PHENOL PLANT IN OSWIECIM AND THE PHENOL PROCESS

• Document Type: CREST
• Collection: General CIA Records
• 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
• Publication Date: March 19, 1953
• Content Type: REPORT

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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
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REPORT
CD NO.
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DATE DISTR. 19 rth
No OF PAGES
NO. OF ENCLS.
SUPPLEMENT TC
REPORT NO
THIS IS 7.71EVA1LATED 11FORMATIO.
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. 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.
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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.
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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.
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? 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
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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.
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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,
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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.
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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
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