Document Gm7EBz3mRqpoKo6Qvm77YmRKx
FOR DU PONT USE ONLY
d a t e January 23, 1976
, TEST CONCLUSION NO. TA-C- 75~:i30 *
OFFICIAL PRODUCT NAME___________l-Bromo-2,4,6-triethylbenzene Crude_________
PRODUCT CODE NO. 770-113-020POUNDS PRODUCT ACTUAL 9775
(100%) jb
AREA ______"Ponsol"b u il d in g n a me
Colors _______________________________________
t it l e
Modification of process to utilize carbon tetra
chloride in full drum amounts.____________________________
p r e p a r e d b y -. D. J. Vrencur
pur po se o f t est :
To simplify operating procedures by eliminating the charging
of partial drums of carbon tetrachloride. A laboratory run incorporating
the proposed changes showed no difference in yield or quality.
r esul t s o f t est :
Eight charges were made via the T.A. procedure. Yield {100%
basis, before distillation) averaged 85% of standard'. Reason for 85% is
not known, when new production is scheduled, attention to this will be
given.
r e c o mme n d a t io n s :
Do not adopt the T.A. procedure.
i
DISTRIBUTION: V. G. J. L. R. T.
C. H. T. E. i__P.
Witterholt Files Gilsdorf Lake Lewis MrCloskey ......
/ kiil
D. 0. Miller (2) M. S. Moores D. Putnam (3) V. F. Ringleb R. F. Stalzer ... J0. (3. Laucius
s u pVS
ma n u f a c t u r in g
AUTHORISED BY:
,
JIATE DATE
SUPT. M/NUFACTUKING 7ltt .
DATE
''MARK NOT REQtfi REO ' WHERE AJ* PL1CABLE
MU-1733 (Rev. 3/76)
r./cH.SUPVR.. t c c h ./p l t
NOT' REQUIRED
QUA LI TV CONTROL OR ANALYTICAL*
NOT REQUIRED.
GEN. S'JPT.. MANUFACTURING*
D. J. Vrencur
DATE
MANUFACTURING MANAGER*
NOT REQUIRED.
TECHNICAL DIVISION"
NOT REQUIRED.
PLANT MANAGER*
FOB* COMPANY USE ONLY 4
hat p
TEST AUTHORIZATION NO. TA-C- ... Z5-130_
February 6. 1975 P&Qr^,st
OFFICIAL PRODUCT NAME___________l-Bromo-2,4,6-triethylbenzene..Crude____________
PRODUCT ROnFVNri > 770-113-020POUNDS PRODUCT PROPOSED.... 5800 lbs .
AREA______ ` "Ponsol" BUILDING n a me
Colors
Tj t l e Modification of process to utilize carbon tetra-
PREPARED BY:. Pi
chloride in J; Vrencur
full drum amounts. ___________
RESPONSIBLE FOR TEST AND TEST CONCLUSION:_____ D. ______________________________ A.
_____________
J. Vfencur H. Pagano
PURPOSE OF TEST: .To simplify operating procedures by eliminating the charging of partial'drums of carbon tetrachloride. A laboratory run incorporating the proposed changes showed no difference in yield or quality.
DURATION OF TEST:..; Four charges.
STANDARD INVOLVED:. CWP 770-113--020 dated October 8f 1971.
'. ANALYTICAL1 CONTROL: S No change
Change described under Test Details
TECHNICAL BASIS FOR CHANGE: OCNB 2900-68.
TEST DETAILS:*' '' ' (Include Safety and Waste Disposal)
.. See attached.
SAFETY: Improved by minimizing potential exposure to carbon tetrachloride.
WASTE DISPOSAL:
The amount of carbon tetrachloride is increased from 2020 lbs. per charge to 2100 lbs. per charge.
DISTRIBUTION: R. H. Terss J. L. Files C. H. Lake T,, E. Lewis
.R. .1 McNally
M. S. Moores
JK. F. Laucius
D. 0. Miller (3) / D. J. Vrencur
G. L. Porter '
A. H. Pagano
D. Putnam (3)
R. F. Stalzer
Witterholt.
a., OPERATIONiS
/DATE ' Cl
SUPERINTENDENT, ANALYTICAL (when Baqulrod)
DATE
AUTHORIZED BY: J: V //n
/
A/ /?'
SUPERINTENDENT, MANUFACTURING (Or Delegate)
OATE
Ah . E ra o.'
SUPERINTENDENT, DYE DUALITY CONTROL (When Req'd) DATE
SUPERINTENDENT, TECHNICAL (If Any)
DATE
DUP050467760
N33002.01
Page 2 TA-C-75--130 l-Bromo-2,4,6-triethylbenzene Crude
Test Details;
*
Replace Steps 1 to 5 in the Chambers Works process with the following:
Process Steps and Limits
1. Charge the 500-gallon enamel-lined reaction kettle with 1,450 lbs. of 1,3,5-triethylbenzene (TEB) and 700 lbs. of carbon tetrachloride. Agitate and cool this mixture to 0C.
The vessel must be vented to the' fume-scrubber box.
Carbon tetrachloride is used as a diluent to minimize formation of by-products.
2. Into a measuring tank, charge 700 lbs. of carbon tetrachloride, add 683 lbs. of bromine and mix these materials.
Suck the solvent into the tank and then blow the bromine into it with nitrogen pressure.
3. Run this mixture into the reaction kettle over a 2- to 3-hour period, keeping the temperature of the bromination mass in the reactor at 0-5C.
If fuming starts or if the temperature rises, slow down the addition of the bromine--carbon tetrachloride mixture. Vent fumes through a reflex condenser to minimize solvent loss.
4. When the mixture has been added, prepare a second mix in the measuring tank of 700 lbs. of carbon tetrachloride and 683 lbs. of bromine, as before.
5. Add this mixture to the reaction kettle over a 2- to 3--hour period, keeping the temperature at 0-5C. .
Two mixes are made up because available measuring tanks are too small for one mix. Technically, this is not necessary.
DUP050467761