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INTEROFFICE COMMUNICATION Ponca City, Oklahoma July 24, 1970
TO: Mr. J. D. Minott, Westlake, Louisiana
subject: APRIL TURNAROUND CATALYST SAMPLES SUMMARY
This is a summary of our activities and conclusions related to the catalyst samples analyzed from the April turnaround.
1. The balanced operation that resulted in more reaction in R303 with lower temperatures in R301 was a major process improvement. The primary mechanism of catalyst deactivation during this campaign was copper chloride migration; whereas during the previous campaign, it was physical deterioration due to large coke centers.
2. Most of the prior analytical test analyses have been repeated and extended and improved for this series of samples.
3. We have developed an experimental technique to measure catalyst acti vity.
4. Experimental catalyst activities were determined for the samples and are included in the attached curve. It can be seen that catalysts that are twice as active as new catalysts exist in parts of the reactors.
5. A detailed theoretical analysis of mass and heat transfer effects within an oxychlorination pellet has been made. Comparisons have been made with results on experimental activity.
6. Based on an analysis with SIMOXY and a recent report on capacity increasef it may be possible to get as much as 25% increase in capacity in the present system if the catalyst activity can bemaintained at its initial value. Eight small-scale pilot runs have been made on a method to reactivate catalyst in the system. The results are Inconclusive at this time.
7. Some preliminary data on the EDC cracking furnace carbons has been obtained.
8. Analysis of EDC from oxy for butadiene was negative.
9. Mercury has been found repeatedly on the spent catalyst increasing in amount from R303 > R302 > R301. You may want to give attention to this fact as a safety precaution at turnaround.
CCR 000008262
Mr. J. D. Minott July 24, 1970 Page 2
Details of these items and further findings will be contained in our report.
F. J. Radd Senior Research Associate Central Research Division
M. C. Hawley Engineering Consultant Process Engineering Department
FJR-MCH-DEM/NP
Attachment CC: HDB-FK-CVF-LNV-GJF-RHG
D6-PF
Chemical Engineer Petrochemical Division Process Engineering Department
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New Catalyst Range
SCANA PROFILE OF OXY SUITE (April 13, 1970 Shutdown) (Harshaw Catalyst)
R302
Bottom (4)
Top(2)
Bottom (4)
R303
Top (4)
Bottom (4)
2
no 73 1 o o o Q0 O CD f\>
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Middle (1) Top (3)* l
Upper Middle
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Gas Flow In Reactor Suite --> (3)* - This enclosed number corresponds to number of experimental measurements.
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OXYCHLORINATION DEBOTTLENECKING
1. Statement of program accuracy with respect to rate changes. Would like operating conditions at two different rates at full catalyst
activity/-
2. Conversions possible in present system at 150% of rate and with present catalyst loadings. Full catalyst activity.What would be hot spot temperatures and steam drum pressures. Pressure drop limitations in system.
3. Changed catalyst loading patterns for more catalyst. What effect on conversions at 19%?
if Smaller catalyst for larger surface area. Delta P limitations and effect on conversion at high rates.
5. Higher inlet pressure to system for higher reaction rate.
6. Possible fourth reactor in series. What catalyst loadings and air split, etc.
7. Given a defined catalyst deactivation (such as at shutdown April 1970) determine conversion in oxy that is possible with appropriate operating conditions.
8. Possible series and parallel arrangements of three and four reactor systems.
9. Possibility of condensing ethylene and recycling to R-301,
10. Possible oxygen in feed with a diluent such as nitrogen, air or EDC.
11. -Possible splitting of ethylene and HCl to the reactors.
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(CCR 000008265
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~ COliiCENTAL VCM PLANT
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CCR 000008267
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RESEARCH ENGINEER WESTERN RESEARCH CENTER Stauffer Chemical Company
T200 South 47th Street Richmond. Calif. 94804
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CCR 00000826' :;S';:; SIGNED
FILE AND FOLLOW-UP COPY
1-51X3
RETURN THIS COPY TO SENDER
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To- Engineering Department
Date; Fet-ruarj- 11, 1966
Attention oi ; Mr . T:. C. r;clt
'Ftqtt.i A,, 1. deVries
Copy to:
Messrs; L. .4l.7r ,* Hot
A,. IV, Me Suite
0. 11, Robert s
?' u Michels si H, Priedman
R. E , Cbrecht
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H. K., Luntz (W L, 1>,vT ,, Vickery
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Oxychlorma c Lor Reac tor Tubes
We. \ t i. c i-a 1 .3. oj Til ,,-kel tube.: :. or trn Latu Cna: it-. Oxyeh ic-i i r.a t tor . Re,actors R-30-,. R-3C2, R-3C-5 have been set at If gape average wall. Tubes fc: R-3QE
Will be ip gage- average wall. Design pr< scare and
temper si. a; * fo?' R-^Ca* unit is less r hat for others.,
ArnerLa;,k uixmloal tiroes nave seen 10 gag'- everage
well wit.:,
experience of no corridor. Vs had
orlgl nxi i,/ r iermec to go to 1.? gage minimum wall
but farm) ir.rc 11 gage average wall is less expensive
tha::. tb-. 'vs gage minimum wall,
RANGE F'OF A' KFAGE WALL
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l-ft inches . L2S Inches . 109 inches
EEiPMUK . it 1 .108 .OS 8
MAXIMUM .1*7 .132 .12C
W *i na, c furT ,n<: r iianged from annealed to stress relieve- i-jcscei . Corrosion reslstar.ee- nut effected but afcr .Eit: resistance is ennanced tub' v 111 be It ss sol i
A? oer *c c tiT'.TisncJa". to. j of Research - we- ait adding the 1? i out over all tube length In Fieactorr H-301*
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(CCR 000008289
1*2'*
REV. 1.1-53
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to: subject:
INTEROFFICE COMMUNICATION
- Ponca City, Oklahoma March 12, 1971
Mr. Jerry Brown, Westlake, Louisiana R-304 DESIGN LIMITATIONS - VCM PLANT
The design calculations submitted by Nooter, the Solar expansion joint specifications, and Mr. Churn's heat transfer calculations covering Oxy Reactor R-304 were reviewed as you requested.
VCM personnel should be congratulated on the conservatism, soundness of logic, and thoroughness of detail in their analysis of this problem. The Nooter calculations appear to be on the conservative side and indicate clearly that the nickel tubes would be mare than adequate for a 400P metal temperature at the proposed inlet pressure of 52 psi. The Solar specifications indi cate that the expansion joint would be adequate at the higher temperature. Mr. Churn's calculations demonstrate that a maximum temperature of 152 C should be the maximum metal temperature experienced if the highest possible considered hot spot internal temperature of 300C is reached. Since this is well below the design conditions for the tubes, there is no reason to expect any hazardous consequences from the proposed higher temperature operation. I have no reservations in approving the change, especially as it appears that original design conditions of pressure and temperature will not be exceeded.
If I can be of further service to you in this matter, please let me know.
NKE-ch Carbon copies to: LNV-RLH-LT
Norman K. Edwards Director Inspection Division Maintenance Engineering Department
CCR 000008291
1.2.S REV. 1-1* S3
INTEROFFICE COMMUNICATION
March 3, 1971 Westlake, Louisiana
To: SUBJECT:
Oxychlorination File Corrosion of R-304
On March 2, 1971, I telephoned Jene Leterle to ask his opinion on the possible risk of severe corrosion if we increased the operating temperature of the oxychlorination cleanup reactor, R-304, 1 gave him the following information:
1) The reactor is used to chlorinate a nitrogen-rich dilute ethylene stream.
.200
2) The material of construction of the reactor is nickel
3) The reactor presently operates with a hotspot temp erature of 200-220C.
4) The inlet gas is saturated with water and has a dew point of 30-40C at 50-60 psig. This corresponds to approximately 2-4 mole percent water.
5) There is very little HC1 in the reactor feed, but the effluent can contain several thousand ppm.
6) The tube wall temperatures should approach the shell side temperatures (125-135C) rather than the process temperatures.
7) We are not sure how hot we might want to run the reactor, but 300-350C is not outside the realm of possibility.
Jene returned the call today and indicated that he felt there would be no problem at the temperature range mentioned. In fact he said that 350C was by no means the limit. He did caution that the tube metal temperature should be kept at least 30C above the dew point. This is because nickel chloride is hygroscopic and will tend to pick up water as the dew point is approached. I indicated that this would be no problem.
Jene said that he had checked 6 or 7 references and found nothing that would "scare him off". Most of the corrosion rate data that he found indicated rates of about 2 mpy, and even if this data were in error several fold, the corrosion rates would not be excessive. He also indicated that the manner in which the data were obtained would tend to make the results conservative.
RHG-BS cc: LNV-RDG-RLH-JDB-J -RWC-JFL
R.H. Gerlach CCR 000008294
STRAIGHT BILL OF LADING -- SHORT FORM -^)RIG1NAL -- Not Negotiable
RECEIVED, subject to the classifications and tariffs In effect on the date of the Issue of this BUI of Lading*
Carrier's No.
J.H. ROSE TRUCK LIMES
From
At
CONTINENTAL V.C.M. PLANT WESTLAKE, LOUISIAIA 70669
________ (Name of Carrier)
Shipper's
356
6-21-71
19
thq properly deseilhcd br1ow, lr appmcril rood ortcr, e*o*pi as noted fcontents and eomlHIoij of r-witents of packages unknown), marked, consigned, and destined as Indicated below, which said carrier (Ihe word carrier being understood throughout this conlrart is mean
ing any person or corp-wallon In po^sc^sinn ol lle pinroily umlur the contract) aureus lo carry lo its usual pfaca ol <fcihv^ry at said destination. II on Its route, otherwise to rie1i*er lo another carrier on the route to said destination It Is mutually agreed, as to each carrier
of sB or amr ol said property over all or any portion ol iaid rouie lo tfis1m.il ion, and as to each party at any lime interested In ail or ary ol sard piopcrty, lhat every scrvtcc lo be performed hereunder shill bo subject to all the terms and conditions of the tlndcrm Domestic Straight Dill of La time sel loith (1) in Uniform freipM Clnsnf.c,>tian tn ellccl on the date hripcf, if this Is a rat) or a rail-water shlpmonl, or (2> m |ne applies bio motor canler classllicallon or tardf If this is a molor carrier shipment.
Shipper herr-hy certifies il*nt he Is (amitiar wiih all the irrms and corulirrons at lho said bill ol Jadmg, Including those on IM hack, (hereof. Set forth lev the classllicaUoci or ttclH which govern* the IfUKportelJcn ol this shipment. d Ihe said terms and conditions
tre hereby agreed l> hr1 the shipper and acfptcd for lu-mell and l.is as'.irns
______
____ .
. ---------
Consigned to___ WESTERN RESEARCH CENTER, 1200 S. 47th St., ATT: WENDELL KNOSHAUG____________________________
(Mall or street address of consignee--For purposes of notification only.)
/ Destination^ RICHMOND * . CALIFORNIA
____ StateCounfyAddress
Del ivory
{To be filled In only when shipper desires and governing tariffs provide for delivery thereal.I
Route_
RUSH - RUSH - DO NOT DELAY
Delivering Corrier_
No. Packages
tr
CTN
Kind of Package, Description of Articles, Special Marks, and Exception!
SILICA PELLETS
_Cor or Vehicle Initials-
, *Welght fSub. to Correction)
25#-
Class or Rate
Check Column
_No~
Subject to Section 7 of Conditions of applicable bill of lading, If this ship ment is to be delivered to the consignee without recourse on the consignor, the consignor shall sign the following statement:
The carrier shall not make delivery of this shipment without payment of freight and all other lawful charges.
(John Minnott)
{Signature of Consignor.)
If charges are to be prepaid, write stamp here, "To be Piseepnaaltld."
ToBe Prepaid
___________
to apply in the prepayment of the charge! on the property described hereon
Agent or Cashier
/ (Collect On Delivery and remit to
$
C.O.D. Charge j5hippef
to be paid by 1, K 1 [ Consignee Q
(The signature here acknowledges only the amount prepaid.)
Charges advanced:
"Shipper's imprint in lieu of stamp; not a part of bill of lading approved by the Interstate Commerce Commission,"
"if Hit sWpmenl mutes bclween two purls by a carrier by vralsf, the law requires thal Ihe bill of lading shall slale whether 11 Is "carrier's or shipper's Weight." NOTE--When the Mle is dependent on value, shippers are required lo state specifically In writing ihe agreed or declared value el Ihe properly. The agreed or declared value ol ijie properly Is hereby spec I Ik ally slaled by Ihe shipper lo be not exceeding
-Continental- VCM Plant-
P.O. Box 605
Shipper, Per
WestlalceT Louisiana 70669
Jesse K. Copiin
The Fibre Boxes used for this shipment conform
to the specifications set forth in the box marker's
certificate thereon, and oil other requirements of
Consol idated Freight Oassi fication.
ROSE TRUCK LDNES
______ Agent, Per,
------ 7---
Permanent postoffice address of shipper,_________
SNAP-A-PART 4-7-4-13
MAPI IN W. *.ik.
CCR 0 0 0 0 0 8 2 9 5
Copper Catalyst Inventory June 22, 1971
Lot 51* (DO HOT USE -PER DAVE PETERS -NOT STOCK) 37 Dr. /&, /"*?
Lot 52-9 Drums
Lot 55-1 Drum
Lot 56-1 Drum
Lot 57 -37 Drums
Total
48 Drums x 275# 13,200# jjJl'-
Teco-Sil inventory 1150 Bags x 75# - 86,250#
CCR 000008296
(conoco)
Interoffice Communication
to J. R. Holcomb
From D. C. Skokna
Date June 20, 1973
subject
Oxy Reactor Catalyst Charge for Summer 1973
The next recharge of the oxy reactors shall contain the following pattern:
R-301 (from bottom to top)
7" of V Raschig rings--six boxes (2 cubic feet each) 26" of 100% catalyst-10 drums (Lot #129) 26" of 65% catalyst--10 drums blend (7 drums catalyst - Lot No. 131) 26" of 45% catalyst--10 drums blend (5h drums catalyst - Lot No. 131) 40" of 32% catalyst--16 drums blend (6 drums catalyst - Lot No. 138) 19" of silica in tubes--48 bags (75 lbs. each)
2" of silica on top of tubesheet--15 bags (75 lbs./bag)
R-302 (from bottom to top)
7" of V Raschig rings--6 boxes (2 cubic feet each) 52" of 100% catalyst--21 drums catalyst - Lot No. 129 26" of 65% catalyst--10 drums blend (7 drums catalyst - Lot No. 131) 40" of 45% catalyst--16 drums blend (7H drums catalyst - Lot No. 131) 19" of silica in tubes--48 bags (75 lbs. each)
2" of silica on top of tubesheet--!5 bags (75 lbs./bag)
R-303 (from bottom to top)
7" of V Raschig rings--six boxes (2 cubic feet each) 91" of 100% catalyst--37 drums (Lot No. 130) 17" of 90% catalyst--7 drums blend (7 drums catalyst*) 10" of 100% catalyst--4 drums catalyst** (Use, "R-303 Special 100% Blend") 19" of silica in tubes--48 bags (75 lbs. each)
2" of silica on top of tube sheet--!5 bags (75 lbs. each)
* (Use: Lot No. 131, 5 Drums - Lot No. 124, 1 Drum - Lot No. 138, 1 Drum) ** (Use: Lot No. 57, 1 Drum - Lot No. 129, 3 Drums)
CCft 00000Q297
J. R. Holcomb Page 2 June 20, 1973
The blends should be made as follows:
Strenqth
Drums Catalyst Per Batch
32% 1-Use Lot No. 138 45% 1-Use Lot No. 131 65% 1-Use Lot No. 131
Bags Silica Per Batch
11 Bags + 16 Lbs. 7 Bags + 23 Lbs. 3 Bags + 16 Lbs.
Special Blending For R-303
1) 10" - 100% Layer: 3 Batches are required. 1 Batch = 92 Lbs. Lot No. 57+1 Drum Lot No. 129
Note: Mark these as, "R-303 Special 100% Blend."
Total No. Of Batches
6 13 14
2) 17" - 90% Layer: 5 Batches are required. 1 Batch = 55 Lbs. Lot No. 124 + 55 Lbs. Lot No. 138+1 Drum, Lot No. 131 +68 Lbs. Silica.
3) 91" - 100% Layer: Use 37 Drums Lot No. 130.
All drums of blended material should be marked with the catalyst lot number, percent catalyst, date blended, and the reactor for which the catalyst is intended.
D. C. Skokna
is CC: RDG-RHG-GGD-H0A(2)-JDM-JCL
0000082*8 cca
Interoffice Communication
to
Date subject
J. R. Holcomb D. C. Skokna September 20, 1973 Recharge of R-304 Reactor September, 1973
For the recharge of R-304 the following amounts of materials are required:
Houdry spheres - 5250 lbs. - 21 drums (250 lb./drum) Norton V spheres - LA 3032 - 4000 lbs. - 34 drums (120 Norton V spheres - LA 3035 - 2500 lbs. - 21 drums (120
%" Raschig rings, ceramic - 70 cu. ft. - 48 boxes 2" Raschig rings, ceramic - 30 cu. ft. - 15 boxes
lb./drum) lb./drum)
The layers of the reactor will be, from bottom to top:
Bottom Top
- 6" of %" ceramic Raschig rings - 17% boxes 40' of Houdry spheres - 21 drums 28" of Norton V spherical LA-3032 - 34 drums 16" of Norton V spherical LA-3035 - 21 drums
- 6" of %" ceramic Raschig rings - 17% boxes 2" of %" ceramic rings over tube sheet - 13 boxes 2" of 2" ceramic rings over %" rings - 15 boxes
The layers are as follows:
6" - 12 lluid oz. 16" - 32 fluid oz. t 40" - 81 fluid oz. 28" - 57 fluid oz.
The top three layers can be "loose poured" onto the reactor tube sheet without accurate measurements. This reactor contains 1380 nickel tubes of 2.157" I.D. and 8' tube length.
D. C. Skokna
is CC: H0A(2)-RHG-RDG GGD-JDM-JCL-CEG
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CCR 000003299