for use while th# diphenyl fraction is naming. #17 Swivel Boxes for Switching Diphenyl Still Distillates Brewing 90-7006 On* for each atHI, Condensate in from Reflux Split Box #16* and. tit* by mtssl adjustment* to either ''Heads and Tails p receiver #1S* or Diphenyl receiver #19. DSW 462159 WATER PCB-SD0000046321 (To follow page 97} Equipment List, oont'd #18 "Head and Tails" Receiver. Brewing 90-8124. . On for each still. Vertical tank with submerged pto^i.and aanhole. *H&daE' or fraction of distillate In fraaSwivel Split Flow Box #17 Steam coll inlet and outlet. Submerged puqp delivery line h&ek to still. Vent line with lower portion steam Jacketed and carrying burst&g disc.. Inspection hole with loos hinged oorer. Bottom outlet." #l8A Submerged Fuap One per Heads and Tan* receiver. For transferring Heads and Tails fraction to Stills #13. #19 Diphenyl Receiver Vertical tank fitted with eubaerged pump #19A. Diphenyl fraction in from Swivel Split Flow Box #17. Finished product out via puxg> delivery line to Aroelor Plant, Store tank or Flaker. Vent with lower portion steam Jacketed and with burst^K dio. Bar hole and cover. Handhole with loose hinged cover. 3team ooil Inlet and outlet. #19A Submerged Ptng> On for each Diphenyl reoeiver #19. For tranaf err ing diphenyl to Aroclor Plant, Store Tank or to Flakor, Explosion proof aotor. #20 Crude Santowax Receiver Drawing 90-7877- Vertical tank with submerged pvmp #20A. Inlet from submerged pimp #XJA of still. Crude Santowmx from outlet of subtaergod puz^p #20 to #34B of S&ntowax Dis tillation Unit. Handhole and loose hinged cover. Banhole and cov*r. Steam coil inlet end outlet. ' Steaa Jacketed vent and burs&og disc. Crude 3antowax to drums through bottom outlet. Second atpam Jacketed vent with hand valve. 98 DSW 462161 WATER PCB-SD0000046323 Equipment List,, eontd #2<M Submerged Pta^ 0m tar m^sh crude Santqw&x receiver, Pop traasferring erode Santwax to #3to Santowax still charging tank. 99 #21 Buffer Storage gaak for recovered benzene. Vertical tank with mnhol and went* Recovered benson la from refltne split box #le> and oat to ptap #21A. Inlet and outlet for ateaa coll. Gauge glass #21A Tm Receiving recovered benzene from buffer storage tank, #21, and delivering to recycle feed tank #3. Ezplosicoproof motor #22 Seat Exchanger . toe for each stIIL Receives hot clreulatlng water fro condenser #15 and dellrers cooled water to pump #23. Cooling tw through tubes. Tim circulating water is Maintained at 304oC during the benzene forertm, and about &0C during the diphenyl fraction, (by band control cm the fresh cooling water tirough the tubes in each ease). Cocpfire page Hja #23 ' . dm for each still. Recalves circulating water froa heat exchanger #22 and delivers to condensers #15. Explosionproof motor. #2^ Make-w Water Tank Om for each still. Receives nak-w> pond water as necessary to replenish, water lost by evaporation on cir culating through condenser #15, Bottom outlet to circu- lating line. Overflow. Constant level device for con trolling receipt of water. Condensed water would, of be better for this sake-up. DSW 462162 WATER PCB-SD0000046324 Egulpoeat List, eontd 100 #S5 Pooler fop gydrogeo. . Drawings 9Q-QoHhs Qrlacoa Russel Co, MYB-1%836# Each of the tom3 parallel, units of the original cooler has been siofrotmded by a mtor jacket to increase the cooling surface. Receives hydrogen, for eooling, from a mla a erring all the eoarertor units# There 1m a rent with hand controlled valve connected to the hydrogen inlet vUt. a benzene trap# The latter is a small pot containing baffles and drain ing to the surge tank #26. #26 Surge Tank for Hydrogen . Irauing 90-8188 .. Receives cooled hydrogen and condensed benzene fro color #25 and benzene from the rent to the hydrogen cooler. I&rdrogea delivered to inlet of eonpreasor #29. Condensed benzene flows by gravity through bottom outlet to either of the two tanks #27 Fitted with 55" water seal'to provide pressure release if necessary. Water seal has a vent with flame arrestor. Line to instrument controlling pressure within Halts of 11-16 os.' Pres sucre gauge. Balancing line to benzene receivers #27. Whan tbs pressure drops to 11 oz,,, the ecB^raasor low stage beoones inoperative and only the high stage operates. When the pressure reaches 16 os both stages operate until the pressing falls again to 11 ez (per sq.in.) # through the roof, #27 Benzene Receivers Drawing 9P-8X88. One for each commas or* Receives condensed benzene from aiffg tank #26, fron low pressure tank #31, and high pressure tank #33 through sight glasses# Benzene out via bottom outlet to punp #28# Balancing line to surge tank #26. Level gauges #28 Fo^> toe for each compress or Receiving condensed benzene fro benzene receiver #27 awl delivering to recycle feed tank #3# DSW 462163 WATER PCB-SD0000046325 Bqttfpaent List, ccotd . 101 #29 Two Stag# Hydrogen Oo^regaort Brewing* 90-8X88, 90-7366j wiring and controls, revised Torsion ant to Mr, Buis, jan.18/50. Two are Installed, Tbs first stage eoapressee the hydro gen to 6<3#, and th second to 3OO2F pressure. Provision for inta^duclag OQg for purging purposes, The ooapreisor tbas elves r@ tr cooled and there in a snail verti cal tubular condenser after each stage, draining to the corresponding pressure tasks, items #31 k #33, IT, Hardy stated, Iofbr 17Athat the controlsaor hare 1 316 stainless shafts and vilv discs, MI-resist cylinder liner* and mire cages, Ooetx gaskets, stalnles* steel or aluatintm type, and that copper and its alleys are tmdeslmbl, Ho copper or tress gaskets should be used, and generally copper and its alleys are avoided, Ifc*. Clegora. Hor/3Q, mentioned gasket* of Babbitt smtal for the compressor* Anniston were asked If tm-lubrieated cylinders with earboa rings would not be better, but they replied that finely divided oarboa, which inight cose over in the hydro gen strsa, would abrade the carbon rings. Drawing 90-7366 showing th wiring and control eratea for a single centres- or, was sent t London, May 24/48. Th* ot^ressor* are fed rather liberally with lubricating ii to cope with the possible condensation of bernene in th* cylinders, but Anniston have not noticed any trouble fro* lubricating, oil getting into the process stream, Mr, A, M, EHeaburg, Jtm 30A8, gave a general discus sion of the operation sad control of the cobras*ora, incidentally giving 150 and 300 p,i,i,g, as the two pressures, but stated that these vuluss were not critical and that the choice ttimed cm considerations of cylinder size and quantity of gas to be bandied. Progressive unloading would be satisfactory as an alterna tive to the "trigger, on & off" unloading control used at Anniston. By !or,/50 the solenoid unloading controls had been replaced by pneumatically operated control*, partly for reason* of safety. Electrical switches would jn any ease be outside the 0Depress or room. The room is iUtdmted by flood leaps placed a few yards outside the windows. nc\A/ 462164 WATER PCB-SD0000046326 Equipment List, eootd #30 Integra taga Pooler One for each Siiply oonsliti of * vertical, water-Jacketed pipe between outlet from first stag of TOaprentor and inlet to low prosaw tank #31, Q& . and rapor in at the top fro* the oonpressor, Condensate nod g&ii out at th bottom to the low pressure tank. Item #31. 102 #32. Low Pressure Tank Ekwing 9G-8lB8,, (to for each compressor, Receives hydrogen at 60#, via Interstage cooler #30 fro* first stag of coapreaar, and delivers to second stage of compressor* Condensed hoaxes Mown to benzene receiver #27, Bottom drain cook* Pressure gauge, Th task has a pep valve to opes at 100 p.s,i,g and a bursting disl(B,S,&B, aluminium* with lead facing e**to pressure side)-*--to-opea at 150 p.s.i.g, Both these have hooded vents well above the roof of the coe?pressor room. The vents should be well away from the roof louvres of tbs conversion rooms, and th still Cnrm.ce room, A connection, originally installed be tween item #31 and the gas inlet to the eospressor, was removed. #32 Cooler Similar to #30>aod cools the gas passing from outlet of second stage of the coapressor to the high pressure tank #33 #33 High Pressure Tank Brewing 9C-6l^, On for each stressor, Receives hydrogen at 300# via cooler #33 from second stage of compressor and delivers to HB-+0 department. Excess vented to atmosphere. Con densed benzene blown to condensed benzene receiver #27. Bottom drain cock, Presstn* gauge, A connection, origi nally installed between item #33 and item #31, with a reducing valve, was removed, There la a spring-operated release valve to atmosphere, opening at lb gauge pressure, also a pop valv to open WATER PCB-SD0000046327 Equipment Mat, eontd . #33 High Pressure Ttmk,, omtA at 380 lb and a rupture diao to open at 580 lb Anniston Installed float typo traps to discharge conden sed beneen# from, the pressure tanks# items #J1 & 33, but discarded the* because of leakage past the valve a It is believed that traps made# for instance of 316 stain- lea* steel# with hardened seatings# Might serve* At present# the benzene is discharged by means of hand- operated valves# as described on page 44 above. > 103 #34b Charging Tank for Santowax Still Vertical tank with submerged pxwp #340. #34B reeeiTea crude Santowax from crude Santcmax receiver #20 via the suboerged pm*> #2QA* Return line from preheater #34c. Delivery of submerged ptm|? is to preheater or# for tbs preheated Material# to the still #35 There is an inter connection# low down on the side of the tanks# between #34A and #34B# also a 4* ecsmeetion# about 8" fro* the top for use in ease the bottom connection should be frozen at the start of the heating process. Inlet and outlet of boating coil* Manhole with hinged lid. #34a Charging Tank Similar to #34B# but only' ooeneefclons are the inter- e emu oting line between the .two. Vessel 3tA. singly , adds to the oapacity provided by 3*ffi# and it has no , pus^i of its own. #34c Preheater A gas fired coil within a brick-lined steel easing. 0a side of firewall remote from the still* Entry of erode Santowax from the puap #34D Is at the top of the ceil# and the flow is countercurrent to the flue gases* There are four gas burners. #34d Submerged Pmy for circulation Tor circulation of crude Santowax through the Preheater #34C. Explosion proof Motor. DSW 462166 WATER PCB-SD0000046328 Itodjaent List, wmM, #35 Santegiac Still Dratflnga 9C-8550 90-8551 90-8552 General Layouts,, Rarisoatal task with ehoirged pf> to external gas heated 11 #35A Preheated charge in from submerged ptffip #3to @f charge tank #3*B* Return lias frca ih till beater #35A ttaderfloif in from column #36. Delivery lift* fro* submerged ptsa^j #35B to th till beater, #35A, or, for still bottow, to the BB~4o de partment or to the pend. Wpour lino to eolwm #36, with bursting disci Inlet and outlet for steam coil. The te^>eratur spread in and out of tb@ Santcwsx still coil Is normUy 25"l80 on a Saatowax R distillation. Tb pif> baa a capacity of 100 jg>m and a 2" extra heavy pipe Is wed for the oil* X04 #35& Stm Heater Similar to Prebeater #3^0, but is longer and bus eight gas burners ,, Q&b supply controlled to give correct tesperature spread between inlet and outlet f the coil. #35B submerged .Pmfs For circulating still charge through beater coils and discharging bottoms to ,pmsd,,8 Explosion proof motor. #35 Ck&g-tt ' 12"pl&t colon. 3 * 1/8 drain. boles in each plate to prevent folocJq&g by fre#siag It is thought 1 x . hoi would be a better safeguard * Inlet for vapour at batten tnm stm #35* Inlet froa reflux split box #38. Wrfl froa bottom tack to still #35# Ykpour out to wodwaer #37* ' A much Binpler colmm will serve if only Bantwax R is to be udi. '- - #37 ^oodoasor dsw 462167 Single pip# in for* of xig~*ag and Jacketed for water or steam* Receive vspcHff1 fro*. tap of eolt^ #36 and deliver* condensate to reflw split box #38, It la i^Hsrtant to ensure that water cannot be trapped in the Jsdket aafi raised to a very high tes^ersture by the mcnfvtn*. WATER PCB-SD0000046329 Equipateot Mst. oootd 105 _ #37 Condenser, oootd Actually; only * dribble of smter la used, In parallel flow with the vapour, and the water stream Is so adjusted that th# roflttt split box teaperature is aroxmd 200C, (point #10 on the Multipoint recorder) for Santowax R. An earlier condenser, of shell and tube design, using Areolar *s a cooling seditna, ms discarded in favour of this siller condenser, because of mintamnoe troubles. There are no drawings, but Mr*. Kllenburg, Aug.23A8, wrote the following description* "The inner tub Is a standard 2* black Iron pip. Jacketed throughout Its 451 of length by a 3 "black iron pipe. -------- by extending & well "insulated 6" riser 8f above the top of the oolum, w were able to gt 45* of condenser to connect to the original location of the split box as follows* Pour 10* lengths of pipe were doubled back cm eaoh other to give & hair-pin slap condenser (a descending sig-eag. E.K.), with pitch of about 1" per foot. Vertical sections about 9 s in length were used to connect the long sections. A final vertical section of &! long connects the split flow box with the xig-sag part or the condenser. The inner pipe Is Jacketed continuously to prevent any cold spots wa the inner tube. -------performance tmder the --- heaviest lead 2000 lb total condensate/hr------. ---------pop the ortho and eta terphenyl fractions. Where Much lower condensate teaperatures are per- Mtasibl the wter rut an b increased.TM It would be worth while to provide a blanked off cocmeotlon for sailing the condensate even if a complete (sMpXlng) arrangement is not installed." #3S Reflux Split Bog ' Standard type, tot no reflux is used in the purification of crude Suntomx to Santomx R. #39 Bmt&mx 5 Receiver A vertical tank operating under a pressure of 50 m of c arury absolute. Receives Santowax R from condenser #37 via, #38. Inlet and outlet far steam coil. Connec tion to vactnm ptsip #40, Bottom outlet to the buffer vessel, itest #39B. Vfclvtr for breaking Tactaa, D3VV 462168 WATER PCB-SD0000046330 Equipment List, ontd $3% Submerged Ptn^a In lta #39S DsXirers to the Aroclor plant* ih Santowax H flaber* or the HB-^O plant as required. 106 #39 Bantwax DjatlHato Repairer Vertical cylindrical trosa! 5' x 51, DistiUat in froM tho reoolYtr* itea #39# s-hd out by aubsrgo4 ptm|>* Itea #39A. tforks wider atmospheric pressure, Saa steaa oil,) #40 Y@.oxam Ptap Manufactured tor Do Ylae. Between iten #39 and the T&etnm Anniston have a auhllmt trap and a raeuira tank in the XiQO|to allow settling of particles, Xo filter is employed, beeatts traces of terphenyl reaching the ptn^) are either dissolved in the oil or discharged to atmosphere.* and do no bars, DSW 462169 WATER PCB-SD0000046331 Equipment List, ontd 10J Iaatngntatloa flee Eravlag 90 >9060. 1. Conferiion Tfcd.t . Saab Mcrcrfeflp mlt hat (a) A L.&H. 'Klcrooscc* re cording-controlling instrument for tbs te^eretor of the convertor pot, which operate by oontroUltsg the ga* supply to th pot# SMj ease tnatrufflent, till responding to the thenao- couple ob the convertor, also controls the gas supply to #2 preheater# If automatic control should lead to towards a drop . In temperature of the #2 preheater, then this Is corrected by turning down burners on the convertor# (b) A Foxboro K0n-0ff" type potentiometer temperature controller for the $2 preheater to prevent the tem perature of this pot froa getting too high# All pilot lines are taken from the gas Hue to th #1 preheater, which only has mnual control of the supply# The Foxboro eontrolley is a safety deriee which will work If the converter control does net operate. The convertor control should cut the gas off on both Ho. 2 pot and th onverter pot If th tesperature gets too high In the eoarrertor, but If the control fail* the Foxboro cats off the g&s la Ho. 2 pot. There Is no definite UMt ott this control, but It operatea at approximate 76o0# () A LMf, fKleroBxl 12-point recording instrument for te^eratures at the following points s \ fl Ffepo\n? from outer vmpourlser coil to #1 preheater# #2 Ffcpoup from Inner vapeuriser coll to #1 preheater# #3 Wpour from #1 preheater# #4 Ffepour from #2 preheater. #5 Fhpow? fro convertor. #0 #2 preheater lead. fcop of oltnm fcondenser water outflow flu gas to vapouriaer dsW 462170 jf10 flue gas from v&pouriser. ill #1 preheater lead, #12 n> line fro* colum. The points for unit #4 and #5 have not been detailed her# -- they are two-pot units of a different and lees satisfactory design# W. ATER PCB-SD0000046332 Tkivdpm&nt List, ooatd 108 A. Cowwt(ia Xtalta, ontd (d) A Poxboro flow controller fop the banxetite supply to each wit, activated by an orifice In the food Um( Foiboro Pneumatic Presem? Transmitters Mr ham, installed In |foreber 1950 thane were installed, with on spare, la a separate room which eatained also the meters for the fuel gas, and which had a mmnleating doer to the control room vto neat of the other instruments war located These indicate the flow and algo transmit the ori fice press wes to the control instrument. There are also located, within the Control Room, hand valvea and pressure gauges for each benzol line See also page 31 above. B Off-gas Treatment (a) A tHg>er&ttn indicating instrument responding to thenaocot^les at the following points on the Hydro gen, cooler 1) Hydrogen in ^2 p_ oints}, !2 Hydrogen out (4 points} k 3' / Cooling water out (4 points). (h) A controller responding to pressure changes at the hydrogen surge tank #26 and controlling solenoid (more recently pn@ussa.tie) operated valves on the com pressors so as to maintain this presstire within the limits of 10-16 os. per sq,.ia. Robber fitting wist not be useS^^erS^^ewill be exposed to th process gas,because of the swelling which would be earned by the benzene in the gas C.- Diphenyl StlHf Each still hasi (a) A L.t I. *Microimzf controller similar to that used go. th convertor pot, but controlling, via the gas supply, the spread of teaperature between inlet and outlet to the heating coil (b) A L.& H. 6Meros*ttif multipoint recording Instrument for temfjemturet of Stm Body, Coil Met, this will he about the same as point #1. Outlet circulating line. Top f ooltsm. __ Reflux to column. ` n-?w 462171 05 #6 Ccedsnaesr Water If ttse circulating pupp should^ step* the gas striply to "* " '* "* ' WATER PCB-SD0000046333 Equipment hint,, contd 109 Z>. Santowax 8tin (a) A LeftH * flierwax' Controller timllnr to that used a the eonvertor pot* but onfepeUtng, via the ga Bvpply the 'spread* f t@^>@r&tur between inlet and outlet to the beating coil, (fe) A It:* We WcPOfWx' multipoin t recording Instrument for temperatures fs Still body* Hwter inlets Beater outlet* Vapour leaving eoltnm* Top inside of eoluaij Sight glass at resolver.* Bottom inside of solemn* Condensate in flow box* Preheater inlet* Preheater outlet Speciaen charts from most of these instruments were sent to Mr..K.Cooper* London* in October 19^7* a. ' Ami*ton. suggest using/glass wool trap* about 1 pint else, to protect instrument lines from blockage % diphenyl etc.* and wing glycerin traps to protect Ins tinmanta operating on benzene rrie#s. DSW 462172 WATER PCB-SD0000046334 coot og Bstnraw Aaolvtao mtSma.te for tte Inst&XX&tloa of 3 dlptenyl units (#u, 12, * 13), Jta 26/I7, ms glroa on paga 58 of tte re port % ffiwrcroft 4 Mather, Septaater 19^7, and. Is not ter, nor ar@ tte In*tailed 00at ftorts for otter part* of tte plant whleh wore glrm. on page 58a of that report. no DSW 462173 WATER PCB-SD0000046335 O'Oismm m the process m 5# ^Earlier Reports" listed on page 2 above, and "Hot on Choice of Process" on page 6 Wre, Effect of fferiatieo in Benzene Quality 3m also nota on benzene under "Specifleatiotm & Test Method, page 54 above. Anniston pepcart 1642, Oet.lSAl* states that. at that tin, ben zene with a distillation rang# of 79 A to 8l60 wu used, but that the freezing point had to b# 50 mlnimm* Traces of toluene caused tbs formtien of etc. which accumulated in the "heads* fraction of the diphenyl distiUettn, The Mount Of this was only about 0.065$ of the diphenyl md@. Aliphatic iJC>uritie war United in asount by the 5C spec iflostion. She material contained 0.06 to O.OSjfc total sulphur, but this was not thought to cause any operating difficulty, and sulpha? m fotmd to delay the foraatioa of carbon on the nefc&l etrr- fmrg of th pots. Experimental work indicated that water in the benzene favoured the formtica of carbon. (Excessive amounts, if pooped Into the vapourlxor, say cause a violent development of steam, endangering the Joints of the equipment.) The report refers to work by F.E,,Hubbard & R.A.Ewing, Sept. 17/41,. showing that fresh benzene gives 1.5 to 1.8$ aore conversion per pass than does recycled benzene, end other reports mention even greater differences. See for examples pages 112 & 113 below. This effect might be explained in one of th following ways* (1) The fresh benzene my contain some Material which pro ssota the reaction. * (2) The recycled benzene my contain some Material which inhibits the reaction. ' (3) The recycled benzene my contain sow mteri&l which desta?cya an inhibitor which is present in the fresh benzene. l&plamtien (3) seem to be ruled out by the observation that in ordinary routine working, with about 80$ recycled benzene, and about 20$ fresh, the conversion goes quite well. A* between (l) & (2) it is argued that #om grades of fresh benzene show even higher conversion rates and it has been shown by experiment that the addition of ertsln chwslcalo does actually speed \^> the conversion. DSW 462174 WATER PCB-SD0000046336 Oo--ota on the Promsa, ooatd Effwt of ^Promoters* in B&ozem 112 th$ report by Conor@p oited on page 3 above girea Urn follow ing results in a laboratory unit. Proaotor Added Ion (recycled. bem&m) Worn (freah tmm&m) Aoetio Acid Ethyl Alocbol Ethyl Ether He. Butyl Alcohol b# Butyl Alcohol iso. Butyl Alcohol Acetone ^ Conreraion at 800C ( Hpberry2Tin product) 10 14,5 23.0 24.0 24.5 26.0 26.5 ' 27.5 30.8 Effect of Size iof Doae 2,Of lax Propyl Alcohol 1.0 m m M 0.5 * m 0.2 n m 9 0.15 0.1 0.0 9 n 9 m 9 9 9 9 9 f Oomrersion @ 750C 17.6 17.0 17.1 l6,o 12.7 10.8 6,3 DSW 462175 WATER PCB-SD0000046337 OoMeats on the Process, oonfcd. ' Effect of "Prcttotorfl11 in Benzene, onto U3 Pronators have not been used at Amis ton In manufacturing work. Conover's report reeeanenda that If the tus of preno tow In routine mmrfMtw is planned, a trial batch ought first to bo carried right through to Aroolor*, to mb ur@ the produet does not contain any dotriaantal by-products, If the plant Is charged with fresh benzene the cowers loo, figure for the standard conditions will be about tut this figure win fan as the imchanged benzene is recycled, and at the end of the day nay be as low as 10$. The incoming benzene, though of very high purity, appears to contain enough of an unidentified promoter to have a Barked effect on the rate of conversion. The falling off in the conversion rate would naturally to very inconvenient in routine Manufacture, so the feed of fresh benzene is mde practically continuously' into the re cycled benzene tank, so that there is always about 20$ of fresh benzene in the feed to the vapourisers. The reports Just quoted discuss the conversion reaction in much greater detail. -` 3^>ts?iiies likely to occur in the fresh benzene are toluene, paraffins, cyeloparaffins, and similar products, boiling around oO0. Pyrolysis of benzene which is contaminated with these will give diphenyl which is likely to be ont&wmated with a variety of products, and .unless these eontaalmots are removed before the diphenyl is chlorinated to give Arodora, the Aro- elor* made from the diphenyl are liable to be contaminated With ehlor confounds in which the chlorine Is more labile than in-true Aroclors. Consequently the contaminated Areolar my be tweeted on the very stringent tests imposed, by some electrical txseri.of *Aroclors* . . .* . t The Biphenyl mde by MGLIs to be used to mk Aroolars, and Mr. T 0# &im, 0et.l7ATj estimated that about half the Aro- ler production would be as 1254 for electrical uses, so the question of stability of the Aroelocra is of importance to ICL. Apparently, however, the trouble has been limited to "Pyranola H, mixtures of Aroolera with trichlorbenzene, and it is the tri- hlartonzea which tea been ulnly at fault, Mr, KUeaburg suggested that ware intensive fractionation of the diphenyl Might eo^emaie for the use of inferior benzene. Dr Btrdy, Dec.23/47* stated that benzene cont&*ijmt@d with paraffins, would yield styrene and apparently vinyl biphenyls, d that these products, on edalerlnatlon, would yield mterials ' . DSW 462176 WATER_PCB-SD0000046338 Co--seats oo the Process, contd Effect of ^frmmtoxm" la Benzene, contd liable t mm skin trouble*. The chlorinated products Might be stabilized by being held at high teaperattn*! , but it ma net certain that the stabilization would go far enough* Toluene on pyrolysis la said to give some styrene* and it was believed at one time at Anniston that chlorine derivative of tyres were oaiiaing skin troubles aaoog the workers in the Aroolor plant* See page 16 above. In a letter dated April 21/^9# Kp Ellmiburg listed alkylated benzenes and alkylated biphenyls as possible by-products from tbs used impure benzene, and he stated that styrene and stilbene have been Identified In the "heads" fraction of the diphenyl still. Benzene hoaologues on pyrolysis give also dibenzyl or deriva tives (H.Szwaro, "Batura", Sept.20A7). Effect of variation In Ti^9-Teaperature of Exposure The process is normlly run with the lead in the 3rd pot at not above 840C and with a benzene fldw rate of 170 B.S.Gal/hr., these conditions giving about 18$ conversion of the benzene into diphenyl, terphenyls etc The retention tine correspon ding to the given flow rat, naturally depends on the pressures at which tb pots are operated. Am the process la carried on day after day, the vapour passages become more and acre restric ted by. the deposition of carbon in them, and this raises the pressure in the pots, sod therefore the retention time increases. Also, orifice plate restrictions are being tried In the exit from the 3rd pots. When the pressures increase, from either cause, the practice is to reduce the teaperatures enough to mints,in the saw coversion figure of about 18. Increasing pressure# also rive lees entrainment of lead because of the lower linear velocity of the vapours, and the lower tesperatures should reduce the corrosion of the pots, but Anniston experience is showing that these advantages say fee dearly . bought, at the oo#t of increased maintenance of the pot covers, gaskets, etc. See also under ^Process in Detail*, page 3^ above. OSW 462177 WATER PCB-SD0000046339 Qoaaeota 00 tbs Process, contd Effect of Variation In. gjaa^enperaturc of Exposure, ootd Anniston report 1642 of Oet.lsAl 1gives the following state, mmt of the effect of variation in pot temperatures * !e^. of lead in lit preheater Tn> of lead in 2nd preheater Tea?) of lead in convertor ' ^ Conversion to crude diphenyl #9 tail 580 TOO 580 5|0 580 580 725 725 720 800 800 840 840 840 825 825 800 Carbon formation becomes 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 variation In pressure la the. lead pot* ms studied by Conover & Hoff of Plant >A*, see report Oct.5/35, At '800C under certain conditions they obtained. 6,2*ecmverclan at 5 pa%, and 14.4 at 38 P*ig. Xt Is stated that ratio of terphsnyls to benzene in the reac tion product is about the same as the ratio of diphenyl to benzene. At 28^ conversion, the ratio of diphenyl to ter- phenyls, etc., (high boilers) is about 4.5 to 1, and the amount of carbon formtien is not too serious, but if the $ conversion Is pushed beyond l8, the ratio of highboiler* to diphenyl in crease salao the ratio of carbon to diphenyl, so 1856 appears to be about the eoonoteio balance for Affleriean. conditions, even though Anniston cannot sell or us the whole output of high boilers. See ^Deetgn lata for 4th TEtait," Aug.9/39/ for a curve of costs v % conversion. . Raising the pot te^>erature gives an increase in output of di phenyl with relatively little increase in the consumption of fuel gas and at times wnaXX variations in conversion rat lave been mM at Anniston to get a greater output of diphmyl, at the cost of a higher proportion of wastage a* falghbotiers Anniston report 1642 cites a report by Durgin, Beald 4 Perry, Kay 15/31, indicating that if Mghbotiers are recycled in the banxene, tbs asoimt of HB in the crude diphenyl Is not increased, but that It has a higher boiling range, Anniston experience Up to Harefiiber/50 indicates that recycling of diphenyl in the b-emsen increases the amount of carbon formation. OS W462178 WATER PCB-SD0000046340 poenta oa the Process, contd UL6 ?he tcnzeti distillate from the diphenyl still is examined be fore being recycled to the e carvers ioa stag. It usually contains very little diphenyl, but If it contained more than about 3# It would be fed back gradually, or In an extrema esse, returned to the beads is ta.Ua tank for redlstiXXation. It was stated In September 1947 that conversion m.s reaching 13# in the teeond prebeater and 18# la the convertor. The extent to which the reaction proceeds in each of the 3 pota, naturally depends oa the conditions of t@s?>eratur and pressure la each pot. Anniston report 1642 gives the follow- lag figures for vapour leaving tbs second preheaters 2nd preheater lead temperature 64oc 720-725C 7750 # conversion 1.0 4.0 to 5.0 10.0 Distillation of the Crude Diphenyl . By-products, which boil between benzene and diphenyl, build up, only very slowly, in the continuous recycling of the "beads* fraction, and it Is not difficult to run the fractionation so as to give diphenyl of the necessary quality. Mr.KLlehtrarg, May 12, 1949# stated that about 0.1# to 0.2# of the diphenyl yield was * Id-tracked la the form of the oil from the "heads" fraction. Amis ton report 1642 gives O.oSfj# on the diphenyl as the amount of styrene, etc. formed* Variation la the diphenyl distillation conditions Might also go soaa ray to offset the effects of iJ^urlties In the benzene used, see pages 55 & H3 above. Benzene recovery from the ^drogea Amis too, reported moderately good results from scrubbing the hydrogen with mineral oH. An activated alumina absorber was in stalled at Anniston, to take up benzene from the hydrogen, but it gave poor results and was discarded In favour of the presmt cadresiioo. system. It i* thought that the alumina was not pro perly re-activated. See Anniston reports 214,Sept,22/33, & 948, Aug.23/35. Since there is a use for the eoz^ressed hydrogen, the compres sion 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, under the taoiti, but difficulties In lemming, the correct air-gas ratio l the burners boos, caused a dlseoaiinmtioo of this use of hydrogen. DSW 4S2179 WATER PCB-SD0000046341 COST MIA labour Requirement . At Anniston In IbwAr 1950 f on operator per shift could look after up to 5 conversion wilts and ojm diphenyl still* Is addition, there was one chief operator per shift, (but Mi reopcmiiihdlitieo Included Arcelor & BBAo8) end there ms a general day fore*an (Cwvy)8 covering a masher of depart- neat*, inoXuding Aro-eiors, Hr, ELleaburg wrote Aug. iS^ASj about the breakdown of the various service charges saosg the different products 1 Diphenyl rude Biphenyl M tilled Steam, Ihe City water, eu.ft. Recovered water, eu.ft. Gas, eu.ft. ELectrieity KH 0.10 0.037 0A9 13.5 0.050 0.91 *.%0 2.2 0.008 The mita are given per pound of product -- for lwne/\Qs and he eassents that there are 8ascoal variations In sucsh figure*. - H7 Repair Work The practice sheets, pages 120 & 121 below, give a record of the frequency of various repair ibs. DSW 462180 WATER PCB-SD0000046342 118 i *it lor t *i( fur X.S. tf c-9 '7*fT i7 f3 <7**7 C^ Ara-q; ; i5 e >i t/c "7 'sv * ~o *C H Yf F MT^ KTVK 1M aCTM. f--af > m <7 l OSW 462181 r*4t4 7*, We C"* *<! 1 * 7 ff IV n f * 64 t7 % ru ~T / ^*4 47 47 ro IM 7*-* T>3 *0 1 3* gl 0 4* 4t <1 11 // MA4 f% 'ft 4 f 71 4 < 1 44 - >A W*0 f7 4N K 1C IS ^ if v6 at *? I 9 TV *4 1 \rt 13 -- Iff *1/ l* tff &&C 47 V JT? n Iff <rr M> ff / r 4/ 0 1 O If 'll */ *f4 1 fi i* r id n <3 ** tr ,,1. - 7lX 4-- - 143 7* 11. 1n -- m a am V. fr3f 1 N% 4-N 7f 01 64 U Ur} ?/ -- > oj Tf Ul ai - t.-g J * >-- xa '^70 1 *Ob - e-f 0 *74 3'M-? <l* '07/ e &J * t ru ' >7/ *o uc W7 0*/ 71" tvr ffdf Olw 077 irra *6-T 00/ 'V# f Ulf 0/4 1ST *1.7 OO/ Ocj/ `*>3 JOf Vfi. no a*f -a ^ ff <* -00/ * e* ) /a#/ ^ % `414 4 **a i-ua.' in 17 i-i.f ' * \af 175 7 off V-4-^ 01/ Olf tKf / *.7 V*f V4l |,Vl cv--. *i:f #/ -03.7 *0 0 J Off 1 / *> >6 - <7 i`1 7T1 ^ * fill * P 0-&- o-4 $? #Cl n " t ^ >* ] *" ] r* 770 ' raff) | r-m , *047 ,, -f- f"*-f ff f * 4 <"* WATER PCB-SD0000046343 MOMAKTO CHTOJCAL --2&c COMPAQ 1. ~4> Ku^eLi- (dsvUUlC*. fcA-b- qL&L* / 4*> >4^ **7- ) u. V rua.-^M. coal . rrmwr a* 4 r. U.sds. s< DSW 462182 -1*4. rt? & 5* SS # A+ *7 l ST on lo^ oil T57 Ov r 1C 'r 55 . 'C\A u7 *7 # 0 6 OOJ o 3 ' ( .OM U 7s* < .# OM *>-0 *7 *-S a-f IOm / 1-' 1.0 5 U T9 " I5 / .0 / o a o* l U .f f-/ y r s o/V rv) JV '3U O-x Cl 5 /-- u ora X iV *d7 ru IX 57 V. 7 /f 27 50 5a a i *7 27 >e a<u -oo^ ora .*'( 5 '5 a jTj roi ,#T *j c7 orC Q5i X f7 X *7 TO- VMf Of # Tv fel /.n is { ^ w ^ w* . **>. ixr 7f -?f M of ^'f V- *>Vt 7 C " 'O iq - < a-0 o-t -TV -^t if . *-7i . M J -- _(Ji _ /.kJf , .*1* ,7* - ,07 , *'01 , TVO < 07 051 nr) . <}>4-7f 7H l-*' 1 OO l 4X7 t>v wf 70 X *7t t 2 OO WATER PCB-SD0000046344 i 12 0 1 3~rT7~Z-' j ~Tiir..7 Vj- * *"*.*. ' * -.**< 5 5<*. ' 1 Se pst# MZ____ A/ ` PoaodlT^ V ALJK M.M f llLSJt ' f9,M t x6,89 r ~~f5FWT i o.rm ftiUaof mrm: I e.im . v6o'Jm> i nrM t rl PfolvtlA* ^ FoudAj 1 TIOF 1 r . .11 0$. felt Da 3.1* I Gmtomx. 0 ' '* i.rm.iv) 1 WroflBa " '< ;. lrr.km 1 Ba Materials tad Missal - Ariml Gallon ifa^Ks `lam * B*ecrwT rs.fiso 1 ftL. UL71 . 0.1703 0.1673 o.*W 1 feuartiter tatio## . l.im o,oco Bte* - l>f. 7,976,000 1 ij-jg e.oei 20.000 *fc*r-Cltr-Ca. Ft. 113,000 ] .019 f 6.sh7 3.000,000 ?asr-E&oor'4-Cu. rt. 3fl.fc03r000 3.026 t lv 10.W.6 IS,338,000 (Jo# - Cu. rt. 0.036 n.*a nwttlflltr -XUS. . 17.666 113 000 1 (VU r ' 8 Sr**! - %CMTB Dm. k,6. Msm Boars Uxr ti#. M.3. 696 1.U8 Otwetlm /TL'tf 6S6' 1.212 7 Matntwvmrw 7.672 1 996 11.720 305 Feoklne 54 ShltrDloc WT 5.39*t 2^.LtO -i 100.0 0.63 99.57 0.7 1 2 1 1 1 1 1 "1 1 1 Unlt-fioura 6.696 > 32 6.602 0pratliK Wne Bovtm - CalratW1 Hour* - Brat Do*n Boun-CBroet Ch>rfLt*d Boars - Detlar 5our*-ff<rt OwroteA .. Unit ourf* 4 JlO 8 1 160.OO 3.WJ( 1 6.60 *5^024 1 93.l0 . 308 1 _____ tSJl J 92.V3 tl*rs 4 af Qroe# 0p<n I1*TBI . Cl S3 OocxwUBOlar flar^ 1 11 1 l.CXt CUon Gcomnac3ni(BmaX} 1 Cl#an Dirtrilmtor `7 2I dMn Carbon Trap Clm Lsad gras 91 fi Clen Colusa Cln Teparlrar Coll* ? C&aruw Mjrtrflbufcar Cat r. 12 Qumm TmI Pot* 11 Omumb LsM Tran Qum* Then-moocmpY/s It Cbsntja ?W-lfc! 1 3 Champs annmarmdk Tlai^ Ciumtrm Fra*ur Gwj&^mi Repair 7ULmu Tin Ifl &&a lAjmswreaS It CU*sm 41 HT Ulst. Wpair atalr 2 8#s*lr fessrfmr (Soil EUab run %smd Plrntm "IW# TlIMya 1 11 P Bumms fe TW Mjrt. k Ojsmm Ocmdsm^m- 11 Oumfis ImJI 2#t p. V. I repair rvwsr. W*i 11 n " Pago- 1 XHFBKinX 8XPCET Paga - 1 46?183 WATER PCB-SD0000046345 ft KELeaburg, January 20AS# gare the following break down oT the fuel gas consumption? cu.ft. Ab Aroolcsr DlstHlatlao. 066 Biphenyl - Crod Units l6eJ Biphenyl - Distillation 2,2 Saafcotwx R Distillation. 1*5 Calorific value of the gas about 10^0 B,th,tr,/eu,ft, at $0F and ataospherla pressure* osw 462184 WATER PCB-SD0000046346 121 c " -Psss^-ayst Papar U-aar-e-OssfS -6- DSW 462185 jf WATER_PCB-SD0000046347 122 A,eXSO|.SDOMEJ[t Uhl* report la mlnly a eoopiXatioo. of lnTermtloo drawn frcm Anniston reports and froa dissuasions and orreiipondenee with mny Bombers of the Annis ton staff** whose billing and able help Is grate fully resneMjerml. The reports mde by Messrs Bavercroft & Mather, September 19^7* hare been Inoorporated, also that of Mr, H L< Harden, August 3950, aM ob serratloaa feade by the author during risifca to Anniston. DSW 462186 WATER PCB-SD0000046348 Index |>ag@ 1 IHDEX (Olderlined figures denote the acre important entry . vmh&r any cm subject) ASSBQHLEmHfflfT................................................................... .... , . , 122 Alladm absorber cm hydrogen (abandoned)...............................116 Aroclor, electrical standard required ........ 55,113 BKBZEHE, catalyst In, see "Benzene, effect of catalyst0 danger from overpunping into feed tank . . , . 30 danger from water in . ,29,83 discharge from H~ pressure vessels . . W,103 effect of catalyst in .....................................5|29~,111" effect of I**>urities in ...... .3,16,55,311- effect of promoters in.......................... , 332- effect of sulphur in....,.......................... .HI effect of water in, see "Benzene, water in" feed arrangements. ...... ........................... 29-,83 see also tmder "Instruments0 feed rate. ........ ............................................ 31 feed rate during starting up............................... . . 37 filters............................................................................... 30,31,85 handling........................................................................ 29-, 83 leakage into Time, method of detection v described. . . ...... 91 mentioned. ..... 32,36,76 leases in the hydrogen stream, Anniston report sntiond ..... 3 physical properties of .10,11 ptmqps. ........................................................................................,83,8% quality, effect of on Aroelar workers, . . 16,114 qmlity of, suggestion to do better free- tiomtion of diphenyl to com pensate for poorer benzene . 55,U3,H6 receiver from diphenyl still 99 recovery fro* off gas, see under recycled, mts more slowly, see benzene, effect of catalyst* recycled fro diphenyl still, examined , . %7,76 recycle feed tank, , . .29,83 recycling................................................................. . .5,29-,XU recycling should be fairly uniform ...... 30 risk of flooding convertor with. ....... 30 DSW 462187 WATER PCB-SD0000046349 JXidex page 2 Benzene, specifleations and teat nethodfl. , , * stare tanks. store tanks, fire arrangements , , , , store tanks, objections to internal colls In. . . . ..................... sulphur In.. test records ...... .......................... . trap failure In Hg system ...... trapping of water from ..................................... water In, dangers from ........ effects of .................................... sources of ........ . Buildings ................................................................................. see also under "Ventilation* Bursting discs, on diphenyl stills, ...... on Eg Teasels . . ............................... By-Pa** flue, see under "V&potxrizer" . . 84 M,iu 44^03 .2STO .29,83 . , 82 .18,96 18,102,103 GAHBOH, build-up, bursting pressure of............................. . . 89 build"tp, favoured by presence of water . . . .Ill build-t^p, favoured by recycling diphenyl, . . .115 build-*$>, in the conversion system. . . . , 34,114,V/ burning out from pots and pipes ...... . . 41 detection of blockages. . . 41 dioxide, connection to convertor. , . . . . .19,31 dioxide, handling ............. .31,38 dioxide, not used in diphenyl still . . . , .18,48 dioxide, suggested use to remove earbco .. . . . 4l . .dioxide, use in checking conversion system, . . 37 lntentiom.1 addition to lead pota suggested 22 precautions in burning out (damage to equipment). . , . 41 (risk of poisoning by lead vapour) . , 4l suggested removal by C02 ......... . . 4l tetrachloride In fire prevention. ..... trap, cleaning of ............ . trap, description of. ........... . 94 trap, operation of. ............ . . 43 Catalyst in fresh benzene, see tmder "Benzene, catalyst in" Charts, see under "Instruments * Chlorination of diphenyl, mentioned ........ see also tmder "Aroclar* Chlorination of Santomx ............. Chlorine, determination of. In Santowax........................ Choice of process . ...................................... GoXothi cm convertor, arrangement of. ....... convertor, choking of......... . convertor, efficiency of................ . DSW 462188 WATER PCB-SD0000046350 lodes pa^ 3 Oolxam on em?srtor, operation of, 43 oniwtop, packed colinm unsuitable. ......................94 coowrtop, repair of*.,..,..,*...93 diphenyl a till , . , , .......................................................97 Santowax still ,104 Cement* on process, ........................... . . , . ,111 Compressors, see under "r4rogtt, eospreftsora* Condenser* as conversion units, descripfelon of ..... 95 operation of 43 on diphenyl stills, description of, ..... 07 operation of. ...... 47 on Santovaz atill ............ 49,104- Control tests. . . ........................ ........ ,43,47,75,116 CmtM^lea pots, baffles ........................................................ ... 33 baffles, sagging of 41 causes of failure of, 4l cover ..............................................................41,42,86- oovers, bolts of, cut,in. . repair work . .....................................88 covers, Joints, see under ''Gaskets" covers, warping of , .................................. 42,87 cracking of well be tween pot & rim . .4l,8o depth of lead In ...........32 description of ............85 _ design of dip-pipes ........ ..86 e>4>tying of ....... ............................ 39 equalizing lines on ....... . 33,90 flue arrangements................................. 3^,41, o? leakage of lead or vapour from, detection of ........ 42 maintenance of................................................4b; 90 living without eaptyisg ........ TO / operation, of...................................... .... ... 32 overheating of upper walla. ...... 4l pressure gauges, see tmder "EqtaUzlng line** also.............................................. 42 pressures in repairing ....... ................................. rims thickened. ....................................................... 88 rim welds cracking. ........ .41,,88 rotation of between different settings. ..........42 setting of.............................................. .33,88 see also, "Conversion Pot*, flue arrangents " starting of.. ....... . .... 37 stopping of................................ 38 teuperatures of ........................... 33,34,51 temperature control methods ..... .107 DSW 462189 WATER PCB-SD0000046351 Index page 4 Conversion pots, teiperature controllers. , , , . , ,34-, 107 to bo free fro* casings. ............................. ."IS? vibration of. See `Vibration* Conversion process, adjustment of tenperettn'e to eoaponsate for pressure varia tions* See "Pressure increase*, ewpeasatiatt for* degree of conversion In moh of the 3 pots. ***** .116 description of............................. .... * . * , 32 effect of variables in ****** *iH- two pot system mentioned * * * , 32,82,85 Conversion test, details of . ***** 75 mentioned ..................................................................,43 Cooling fans...................... .19,20 Copper and alloys, f&ilm* of in Hg system. * * 24,44,101,103 not reamended for condensers ........*..95 Corrosion, effect of iB*purlties In lead feared* ***** 57 general note .............................................................. .... . . 22- of convertor pots. ..........................................................* 4l of convertor pots by lead blast (Anrfeton report}* ********** 3 try stainless steel for traps in Eg system . .103 Cost of equipment .................................................. *110 Cost of manufacture................................. ................................. .117- manufacture, practice sheets* ......... .120- manufactura, versus % conversion. . , *......................115 Cost sheet, diphenyl. ................. .118 Cost sheet, Santomax B. ........................ .......... .119 Crude diphenyl, analysis method for 76 eoafjoeitlem of, see *Vlcm Sheet* tanks, description of ... * , 95 Crude Santowax, see "Santowx, Crude" mSiGI DATA. BOOKS (Anniston), listed *..*,.*. .3*4 Design data book, (Loadon) discussed by Anniston staff. . *4 Diphenyl distillation, consents on. .......... .116 control teats* . .47,76,116 out point* *......................... 45,46,5^116 cut points, variation of msggested to co^en- sat for poor benzene * * *55^113^116 description of ,.*.*.. * 45- fire hazard In 1? heed! fraction, aaotnt eliminated .... * *28,48,116 reflttt ratios 45^4-7,52 Diphenyl, M3L do not expect to tell....................... *7,48 physical properties of, ********** 11,12 specifications awl teat methods. *.............................. 58 sw 462190 WATER PCB-SD0000046352 Index page 5 Dlphaojl still, bmzme receiver of, described, . ,, bottoms, see "Crude S&ntowax* bursting disc on, eolum, see under "Colwma'' condenser described . , ..................... condenser, Indirect, cooling of , condenser, t^>, control of ... . condenser, heat exchanger on . water of . condenser, crude Santovax receiver, description of diphenyl reeeirer distillate switch box............................. formerly direct fired............................. heads & tails receiver, ...... heat cut off If pmp falls, . , . heat exchanger on condenser water , heating coll* ........... preoat^tioca In charging discharging. , . . . starting safety disc, see "Biphenyl Still, bursting disc", temperature control temperature recorder, test records.......................................................... Distillation, see "Biphenyl distillation" and "Santcra&x distillation" Drawing list. ..................................................................... .... , 99 96 97 : V`Vt oo 9S ,97 108 n . 48 18,48 . . 45 , . 108 . 52,53 .77 MJRLXKR HSPOrars, see "Previous reports" Earthing of vessels 17.84 Effect of variables, benzene quality. .......... Ill catalyst, see "Benzene, effect of catalyst In" pressure ......... 34,87,114,115 promoters.............. 112 - recycled bensene 112 recycled diphenyl, ......... 115 recycled high boilers, 115 tia~te*f>arature 114 - Efficiency figures, see "Cost of manufacture" Anniston report mi losses of benzene in off gas. ....... i . * 3 Electrical us of Aroclors, see "Aroclors, eleotrieal standards" Baptylng of lead pots, see "conversion pots, n>tyAng of Equalizing lines <m convertors, e "Conversion pots, equalising Hues ea" Equipment Cost. ................................................................................................... . 110 Equipment list *. .,... ..#, 83 * Equipment list, general notes on. ..........................................................8g Extinguishes1, 8 "Fir Fighting" WATER PCB-SD0000046353 Index page 6 FENCE, round the pet 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 eontrollera In bannene recycle feed tank, e "Benzene feed arrangwaants" Plow controllers, see "Xnstmnents* Plow sheet of Materials ................................. 25- Fractlonatlng eolusms, see "Columa * Fuel gas, burners ............. ........................... 85 calorific value of. ............. 120a. ealorlfio value, Mentioned ......................................................93 connections 3^ constuition of. ............. 117,120a. ecmsiSEption of, re?,a)e<l to pot tex^eratures .35,115 control 36,107 asters................................. 31,36 GAS, see Fusl gas" Gaskets ......... ..................... ..... .......................... 24 Gaskets, making of for pot covers ..................................................87 Geraon reports listed .... ..................... 2,3,6 HB"4o, Mentioned ......................................................................... 7,18 Heads & tails fraction, build-up of by-product In, see "Diphenyl distillation, heads fraction amount eliminated Heads & tails fraction, eoa5>osition of, see . tinder "Plow Sheet" Rads & tails receiver, described .......................................,.98 Heat balance. .... .......................................... ......... 15 Heat exchanger on condenser water, diphenyl still .... 99 Heating coil for diphenyl still, described. ....... 9o operation of, see ^Diphenyl distilla tion, description" Beating colls for S&ntomx still ......... 103,104 Heat of reaction. ....... ........................... ....... 15 Heat treatment of stainless steel recoaaaanded ...... 22 Health considerations ............................................... 16 See also ^Welfare" skin troubles In Aroclor. ..... ,16,56,: High boilers, ratio of to diphenyl, produced. ..... " required. ..... Hydrogen, alumina, absorber for benzene abandoned. . . . .116 benzene recovery from (Anniston reports). ... 3 benzene recovery from, oamaants on. ..... ,216 carbon dioxide contamination of......................,19,38 ensures s Ion, choice of pressures at two stages. . , . . <. . . .44,101 <N cn CCNO*r 00 Q WATER PCB-SD0000046354 Index page 7 Hydrogen, agression* flow sheet of materiala, see under "Flow Sheet* compressor, described, ....... apresBor, lubrication of ... . . eoj^presgor, operation of Coolers. ....... ............................ ...... 101 101 .. .*4,101 100,102 cooling and eagres a loo. ...... . .44,101 dangers.................. .... ....................................... formerly burnt with fuel gas . . , . 18,12,101 116 oxygen determination unnecessary . . ... 19,44 pressure control .......... 44,100,101,108 recelrors described. ........ , . . 100,15? surge task ............. a 0 0 100 tesperature recorder os ooapressor . a 4 10Q traps on Instrument lines....................... 9 9 & & m 10O traps for benzene...................... . . . . . . .44,103 uses for. . ............ 7, vest connections frost crude diphenyl etc, tanks, . . < . 19 IOTERMEBIA.TE FRACTIOUS, eoaposition of, see under "Flow Sheet" Instruments 107- bonzeae flow o ontrollera ......... 31,108 charts sent to MSL ...............................34,50,109 conversion pot temperature controller, . , 34,107 conversion unit tesperature recorder , 34,107 diphenyl still ......... ...................... 45,108 diphenyl still, cooling water, so . longer instrumented. ..... *7 float controllers in benzene feed, vessel, "see "Benzene feed arrangements11 Santowax still .............. 50,109 Insulating coapoxaad "66" for pot furnace Joint, . .... 88 Insulation..................................... .... 90*94 LAROTO RBQtJIREKEBT............................................................... . . . , .117 Lead, depth of, in pots ... 32 effect* f impurities in. .......................................... . . .22,57 emptying pots *00 39 entrainment from pots ............ . .38,41 forced back to vapourizer .......... . .38,91 see also, ^Conversion pots, equalizing lines" handling (roping off the area). ....... . .20,39 leakage into furnaces ............ 23,42,85 detection of ... * . ... 42 Baking up losses of ....... . . i . . .32,40 olds . ...... , , ... 22,40,93 DSW 462193 WATER PCB-SD0000046355 -I Index page 8 Lead, oxide, corrosion of pots by. ......... .22,23 poisoning, little risk of. . . . .................................... 19 pots, see "Conversion pots" quality of 57 renelting # 40 pectrographle analysis! of, aentiooed ...... 57 Lead trap, cleaning 0$ described.................. ...........................,92 nentioned ............ 39 description of. ............... 92 central tuba of, shortened, ......... 92 Bust be heavy steel ............. 93 need not be stainless . ................................ ... 03 operation of....................................................................... 43 repairing of................................................................ . 93 MIfflEEAJfCE OF LEAD'POTS ......................................................... 39,41,89 JfeJte-tflp water tank on diphenyl still condensing . syatea ...... 99 Monel badly corroded trader pot conditions, ....... 22 Montar 9 ..... . ....................... ........... 7,4o Motors, type of. ............................................ 18 HI0KEL, and alloys rich in nickel, badly corroded trader pot conditions ...... 22 OFF GAS, see "Eydrogen" Operation Manual, (not yet written at Anniston). .... 4 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 variables" roaring of gas through. ... 35 Outlets for products, as cable box coapound ....... 7 electrical use as Aroclor. . . 55,113 as firelightera (not suitable), . 7y general ............................................................... . 7 in BB-40..................................................... 7 hydrogen. .7,115 roofing ocs^Jotmdfl ......... 7 Outline of process. ............................................. 5 PACE3M, diphenyl welted into drtiM Is inconvenient . . ,48 Santowax E is now flaked ........... .50 Patent position, Anniston report cited. . ....................................9 cm high chrose alloys for lead pots. . .22 DSW 462194 WATER PCB-SD0000046356 Index pa*s 9 PIpa lines Jacketed, ........................................................................82j 83*95 See also under "Water in Jackets" Pipe lines traced, . , . ......................................... 82 Preheater pot, see trader "Conversion pots" Preheater* tubular* see tinder "Conversion process* two- pot system". Pressure Increase by carbon deposition ....... 34*114 Pressure* compensation for by altering tenperaturea. 34,114 Pressures thronghout the conversion trait . . . , . *34*35 checking . with C02. ... 37 Previous reports listed. ................................... 2- Procesa In detail. ................... 29 - Pronotors in benzene* see under ''Effect of variables " Propei'tiea 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 trader "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 trader "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 Santomi still described. . . , 105 Repairing coluaaa and lead trap......................................................... convertor pot 42 Repair work figures ................................................... 117 Reports (earlier) listed* see under "Previous Report*" Roofing caapoimd from chlorinated Saatowax. ...... DSW 462195 SAFETY CONS ITERATIONS ...................................................................................16- hydrogen, .18*19*101 showers ............. 19 Saaples sent to KCL listed. .............. 21 Ssntowsx* crude* analysis of by distillation. ..... Jo charge tanka for still ........ 103 eonposition 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 dscoribe^l 9o WATER PCB-SD0000046357 Index page 10 S&ntowax fCrude, still,, ................................. . . , , 104 column on, 104 condenser on ........ .,#9,104 designed for separation of the laopwrs #9 eapUsp design Mentioned . . . 49 beetor described..........................................104 operation of..................................., . , . 49 preheater described, 103 recoil's? ............. 105 leap era,ture controller ...... 109 tasperature recorder ....... 109 vacuum vessel. , ................................ 106 Santovax isomers, amounts sold......................... 8 Anniston report on separation ' of cited, ...... 2 outline of separation process . . , , 5 specifications and test methods , . , 70 Ssntowax 0.M.&P. see "S&ntowx Isomers" Santowax R, flaking of, .......................................................................5,49,67 handling of....,.,,.,,,,,*, 50 packing of. .................................. , . 50 reoorda of test results .......... 69 specifications and test methods ...... 64 Scale of working. . , . .................................................................. . 8 Skin troubles attributed to poor benzene, . . . . 16,56,114 Specifications and test methods , . . ............................... 54". Stainless steel pots, oarburatioa of surface suspected, . . . 22 corrosion, see tinder "Corrosion11 effect of lapunities In lead, see wader "Lead, effect of iBfpurities in* effect of lead oxide on, see water "Lead, oxide" heat trestnant recosaanded, . , , 22 types of stainless steel 22-,86,88,89 Steel floors, advantages of open grids, . , . ,19,50,82 Still bottoms, see "Santotmx, crudeH Styrene, effects of on workers, see tinder "Skin troubles" Sulphur in beoxene, see tinder B0ppr* Sulphur delays the attack of ben*one etc, cm. pots , , . 111 Sulphur, determination of. In Santonox. ..*,, 68 Stn^ tanks, see "Crude diphenyl tanka* TEMPXRATTOES, adjustment of to oo^ensat# for variations in pressure , , . . ,34,114 Te^erature control, detection of overptaping of benzene to convertors, , , ,30 DSW 462198 WATER_PCB-SD0000046358 Index page 11 Tesficrature control In diphenyl still. ........ 45 Tprature controllers# see under "instruments " Tesperattn?, effect of variation of# see under "Effect of Variables* Tempera at various pointa in the oonversion ' system 22^2i>51 Tes^veratucr of pot# varying with the benzene mte. , . 84 lagging behind controller. .... 84 Terphenyls# see "Ssntowax isomers" Teat method,# see Tontrol Tests3 and "Specifioatioas and Test Ssthcds" Tbaraal balance# &o "Heat Balance* Tube process# see under "German Reports* and tinder "Choice of Process " Tubular preheater# see under "Conversion process# two-pot system" TOPS for products# see under "Outlets* "VACUUM pu^J for Saatowax still described. ...... 106 Vsouffli 8tm, see "santowax crude still" vessel# see "Santowax crude still vacuum vessel" Valves. . ...................... 82 Vfcpourizer# blockage by lead, see "Equalizing Lines * and "Lead forced back to vapourlzer" blockage by solid# unlikely . . * . 3 ooil life ............................................... .... 91 described ............ ... 91flue arrengeaento ........ 32#37,86#91~ leakage of benzene into, see "Benzene# leakage into flues" operation of. .......... overpus^Jing of benzene into pressure drop through ...... tanparaturea In.............................. . Ventilation ................. Venting of conversion unit. . ............................... . Vibration of pots........................................... .... . . .32,37 . . 30 ,. . 34 . . 32- 16 19,82 : WATER in benzene, see "Benzene# water in" . Jackets of pipe line*# danger froa .... 96# 20% see also tinder "Pipe lines" Welfare.................. .... . , . ............................. .... 19 So also under "Health" Welding, fire hazards In. ............. .17,18 boat treatment reeonaanded after ....... 22 on oolump and lead trap. ...... .....93 HELD IMTA# sse low Sheet" dsw462197 WATER PCB-SD0000046359