PHENOL PLANT IN OSWIECIM AND THE PHENOL PROCESS

Document Type: 
Collection: 
Document Number (FOIA) /ESDN (CREST): 
CIA-RDP80-00810A000500430009-0
Release Decision: 
RIPPUB
Original Classification: 
S
Document Page Count: 
4
Document Creation Date: 
December 15, 2016
Document Release Date: 
October 27, 2003
Sequence Number: 
9
Case Number: 
Publication Date: 
March 19, 1953
Content Type: 
REPORT
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PDF icon CIA-RDP80-00810A000500430009-0.pdf424.98 KB
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Approved For Release 2003/1.2/02 : CIA-RDP80-00810A000500430009-0 CLASSIFICATION LJI:CR55 CENTRAL Id A(ENCY INFORMATION REPORT COUNTRY icind SUBJECT Phk...nc PLACE ACQUIRED DATE OF INFO .ant in OsaIeciLi an the Phencl Process 25X1 25X1 REPORT CD NO. 25X1 DATE DISTR. 19 rth No OF PAGES NO. OF ENCLS. SUPPLEMENT TC REPORT NO THIS IS 7.71EVA1LATED 11FORMATIO. 25X1 . The original contract for construction of the phenol plant at Oswiecim, . tformerly I. G. Farben, Auschwitz) was let in August of 1948 but .he first deliveries of building equipment did not arrive until the fell of ,950. The buildings for the phenol plant had not been completed by September 1951. The following companies supplied building materials and equipment for he phenol plant: Corblin of Paris, Schneider-GrusseSU of Paris. and Bergdnr Eisenwerk of Bremen. Skoda of Czechoslovakia supplied some large eompressere for a syn- thetic benzene installation. Skoda also supplied new high pressure boilers to augment existing facilities. The Skoda-supplied compressors were eewly con- structed from old designs. German Krupp compressors were available but were not used since replacement parts for them could not be obtained. :-Ielarce heard that the electrolytic plant previously dismantled and shipped from Aueehwitz by the Soviets was being returned but that the Poles would' have to pay fur iL. The power consumed in the phenol plant came fro:1 a coal power plant in the area of Oswiecim as well as from external sources. The estimated daily consumptien of the phenol plant was 10-12,000 kilowatt-hours. Low temperature coking ovens and an assetiated rectification plant at Oswiecim were being set ue by the Lurgi firm of Frankfurt/Main, Germany. The actual construction of the plant was carried nut by a Polish firm, formerly a part of the chemical works but nov under a sep- arate ministry, thus necessitating a separate contract. The monochlerobenzene and phenol distillation building was of steel girder construction, 20m x 40m x 20m high. An existing building of similar construction, 20m x 50m x 10m high, served for the high pressure installations, laboratories, and offices. A wall 80 cm. thick separated the high pressure units from the laboratories and effices. 2. SGme of the chlorine used in the plant processes came from Bitterfeld and some from Moscice near Krakow since there were no facilities at the Oswiecim factory for the manufacture of electrolytic chlorine and caustic. Because there was a good market for chlorobenzene in Poland, the chlorinator at the plant was run near maximum capacity (about 25 tons per day). The excess of chic-Tr/benzene over that required in the phenol process was sold for use as paint thinner, solvent, and possibly as a softening agent or plasticizer. CLASSIFICATION r [STATE X NAVY .-Ic NSR8 I r DiumBunoN 1,----- I T 1.?"11. fx MR 4( nm b1.r v x I H Approved For Release 2003/12/02 : CIA-RDP80-00810A000500430009-0 25X1 TI 25X1 25X1 Approved For Release 2003/12/02 : CIA-RDP80-00810A000500430009-0 SECRET 25X1 -2- The plant employed about 2000 persons, many of whom were Of German origin. Some of these employees commuted to Work from as far away as forty kilo- eeters. Because of thisonew three story apartment dwellings with twenty- four apartments in eaca for the plant workers had been started Eech apartment had a living room, kitchen., and two bedrooms. 4. In addition to a period' Kcourse of instruction), the tech- 25X1 nical nature of which was subordinated to the political aspects, the workers received two to three hours of political indoctrination each week. A Polish translation of a technical booklet for engineers was issued to each worker ? who in turn had to memorize the entire contents whether or not he unaerstood those contents. In nearby Katowice, a city of 80,000 population, was a ? large library of technical publications translated into the Lussian language. Second-hane German technical books were available bet :ere expensiee. 5. 25X1 contained A detailed descriptioe nf the phenol process.by stacestisi in the following paragraphs '' A. Chlorebenzene Stare benzene from storage was passed through a drier packed with solid caustic (fle1011), thence to a lead-lined chlorinator packed with iron Raschie rings. The actual feed lino entered above the middle of the chlorinator ant' passed through the packed region to a point near the bettom, thus allowing a short pre-eeatsing period for the benzene, The metered chlorine was feci 1.1110 the bottom ef the reactor and controlled to give a 25-30 ';') chlorination, thereby minimizing:the production of di- and higher-chlorinated benzenes Initialie, the chlorinator was heated with process steam to the des. red temperattre and thereafter the exothereic reaction was controlled be-river water coin e or the jacket. The chlorination mixture was sent to a steipeine column In which a benzene cut (800C) was separated free the monochlorobenzene (11CB)-aee recycled to the chlorinator. with sufficient benzene for process make-era Frau the stripper, the crude monochlorobenzene plstilline at 132?C, wastransferreC to a rectifying colemn where it was eurified and then sent to storage, The tottoms were being discarded in Ceteeer 1952. iiore than the required ampunt of uenochlorobenzene needed .for the phenol process was being peoduced becaese of the ready market for it in Iolande The capacite ef tee wonecelorobenzene snit could easily be steppedup by chlorinating to a higher degree but in so seine a larger cut of higher chlorobenzenes would be obtained, llyerecaloeic .acid resulting from the reaction was piped to an absorber where it was reeleeeee as aqueous acid for use later in the process. This absorber was a vertical Pyrex column kedwith graphite and employing concurrent flow. The hydro- chloric acid! stripped from the benzene chlorinator with the aid of 600 refrig- eratien at the column head. ? Bcadifficulties had arisen concerning corrosion because the process at this stage was anhydrous tantalum eqdipment does not exist in Poland nor is it readily available in the rest of Europe. B. Monochlorobenzene Conversion to Phenel Stage. 25X1 ? In this stage,hW caustic was diluted to 20,- strength using process con- densate in a power-agieated mixing vessel to which was added l0 diphenyl ether to suppress the side reaction by which diphenyl ether is foreed, In a molar ratio of two sedium hzdroxide to one monochlorobenzene, the compenents were fed to the hieh pressure reactors thrnugh a high pressure propoettenine ucmr,T Approved For Release 2003/12/02 : CIA-RDP80-00810A000500430009-0 Approved For Release 2003/12/02 : CIA-RDP80-00810A000500430009-0 SFCRET 25X1 -3- pump- The feed rate ef this pump was controlled b,, the speed of the drive motor while one of tee piaten strokes could be varied during operation.-- This variable stroke pistoe contrelled the feed rate of the monochlorobenzene. .The mixed feed at 300 atmospheres pressure next passed through a high peessure heat exchanger heated be the countercurrent flow of the completed reaction mixture, The ?three high pressure reactors were well laeeed and collie the first tuo were electrically heated to about 4000 C, the third befele a holcer to afford sufficient time to complete the reaction. . After initial cooling in the high ? pressure- heat exchanger, the mixture consisting of sodium phenolate. eiphenel etherr, salt, and water with a spell amount of un-reacted monoch:lorobenzene eas further coeled to below 100 C before it was admittea to the eeleaeseen valee. This pressure reducer was of the homogenizer tepe with a rotating cone impingere Tesemieture aext went to a combination condenser-separater wetere the olphenel ether supplied to and formed in tee reaction was decanted contieucust and sent Le storage, The excess dipeenel ether was being sold for use as a 'cleat transfer medlsm in eeraed. The paenolate 'Liquor was then conducted to the eeuiralizer, ;eetraIiesetion of the Fhenolate Liqeor. Tse liqeor eroe the previous stage plus the aqueous kdetchloric acie obtained frem the abeerber were fed to a veseel eaaipped vith a poeered ngitaeet to free the phenol from its sodlum salt- The reselting liquor separatee Mite see els-- tinct phases which were then withdrawn with the aid of a sight Jess an. valves to eheir respective storage containers. The phenolated. bridle was in the lower phase while the aqueous phenol was in the upper phase,- - D. Phenol Purification,. Tee phenol liquor was transferred to .s. stripping column in uhice. tee peenol was separated from any residual monochlorobenzene and eater 'enrollee the use - ,\C a 92?C ternary. azeotrope composed ef phenel-water-monochlorobeeeene. This aseetrope wac condensed and separated_ Tte .pper pbese as retereee ke process coeeensate for re-use and tee lowe phase as retureed to a sir:table point on tee column The. phenol component was sriteeeavn from the stell-pot are. sipeet se a- rectifeing column where ie was distilled at atmospheric presseee? The final preeect had the following characteristics (1e2? C fraction) Recuired,......_freezine point 39_6 - YeLOCC Actual,? .,, .freeziee point e0,4 40,541/ (eolorless, soluble in eatee without turbiaity The bottoms were being discarded- nhenolated Brine Treatment, Tee brine, containine about 2 e phenol, eau sent to a strpping came neeo a elnary water-phenol azeotrope containing 11 e phenol was chLaleedvueisn oe con-ensation separated into two phases. The lighter phase consisted ),L. aqseous phenol uhile tee lover phase consisted of about 50 e phenel.. The 6 Illuor was returned to process condensate for re-use and the 50 e phase was combined with tee raw phenol feed to the phenol stripping column. Be this process of receeling, the phenol losses from the process were held to an abselute minimum. The stripped brine, although being discarded, will eltimatel: be eencentrated in double effect evaporators after passing through regenerative active earben purifiers. The resulting concentrated brine will suppie the electrolytic cells with which it is intended to produce the necessare Caustic. and chlorine for the entire process. In October 1952, however, no facility exlsted in the plant for producing electrolytic Caustic. requirement s hal to be felfieled frau the electreletic caustic plant at niosciee eiscelianeous Notes en Lluipment and Precesaing. .hen she 301iC caustic drier was exhausted, the spent caustic' was made up Le tee required 6Oe coneeetration and eeld n storage ree the hydrelesis seep. Approved For Release 2003/12/02 : CIA-RDP80-00810A000500430009-0 25X1 Approved For Release 20657M112 : CIA-RDP80-00810A OAP MO430009-0 The iron for the iron-catalyzed chlorinatien was furnished by the iren Vaschig ring packing. Heat for the chlorinator and the two monoehlorobenzene columns was supplied from process steam at &abut 225 psi. The Pyrex for the hydrochloric acid absorber was obtained from Taigland The phenol purification columns and the brine stripper were all heated by the use of cireulateg hot water held under suitable preseure to obtain temperatures of 200 - 250 C. this was an innovation. of the Krebs Company and that no particular difficulties had been experienced in its use, The feed for the system was made up by use ef process steam condeeeate which was consievred to be economical and safe and to have desirable heat transfer charaeteristies. The activated carbon absorbers were reactivated with steam as needed Two units ware available in each line. The prepertioniig pump was obtained from the Corblin Company, Paris. It was a three piston ueit giving the desired pressure and proportioning aimultaneously The speed varied from 6o - lee rpm with only the monoehlerobenzene piston having thf variable etcee The pressure release by means ef a blow-out disc was set fir 140 atmeeeheres The pressure reducer was obtained from Bergdorfer Eiseewerk, Bremen, A long range objective was to obtain free phenol in the hydrcl.sis step through the use of higher temperatures and less caustie. No progress had been made on this point by October 1952. The total plant capacity was designed for 3oa metric tons eer month, allowing five days each month for maintenance and repeir. The instahlation consisted of two complete waits in parallel, only one ef which was in eperatieh (half the rated output by October 1952) pending treinieg of suitabe opeeators to 25X1 handl* both units simultaneously. I Ithe scvel of competence of the available operators wan so low that damage to the plant through mis- handling, especially in the high pressure inetallations could be expected. The ultimate use of the phenel was fer phenol-fortaldehyde type resits and synthetic fibers. A small amount of it ves to be used for medicel purlaee because of its high pueity. .Someeshipments uf phenol, consigned to the Warsaw area, were noted, Three Krebs employeee still supervised eroduction and the training of personnel for the phenol unit in October 1952 The avvolopment of synthetic fibers in Poland vus said to be far behind that of other countries. Plans had been purchased frem the Soviets for vethanole acetaldehyde and acetic acid plants, the equipment for which was to et menu,. facture(' in Poland- Certain techniques available in Poland were said net to blesupeto the demands and specifications of the chemical industry. For example, 25X1 It copper lining on the eressure vessels in another part of the plant blistered considerably and even peeeed away from the base metal. Bearings in Pelish-built compressors gave part:cular difficulty sine* no aronzes were to be had, only white metals and.babbits. flow, 25X1 ever, good .lubricating oils were available ,I 'the data on the esearigerating-unit lubricants as beiag a turbine oil #3 with high eiscosity at low temperature, 5?. Engler value at 50?C and 14? Engler value at room tem- perature, and a 28PC freezing point. 25X1 001IpiEN'T : Although the production of phenol as described in this report is conven- tional in most respects, the process has been reported in detail because several novel features were noted SECRET Approved For Release 2003/12/02 : CIA-RDP80-00810A000500430009-0