Document N1LMG5R4Z6Y46JE5yZrj0yQQ
W. K. Kessler April, 1974
Chambers Works 234-448 300
I-1-1
"LITHOSOL" ACID RBA {4-Aminotoluene-3-sulfonic Acid Purified)
Principle
4-Aminotoluene-3-sulfonic acid crude is dissolved in water as the sodium salt by the addition of spda caustic liquid. Darco and Super Cel are added to adsorb the colored impurities and to aid filtration. The solution is heated to 95C, filtered, and the filtrate acidified witli sulfuric acid to precipitate 4-amino-toluene-3-sulfonic acid as the free acid. After cooling, the 4-aminotoluene-3-sulfinic acid is isolated in a nutsch, dried and ground for sale as "Lithosol" Acid RBA.
Reaction
The only chemical reaction involved.is the conversion of the acid to the soluble sodium salt and, after clarification, the reconversion to the free acid by the addition of sulfuric acid. The product structure is:
CH3
NI12
4-Axninotoluene-3-sulfonic acid ("Lithosol" Acid RBA) M.W. 187.2
OPERATI NG INSTRUCTIONS
W* K. Kessler April, 197 4
Chambers Works 234-448 300 III-l
4-AMIN0T0LUENE-3--SULFONIC ACID PURIFIED
"LITHOSOL" ACID RBA
SUBJECT:
:_______________________________________________ OPERATION:
Equipment
K--2 F-l TS-15
T-l T-2 P-27
TS-18 P-54 P-45
N--1 N-2
GB-3 ML--1
Bill of Materials {100% Basis)
Materials and Orchem Product Code Numbers
Lb./ Chg.
4-Aminotoluene-3sulfonic acid crude
049 335 Caustic Soda Liquid 30%
877 500 Sulfuric Acid
945 000 Darco S-51
190 000 Super Cel
946 200
2,600
535.5
665 100
50
Product
4-Aminotoluene-3sulfonic acid purified
049 340
or "Lithosol" Acid RBA 448 300
2,400
Reference:
Chambers Works Process for the Manufacture of "Lithosol1' Acid RBA, dated July 28, 1969.
Batch Size and Yield
The Bill of Materials is written for a standard 2,400-lb. charge in a 2,800-gal. solution kettle. The charge size may be varied proportionately within the working limits of the available equipment.
No goal yield has been established.
DUP050467890
N33036.01
OPERATING INSTRUCTIONS
W,, K. Kessler April, 1974
4-AMINOTOLUENE-3-SULFONIC ACID PURIFIED
SUBJECT: "LITIIOSOL" ACID RBA
OPERATION:.
Chambers Works
234-448 300 rn-2
Hazards
Sulfuric acid is a highly corrosive, dangerous liquid. It generates heat on dilution with water. The weak acid attacks most metals with the liberation of flammable hydrogen. The acid attacks and destroys skin tissue. Wear rubber gloves and face shield when handling this material as the piinimum protection. "Ohera Sutis" should be worn where splashes or leaks are possible. If splashed, wash off with copious amounts of water and report to the hospital.
Soda caustic liquid is extremely corrosive in contact with all body tissue, whether a3 liquid or vapor, and even in dilute solutions. It is nonflammable, but generates heat when'mixed with acids or water. If splashed, wash off with copious amounts of water and report to the hospital.
"Lithosol" Acid RBA (4-Arninotoluene-3-sulfonic acid) is an aromatic amine compound which may be hazardous. Avoidcontact with this material. Wear respirator for dust exposure.
Waste Disposal
The sludge from the clarification press is sent to the dump. The final filtrate is a dilute solution containing sodium sulfate and traces of 4-aminotoluene-3-sulfonic acid. This waste is run to the plant ditch.
Cycle Time
The cycle time from beginning of charging in K-2 to shoveling off the nutsch is 24 hours.
Drying time is 24 hours. Milling time is 8 hours.
HU *2
DUP050467891
OPE RATI NO INSTRUCTIONS
W. K. Kessler April, 197 4
4-AMINOTOLUENE-3-SULFONIC "LITIIOSOL" ACID RBA SUBJECT:
ACID PURIFIED OPERATION:
Chambers Works 234-448 300 III-3
Equipment Flow Sheet
X><TCK'
DUP050467892
( OPERATING INSTRUCTIONS
W. K. Kessler April, 197 4
Chambers Works
234--448 300 II1-4
4-AMINOTOLUENE-3-SULFOHIC ACID PURIFIED
"LITIIOSOL" ACID RBA SUBJECT:.
OPERATION:
1. Charge. K-2 kettle with 60 inches of water. Turn agitation on.
Measure dip on straight side of kettle.
2. Add 166 gallons of Caustic soda to K-2 through meter. (533.5 lbs. 100%).
WEAR RUBBER GLOVES AND FACE SHIELD. CAUSTTC SODA IS CORROSIVE AND WILL CAUSE SEVERE BURNS ON THE SKIN. WASH ANY FROM HANDS WITH WATER. REPORT TO MEDICAL DEPT.
3. Start heating K-2 to 90-95C. and turn on agitator. Charge in about 2400 lbs. of 4-Arainotoluene-3-Sulfonic Acid Crude.
Agitation must be on. 200 lbs. of crude is held out to adjust to test. Use gloves, if dusty use respirator.
4. Check alkalinity on Brilliant Yellow papers.
Test must be orange, not red color.
5. Adjust K-2 with balance of crude (200 lbs. held out) and with caustic soda as needed.
Use 2600 lbs. crude total. Final alkalinity on Brilliant Yellow Paper must be a light orange, not red. Add crude if test is red. Add caustic if test is yellow.
6. Add 100 lbs. Darco.
Add slowly--sprinkle. Otherwise foam-over may occur.
.7 Add more water to K-2 to bring volume up to 80 inches total.
Measure on straight side of K-2. Stop agitator before measur in
8. Heat to 95C. and hold 1/2 hour.
9.. Test for color by filtering a sample. The filtrate should not be darker than a light amber color.
Add 50 lbs. more Darco and repeat test if too dark. Check supervision if color remains dark after addition.
h u u< *
DUP050467893
OPERATING INSTRUCTIONS
W. K. Kessler April, 197
Chambers Works 234-448 300 III-5
4 -AMIWOTOLUENE - 3 - S ULFONIC ACID PURIFIED "LITHOSOL" ACID RBA SUBJECT:
10. Steam press and lines to be sure they are clear and hot.
Lines and press must l*e hot or plugging will develop.
11.
Start pump P-54 and circulate solution to F-l press dressed
with cotton duck and back to 1C-2 until all spigots turn
clean and clear.
<
All Darco must be removed; otherwise quality will be impaired.
12. Switch lines to run filtrate to T-l & T-2 dividing the charge evenly.
Both tubs will hold the charge from K-2
13. When K-2 is empty, wash press with hot water back to K-2.
Fill K-2 cone
14. Blow press dry to K-2 and dump to cans. Lable cans "Darco Sludge from Lithosol Acid RBA".
It is sometimes necessary to rework Darco sludge to avoid yield loss if the press does not wash properly. Supervision will advise if this is necessary.
15. Turn on agitation. Heat T-l & T-2 with coil steam to 95C.
Be sure agitation is on
16.
Shut steam off tub coils and start slow addition of sulfuric acid to both tf-l & T-2. Acid is added until both tubs are definitely acid (blue) on Congo Red paper.
The acid addition should take about one hour. (Stream the size of a pencil.) Be sure steam is off coils or tubs tend to boil over. Temperature must be at 95C. during addition. Shut acid off either tub should it become acid before the other. Do not add an unnecessary excess of acid.
WEAR RUBBER GLOVES AND FACE SHIELD.
DUP050467894
OPERATING INSTRUCTIONS
W. K. Kessler Aprilf 197
Chambers Works 234-448 300 III-6
4-AMINOTOLUENE-3-SULFONIC ACID PURIFIED "LITHOSOL" ACID KBA SUBJECT:OPERATION:
17. Cool charge to 25-30C and test for complete precipitation.
Additional sulfuric acid added to a sample of filtrni; should show no precipitate.
18. Drop charge to either N-l or N-2. Bo til tubs go on 1 nutsch,
l'J, Rinse out tubs to nutsch.
Avoid using a large quantity of water. 20. Put 2 spray washes on the cake on the nutsch and suck dry.
Spray 2 to 3 minutes per wash.
21. Transfer to clean cans.
Label "4-Aminotoluene-3~Sulfonic Acid Purified Wet".
22. Dry in GB-3 at 100 + 5C.
One charge will usually be dried at a time. Follow instructions for graining bowl operation.
23. Dump dry product to leverpaks and allow to cool for milling.
Use a respirator and gloves. Dump at 0.5% water or less. Dryer is usually dry in morning after loading on day shift.
24. Grind on ML-1. Pack product at 225 lbs. net.
Sample each charge for: % Purity at lab. One sample for file. Follow separate instructions for milllnr.
25. "Label: "Lithosol" Acid RDA.
10 to 12 packs per charge.
26. Containers must be wiped clean before shipping.
*
MU *'
DUP050467895
OPERATING
W. K. Kessler April, 1974
INSTRUCTIONS
Chambers Works 234-448 300 III-7
4-AMINOTOLUENE-3-SULFONIC ACID PURIFIED
SUBJECT: "LITHOSOL'_' .ACID RRA
OPERATION: _
ANALYTICAL REPORTar ea rnsT rnra: 1351 pRonurr ronp SFMT RY. DATE:
ANALYZE FOR
INTERMEDIATESbl d g . P M A SAMPLE OP
A. M. P. M.
j
LITHOSOL ACID R B A<
TECH. NO.
RESULTS
PURITY
SCREEN TEST 40 MESH 60 MESH
CHARGE NO.
LAB ONLY
--
MU-156*6 MU S39I NS
t.r:/ A<.J sA 1 HAZARDS
No.
if............
LOT
CHARGE
OUILDIHCK
..
DATS ADDN'L, INTO.
ABM
iX TIMS
UQVtPMKNT
...../....
TAKEN BY
'W
COMOSIVQ
O
rtJLMMXtfUS
D
MU>7JA'ftI
no ; unusual HMa r d
o
DUP050467896
OPERATING INSTRUCTIONS
Contains:__ o/i*?yte >3
fn- 6cv*i
From:.
Shipped By
HAZARDS:
Corrosive
Cyanotic yf
Flammable t}
Toxic
n
Wo-Unusual j$v-
N>V7aVH:"'
/****'. ^ct<f
Other Hazard (Describe)
DUP050467897
gPtHATIINU INSTRUCTIONS
W. K. Kessler
Chambers Works
April, 1973
234-448 300 III-^f
4-AMINOTOLUENE-3-SULFONIC ACID PURIFIED
"LITHOSOL" ACID RBA SUBJECT:--------------------------------------------------------------------- ___OPERATION:____________________________________
(
-v / )
"These Operating Instructions have been issued after a full review of current technology and building experience as of
(date), and conform with the current process technology as recorded." (signed)j|^yi|^,jfcLaJ^fc<^(Supervisorts signature).
Building Supervisor. Senior Supervisor.
D ate /- /7~ 7 y' _Date_ /Szo/? V
Chief Supervisor, Operations
/ A' U Jc_
i /y/Date ,/?
Chief Supervisor, Tech, or Plant Assist.
: 1/ Date
' 'V i`
/ehb # 2604
DUP050467898