Sign In to Follow Application
View All Documents & Correspondence

An Improved Process For Preparing Fatty Acid Derivatives And Oleo Chemicals

Abstract: An improved process for the preparation of fatty acid derivatives and oleo chemicals comprising reacting stearates such as glycerol tristreate, stearic acid with glycerine in a reactor at a temperature of 80°C-160°C while stirring the both components and slowly adding caustic soda and visinol palmitic acid to obtain glycerol mono stearate and the mass is melted with mixed ethyl alcohol to obtain ethylene glycol mono stearat and ethylene glycol di stearate, reacting stearyl alcohol/ ceto stearyl alcohol and stearic acid at a temperature of 100°C- 160°C while stirring both components and slowly adding visinol palmitic acid and caustic soda NaOH to obtain stearyl stearate/ceto stearyl stearate, reacting penta erythritol and stearic acid at a temperature of 200°C-260°C while stirring both components and slowly adding visinol palmitic acid and caustic soda NaOH to obtain penta distearate/penta tetrastearate,

Get Free WhatsApp Updates!
Notices, Deadlines & Correspondence

Patent Information

Application #
Filing Date
01 September 2009
Publication Number
41/2012
Publication Type
INA
Invention Field
CHEMICAL
Status
Email
Parent Application

Applicants

ACMECHEM LIMITED
9A, SAKET APARTMENT, 2, HO CHI MINH SARANI, KOLKATA 700 071, WEST BENGAL, INDIA

Inventors

1. NARAIN HOLANI
9A, SAKET APARTMENT, 2, HO CHI MINH SARANI, KOLKATA 700 071, WEST BENGAL, INDIA

Specification

The present invention relates to an improved process for preparing fatty
acid derivatives and oleo chemicals such as glycerol stearates, glycerol mono
stearate (powder), glycerol mono stearate (flakes), glycerol mono stearate
(NSE), ethylene glycol mono stearate, ethylene glycol di stearate, stearyl
stearate, ceto stearyl stearate, penta di stearate, penta tetra stearate, zinc stearate
oleate, di stearyl phthalate, di ceto stearyl phthalate, penta adipate stearate,
mixed ester of penta adipate stearate and glycerol mono stearate, sorbitan mono
stearate, cetyl palmitate, amide ester, mixed ester of fatty acid, mixed ester of
penta adipate stearate, sorbitan mono palmitate, ethyl bis stearamide, ethy bis
oleamide and/or blends thereof.
Fatty acid derivatives and oleo chemcials are used as food emulsifiers,
food preservatives, food emulsifier blends, lubricants for PVC, lubricants for
plastics, viscosity depressants for PVC plastisols, processing aids for polymers,
antistating agents, rubber processing aids, auxiliary chemicals for cosmetics and
pharmaceuticals.
In the known art preparation fatty acid derivatives and oleo chemicals are
already known. However, the same has the following disadvantages:-
1. They emit bad odour;
2. They are expensive to make;
3. They are not eco-friendly and therefore erecting plant for their
manufacture is discouraged by Government and to obtain permission for their
manufacture from different departments of Government is very difficult.
The object of the present invention is to develop the process and to
overcome the disadvantages of the known art and it is simple in nature, more
economical and less hazardous.
These and other objects of the present invention have been achieved by
the process of the present invention
According to the present invention there is provided an improved process
for the preparation of fatty acid derivatives and oleo chemicals comprising
reacting stearates such as glycerol tristreate, stearic acid with glycerine in
a reactor at a temperature of 80°C-160°C while stirring the both components and
slowly adding caustic soda and visinol palmitic acid to obtain glycerol mono
stearate and the mass is melted with mixed ethyl alcohol to obtain ethylene
glycol mono stearat and ethylene glycol di stearate; or
reacting stearyl alcohol/ ceto stearyl alcohol and stearic acid at a
temperature of 100°C-160°C while stirring both components and slowly adding
visinol palmitic acid and caustic soda NaOH to obtain stearyl stearate/ceto
stearyl stearate; or
reacting penta erythritol and stearic acid at a temperature of 200°C-260°C
while stirring both components and slowly adding visinol palmitic acid and
caustic soda NaOH to obtain penta distearate/penta tetrastearate; or
reacting stearyl alcohol/ceto stearyl alcohol and lauryl alcohol at a
temperature 100°C-200°C while stirring both components and slowly adding
phthalic anhydride in presence of Tego 233 and Finanox-8 to obtain di stearyl
phthalate/di ceto stearyl phthalate; or
reacting stearic acid and mixed ethyl acetate at a temperature 150°C-
200°C while stirring both components and slowly adding visinol palmitic acid
and sodium borohydride to obtain amide ester/mixed ester of fatty acids; or
heating stearic acid/palmitic acid and sodium borohydride at a temperatue
200°C-300°C and stirring with sorbitol, hydrogen peroxide, caustic soda NaOH,
antifoam to cooling down at a temperature 100°C and finally bleach the product
with sodium chlorite to obtain sorbitan mono stearate/sorbitan mono palmitate;
or
heating stearic acid/oleic acid with sodium boro hydride, antifoam,
Finanox-8 and then adding ethyl diacetate keeping the temperatue 150°C-200°C
and finally adding visinol palmitic acid, BHT, TNPP to obtain ethylene bis
stearmide/ethylene bis oleamide.
The reaction is preferably carried under vacuum which should be 700 to
760 mm (minimum) and temperature of the process is carried out at around
100°C to 200°C for atleast 4 hours under vacuum.
The object of the present invention is in the above mentioned process the
acid value should be below 3.0.
Further object of the present invention is if desired, vicinonl palmitic
acid, mixed ethyl glycol, Finanox-8, ceto stearyl alcohol Tego 233, sorbitol is
added to the reaction product while stirring.
Yet another object of the present invention penta erythritol is added to the
reactants for 5-6 hours and sodium borohydride is added to the reactants and
heated to the temperatue of 150°C and then treated with lime and amide ester.
The obtained product is powdered in a mesh size of 18 to 25 and
thereafter same is subjected to step of purification by known method.
We shall now describe the process for the preparation of fatty acid
derivatives and oleo chemicals with reference to accompanying examples which
are given by way of illustrations but does not restrict the scope of present
invention:-
Example 1
Process for preparation of Glycerol mono stearate
RAW MATERIALS QUANTITY
1. Glycerol tri stearate 2100 Kgs -2300 Kgs
2. Glycerine 390-425 Kgs
3. Caustic Soda NaoH 15 Kgs -20 Kgs
MANUFACTURING PROCESS:-
1. Add Glycerol tri stearate into the reactor, then add glycerine
2. Close the reactor and star heating. Raise temperature to 100°C-140°C. Start the
Stirrer and mix well for 10 minutes. Add Caustic Soda NaoH slowly.
3. Close the reactor and apply Vacuum. Vacuum should be 750 mm minimum.
4. Raise temperature to 200°C and maintain for 4 hour under Vacuum.
5. After maintenance is over, break the vacuum, open the reactor and check for
clarity. Check acid value (below 3.0 ).
6. Powder the Material.
7. Clean the reactor after every batch.
Example 2
Process for preparation of Glycerol mono stearate
RAW MATERIALS QUANTITY
1. Glycerol tri stearate 2100 Kgs -2300 Kgs
2. Glycerine 390-425 Kgs
3. Caustic Soda NaoH 15 Kgs -20 Kgs
MANUFACTURING PROCESS:-
1. Add Glycerol tri stearate into the reactor, then add Glycerine
2. Star heating the mass & raise the temperature to 110°C-150°C.
3. Start the Stirrer and mix well for 60 minutes.
4. Add Caustic Soda NaoH slowly.
5. Apply Vacuum & raise temperature to 200°C -250°C . Maintenan for 4 hour. Vacuum
should be 750 mm minimum.
6. Close the heating valve & check clarity & also acid value.( Acid value should be
below 3.0)
7. Start flaking.
Example 3
Process for preparation of Glycerol mono stearate
RAW MATERIALS QUANTITY
1. Stearic Acid 1800 Kgs -2000 Kgs
2. Glycerine 630-700 Kgs
3. Visinol Palmitic acid 2.6 Kgs -4kgs
4. Caustic Soda NaoH 0.6 KG -1.5 Kgs
MANUFACTURING PROCESS:-
1. Add Stearic Acid into the reactor, & then add Glycerine
2. Star heating the mass to 150°C Start Stirrer. Mix well for 50-60 minutes.
3. Add Visinol Palmitic acid while Stirring.
4. Close the reactor. Open the steam line & raise the Temperature slowly to 250°C ±
5°C.
5. Allow steam to go out for two hrs. Then apply vacuum 750 mm minimum for 3-5 hrs.
Maintaining temperature at 250°C ± 5°C.
6. NOTE: Close Acid value (Acid value should be below 1.0) If Acid Value is more ,
continue the reaction under vacuum till A.V. is below 1.0.
7. Break the vacuum and add Caustic Soda NaoH solution (1:1) slowly to kill the
Catalyst. Settle the material for 4 hr. & remove the excess L-210
8. Powder the Material.
Example 4
Process for preparation of Ethylene glycol mono stearate
RAW MATERIALS QUANTITY
1. Stearic acid 2000 Kgs -2500 Kgs
2. Mixed ethyl glycol 450 Kgs -500 Kgs
3. Visinol Palmitic acid 9 Kgs -15 kgs
4. Caustic soda NaOH 1.5 KG -3.0 Kgs
MANUFACTURING PROCESS:-
1. Add Stearic acid & Mixed ethyl glycol in the reactor. Melt the mass & start Stirrer.
2. Add Visinol Palmitic acid under Stirring.
3. Raise the temperature to 250°C ± 15°C and allow steam to go out for 4-5 hrs..
4. Close the reactor. Apply vacuum should be minimum 750 mm.
5. Maintain the mass under vacuum for 16 hours.
6. Check Acid Value. Acid value should be less than 1.0.If Acid Value is greater than
3.0, continue till Acid value is below 1.0.
7. Add Caustic soda NaOH solutions (1:1) slowly to kill Visinol Palmitic acid
8. Powder the Material.
Example 5
Process for preparation of Ethylene Glycol di stearate
RAW MATERIALS QUANTITY
1. Stearic acid 2500 Kgs
2. Mixed ethyl glycol 400 Kgs
3. Viscinol palmitic acid 10 Kgs
4. Caustic soda NaOH 3.0 Kgs
MANUFACTURING PROCESS:-
1. Add Stearic acid & Mixed ethyl glycol in the reactor. Melt the mass & start Stirrer.
2. Add Viscinol palmitic acid under Stirring. Allow steam to go out.
3. Close the reactor & raise temperature to 250°C ± 5°C. Apply vacuum. Vacuum should
be minimum 750 mm.
4. Close the reactor. Apply vacuum should be minimum 750 mm.
5. Maintain the mass under vacuum for 16 hours.
6. Check Acid Value. Acid value should be less than l.O.If Acid Value is greater than
3.0, continue till Acid value is below 1.0.Add Caustic soda NaOH Solution (1:1)
slowly to kill T-311.
7. Add Caustic soda NaOH solutions (1:1) slowly to kill T-311
8. Powder the Material.
Example 6
Process for preparation of Stearyl stearate
RAW MATERIALS QUANTITY
1. Stearic acid 1200 Kgs
2. Stearyl alcohol 1200 Kgs
3. Viscinol Palmitic acid 20 Kgs
4. Caustic soda NaoH 3.5 Kgs
5. Finanox-8 2.0 Kgs
MANUFACTURING PROCESS:-
1. Add Stearyl alcohol & Stearic acid in the reactor. Heat the mass & to 150°C melt &
start Stirrer.
2. Add Viscinol Palmitic acid under Stirring. Mix well.
3. Close the reactor. Raise temperature to 250°C. Allow steam to go put for 4 hrs. Apply
vacuum. (Vacuum should be minimum 700 mm) & maintain the mass at 250°C for 16
hrs.
4. Check Acid Value. Acid value should be below lO.O.If Acid Value is more thanlO.O,
continue till Acid value is below 10.0.Again check Acid Value.
5. Add Caustic soda NaoH and stir for 60minutes
6. Powder the Material.
Example 7
Process for preparation of cetyl palmitate
RAW MATERIALS QUANTITY
1. cetyl alcohol 400 Kgs
2. Palmitic acid 35 Kgs
3. visinol palmitic acid 5 Kgs
4. Caustic soda NaoH 1.0 Kgs
5. Finanox-8 2.0 Kgs
MANUFACTURING PROCESS:-
1. Add cetyl alcohol & Palmitic acid into the reactor & raise temperature to 150°C. start
the Stirrer.
2. Add Visinol palmitic acid & mix for 60 Minutes.
3. Raise temperature to 250°C. Allow steam to go out for 8 hrs.
4. Apply vacuum for 16 hours. Vacuum should be minimum 750 mm.
5. Acid value should be below 10.0.If not continue till Acid Value is below 10.0. co
6. Add Caustic soda NaoH at 250°C and run the batch for 60 minutes.
7. Powder the Material.
Example 8
Process for preparation of Ceto stearyl stearate
RAW MATERIALS QUANTITY
1. Stearic acid 1200 Kgs
2. Ceto stearyl alcohol 1000 Kgs
3. Visinol palmitic acid 15 Kgs
4. caustic soda NaOH 5.0 Kgs
MANUFACTURING PROCESS:-
1. Add Stearic acid & Ceto stearyl alcohol into the reactor & raise The temperature to
150°C. start the Stirrer.
2. Add Visinol palmitic acid & mix for 60 Minutes.
3. Raise temperature to 250°C & Allow steam to go out through vent line. Run the batch
for 6 hrs. Determine acid value it should be 10.0 If not continue without vacuum till
A.V. is below 10.0.
4. Apply vacuum for 8 hours. At 250°C ± 5°C ( Vacuum should be minimum 750 mm).
5. Determine acid value it should be below 10.0. Otherwise continue till A.V. is below
10.0.
6. Add caustic soda NaOH and run the batch for 60 minutes.
7. Powder the Material.
Example 9
Process for preparation of penta di stearate
RAW MATERIALS QUANTITY
1. Stearic acid 2000 Kgs
2. Penta erythritol 600 Kgs
3. Visinol Palmitic acid 16 Kgs
4. Caustic soda NaOH 5.0 Kgs
MANUFACTURING PROCESS:-
1. Add Stearic acid into the reactor. Raise temperature to 250°C.
2. Star Adding Penta erythritol slowly into the reactor. Total time for addition 6 hrs.
3. After all the Penta erythritol is added run the batch for 8 hour.
4. Add Visinol Palmitic acid 5 Kgs. Allow steam to go out. Run for 60 minitueas.
5. Again add Visinol Palmitic acid 5 Kgs. Allow all steam to go out.
6. Again add Visinol Palmitic acid 5Kgs.Allow all steam to go out.Temp. 250°C for 8
hrs. Determine A V.
7. Apply Vacuum for 4-5 hrs. Vacuum should be minimum 750 mm. Determine acid
value. It should be below 10.0 .If not continue acid value is below 10.0
8. Kill the Visinol Palmitic acid by adding Caustic soda NaOH at 190°C ± 5°C
9. Power the material.
Example 10
Process for preparation of penta tetra stearate
RAW MATERIALS QUANTITY
1. Penta erythritol 250 Kgs
2. Stearic acid 1314 Kgs
3. visinol palmitic acid 10 Kgs
4. caustic soda NaOH 2.0 Kgs
MANUFACTURING PROCESS:-
1. Add Stearic acid into the reactor. Raise temperature to 250°C.
2. Add visinol palmitic acid 5 Kgs.
3. Add penta erythritol slowly in to the reactor. Addition should be done in 5-6 hrs.
4. Run the batch for 4 hour. Determine acid value.
5. Add 5 Kgs. Vicinol palmitic acid & run for 4 hrs.
6. Check the acid vale.
7. Apply vacuum 750 mm minimum for 6-8 hrs,. till acid value is below 10.0.
8. Kill visinol palmitic acid by adding T-310 slowly.
9. Power the material.
Example 11
Process for preparation of zinc state oleate
RAW MATERIALS QUANTITY
1. stearic acid 332.5 Kgs
2. Oleic acid 175 Kgs
3. Zinc oxide 80 Kgs
MANUFACTURING PROCESS:-
1. Charge stearic acid and Oleic acid to the reactor and star heating.
2. Start stirring on melting and take temp to 200°C.
3. Start addition of Zinc oxide slowly (6.0 hrs ±1.0 hrs min) taking care that the reaction
mass does not rise up and overflow.
4. After addition of Zinc oxide take temp, to 250°C under stirring and powder.
Example 12
Process for preparation of di stearyl phthalate
RAW MATERIALS QUANTITY
1. Stearyl alcohol 1800 Kgs
2. Lauryl alcohol 100 Kgs
3. Phthalic anhydride 500 Kgs
4. Tego 233 10 Kgs
5. Finanox-8 5 Kgs
MANUFACTURING PROCESS:-
1. Add Stearyl alcohol and Lauryl alcohol into the reactor and star heating at 150°C .
Start the Stirrer & slowly Add Phthalic anhydride (5.0 Kgs) & Finanox-8under
stirring.
2. Raise temp. to 200°C & Start Phthalic anhydride addition Slowly over a period of 6
hrs, Allow steam to escape. (Maintain temperature up to 200°C during addition).
3. Slowly raise temperature to 250°C and run for 6 hrs. Check A.V. (100 ± 5).
4. Raise Temperature to 250°C & run for 6 hrs. Check A.V. (50± 5).
5. Add remaining Tego 233 (250 Kgs) & apply vacuum for 8-10 hrs at 250°C.
6. When A.V. is below 10, powder the material.
Example 13
Preparation of di ceto stearyl phthalate
RAW MATERIALS QUANTITY
1. Ceto stearyl alcohol 1700 Kgs
2. Lauryl alcohol 100 Kgs
3. Phthalic anhydride 500 Kgs
4. Tego 233 10 Kgs
5. Finanox-8 5 Kgs
MANUFACTURING PROCESS:-
1. Add Ceto stearyl alcohol and Lauryl alcohol into the reactor and star heating at 150°C
. Start the Stirrer & slowly Add Tego 233 (5.0 Kgs) & Finanox-8under stirring.
2. Raise temp. to 125°C & Start Phthalic anhydride addition Slowly over a period of 3
hrs, Allow steam to escape. (Maintain temperature up to 125°C during addition) .
3. Slowly raise temperature to 200°C and run for 2 hrs. Check A.V. (100 ±5).
4. Raise Temperature to 250°C & run for 4 hrs. Check A.V. (50 ± 5).
5. Add remaining Tego 233 (5 Kgs) & apply vacuum (750mm minimum) for 12 hrs at
250°C.
6. When A.V. is below 10, powder the material.
Example 14
Preparation of amide ester
RAW MATERIALS QUANTITY
1. Stearic acid 2000 Kgs
2. methyl ethyl acetate 300 Kgs
3. visionol palmitic acid 15 Kgs
4. sodium boro hydride 1 Kgs
MANUFACTURING PROCESS:-
1. Add Stearic acid and methyl ethyl acetate into the reactor. Melt the mass & Start
Stirrer.
2. Add sodium boro hydride (1 Kgs in 500 ml water) and mix well.
3. Add visionol palmitic acid while stirring.
4. Raise Temperature slowly to 200°C in 5 hrs. time.
5. Allow steam to escape. Then apply vacuum for 6hrs. (750 mm min.)
6. Check Acid Value . It should be below 50.
7. Use the material in the manufacture of mixed ester of fatty acid.
Example 15
Process for preparation of mixed ester of fatty acid
RAW MATERIALS QUANTITY
1. stearic acid 600 Kgs
2. Lime 125 Kgs
3. amide ester 750 Kgs
4. sodium boro hydride 1 Kgs
MANUFACTURING PROCESS:-
1. Heat stearic acid to 120°C ± 5°C & Start Stirrer .
2. Add sodium boro hydride +100 ml water.
3. Heat to 150°C±5°C.
4. Add lime slowly for 3 hrs.
5. Raise Temp to 200°C
6. Start adding amide ester with continuous heating & stirring .
7. Raise Temp to 250°C ± 5°C
8. Power the material.
Example 16
Process for preparation of Penta adipate stearate
RAW MATERIALS QUANTITY
1. stearic acid 1850 Kgs
2. Adipic acid 400 Kgs
3. penta erythritol 400 Kgs
4. Tego 233 5 Kgs
5. Finanox-8 1.5 Kgs
MANUFACTURING PROCESS:-
1. Heat Stearic acid to 110°C -120°C .
2. Add Finanox-8at 110°C-120°C
3. Add Adipic acid maintaining temp 200°C
4. Raise temp to 250°C .
5. Add Tego 233 (2.5 Kg). Run 30 minutes slowly for 3 hrs.
6. Add penta erythritol for 3 hrs at 250°C
7. Run the batch till A.V. <30
8. Add Tego 233Run 30 min.
9. Apply vacuum 6hrs. & check A.V. Raise Temp to 250°C ± 5°C
10. Add Tego 233, Run 30 min.
11. Apply vacuum 6 hrs. Check A.V.
12. Add T-313, Run 60 min.
13. Apply vacuum, Check A.V.
14.Check A.V.<6
15. Powder & pack. 25
Example 17
Process for preparation of Mixed ester of penta adipate stearate and
glycerol mono stearate
RAW MATERIALS QUANTITY
1. Penta adipate stearate +
Stearic acid 1625 Kgs
2. Glycerol mono stearate 1000 Kgs
MANUFACTURING PROCESS:-
1. Transfer Penta adipate stearate molten or power in to the reactor. If power material is
used, melt and raise temp. to 200°C
2. Add Glycerol mono stearate molten or powder to the above and raise temp, up to
250°C
3. Mix well for 4-1 hr.
4. Powder the material. .
Example 18
Process for Preparation of sorbitan mono stearate
RAW MATERIALS QUANTITY
1. sorbitol 1200 Kgs
2. sodium boro hydride 1.0 Kgs
3. stearic acid 1650 KGS
4. caustic soda NaOH 5.0 KGS
5. sodium chlorite 5.0 KGS
6. Hydrogen peroxide 10 KGS
7. antifoam 5.0 KGS
MANUFACTURING PROCESS:-
1. Add sorbitol (70%) to the reactor.
2. Add T-315 dissolved in equal part of water about 5 gms of sodium boro hydride.
3. Raise the temp . to 200°C to 6 hrs. to dry the sorbitol.
4. Manually check the dried sorbitol.
5. Add entire quantity of stearic acid into the reactor.
6. again raise temperature to 250°C
7. Add caustic soda NaOH & close the reactor.
8. Apply direct vacuum, about 600 ± 50 mm. Initially (temp. 200°C & vacuum 700±25
mm finally (temp. 250°C).
9. Raise temp 250°C (it should take more than 6 hrs. for the temp.
10. Maintain at 250°C for 200 min. Check melting point, it should be 58-60°C.
11. Cool to 100°C under vacuum.
12. Stop the stirrer & release vacuum but continue cooling up to 150°C.
13. At 90°C, remove the settle charred unrelated sorbitol (about 10-15 kgs)
14. Bleach the remaining mass at 150°C initially by sodium chlorite (50%) sol.
15. Powder the product.
Example 19
Process for Preparation of sorbitan mono palmitate
RAW MATERIAL QUANTITY
1. sorbitol 350.0 Kgs.
2. sodium boro hydride 0.500-0.600 Kgs.
3. Palmitic acid 600 Kgs.
4. caustic soda NaOH 1.5 Kgs.
5. sodium chlorite 3 To 5 Kgs.
6. Hydrogen peroxide 5.0 Kgs
7. Antifoam 2.0 Kgs
MANUFACTURING PROCESS :-
1. Add sorbitol (70%) to the reactor
2. Add sodium boro hydride dissolved in equal parts of water with about 5 gms of
caustic soda NaOH
3. Raise the temp. 200° - 220° C for 2 hrs. to dry the sorbitol
4. Manually check the dried sorbitol
5. Add entire quantity of Palmitic acid into the reactor.
6. Again raise temperature to 220° C
7. Add caustic soda NaOH and close the reactor
8. Apply direct vacuum, about 600 ± 50 mm. Initially (temp. 220° C) And vaccum
725 ± 25 mm. finally (temp. 225-240°C)
9. Raise temp. To 250°C (it should take more than 6 hrs. for the temp. To reach
250°C )
10. Maintain at 250°C for 2 min. only.
11. Cool to 150°C under vacuum.
12. Stop the stirrer and release vacuum but continue cooling upto 100°C.
13. At 100°C , remove the settled charred untreated sorbitol (about 10-15 Kgs.)
14. Bleach the remaining mass at 90°C initially by sodium chlorite (50%) sol .
Followed by Hydrogen peroxide for about 20 min.
15. Powder the product.
Example 20
Process for preparation of Ethylene bis stearmide
RAW MATERIAL QUANTITY
1. stearic acid 1500.0 Kgs.
2. ethyl diacetate 200 Kgs.
3. sodium borohydride 1.0 Kgs.
4. antifoam 2.0 Kgs.
5. Visinol palmitic acid 20.0 Kgs.
6. BHT 0.5 Kgs
7. TNPP 0.5 Kgs
8. Finanox-8 5.0 Kgs.
MANUFACTURING PROCESS :-
1. Add stearic acid to the reactor and raise temp. To 100°C. Start the Stirrer. Add
sodium borohydride and antifoam Deformer and Finanox-8
2. Weigh ethyl diacetate in addition Vessel. Close the heating valve & Start Cooling.
Start adding ethyl diacetate slowly in the reactor. (Time required 1 ½ hour).
Temp. 125°C.
3. After ethyl diacetate addition is over, start heating slowly and raise Temp. To
140°C±5°C. (Time:4 hrs.)
4. Allow steam to escape completely. Avoid overflowing of the Batch. Now raise the
tern. To 200°C.
5. Immediately determine free amine of the batch (It will be around 1.0).
Note :- Free amine of the batch should be 1 max. Accordingly batch should be run
depending upon initial Free amine at 180°C. Normally there is a drop of 0.5 Units
in free amine per hour, therefore quality control Will inform production
accordingly how long the batch Should run.
6. As soon as free amine is in the range, add BHT and TNPP After about 5-10
minutes add visinol palmitic acid.
7. Maintain the batch at 200 ±°C for 5 to 5 14 hrs.
8. Powder the material. (Keep first bag aside) and subsequently Pack the material in
standard bags.
Example 21
Process for preparation of Ethylene bis oleamide
RAW MATERIAL QUANTITY
1. oleic acid 1500.0 Kgs.
2. ethyl diacetate 200 Kgs.
3. sodium borohydride 1.0 Kgs.
4. antifoam 5.0 Kgs.
5. Finanox-8 5.0 Kgs.
6. BHA 2.0 Kgs.
MANUFACTURING PROCESS :-
1. Add oleic acid to the reactor and raise temp. To 100°C. Start the Stirrer. Add sodium
borohydride and antifoam and Finanox-8
2. Weigh ethyl diacetate in addition Vessel. Close the heating valve & Start Cooling.
Start adding ethyl diacetate slowly in the reactor. (Time required 1 Vz hour). Temp.
125°C.
3. After ethyl diacetate addition is over, start heating slowly and raise Temp. To 150°C
±5°C. (Time : 2.5 hrs.)
4. Allow steam to escape completely. Avoid overflowing of the Batch. Now raise the
tern. To 200°C.
5. Check A.V. & Total Amine. A.V should be below 10 & Total Amine should be below
5 Run the batch till above values are obtained.
6. Powder the material.(kept first bag aside) and subsequently Pack the material in
standard bags.
WE CLAIM:
1. An improved process for the preparation of fatty acid derivatives and oleo
chemicals comprising
reacting stearates such as glycerol tristreate, stearic acid with glycerine in
a reactor at a temperature of 80°C-160°C while stirring the both components and
slowly adding caustic soda and visinol palmitic acid to obtain glycerol mono
stearate and the mass is melted with mixed ethyl alcohol to obtain ethylene
glycol mono stearat and ethylene glycol di stearate; or
reacting stearyl alcohol/ ceto stearyl alcohol and stearic acid at a
temperature of 100°C-160°C while stirring both components and slowly adding
visinol palmitic acid and caustic soda NaOH to obtain stearyl stearate/ceto
stearyl stearate; or
reacting penta erythritol and stearic acid at a temperature of 200°C-260°C
while stirring both components and slowly adding visinol palmitic acid and
caustic soda NaOH to obtain penta distearate/penta tetrastearate; or
reacting stearyl alcohol/ceto stearyl alcohol and lauryl alcohol at a
temperature 100°C-200°C while stirring both components and slowly adding
phthalic anhydride in presence of Tego 233 and Finanox-8 to obtain di stearyl
phthalate/di ceto stearyl phthalate; or
reacting stearic acid and mixed ethyl acetate at a temperature 150°C-
200°C while stirring both components and slowly adding visinol palmitic acid
and sodium borohydride to obtain amide ester/mixed ester of fatty acids; or
heating stearic acid/palmitic acid and sodium borohydride at a temperatue
200°C-300°C and stirring with sorbitol, hydrogen peroxide, caustic soda NaOH,
antifoam to cooling down at a temperature 100°C and finally bleach the product
with sodium chlorite to obtain sorbitan mono stearate/sorbitan mono palmitate;
or
heating stearic acid/oleic acid with sodium boro hydride, antifoam,
Finanox-8 and then adding ethyl diacetate keeping the temperatue 150°C-200°C
and finally adding visinol palmitic acid, BHT, TNPP to obtain ethylene bis
stearmide/ethylene bis oleamide.
2. An improved process for the preparation of fatty acid derivatives and oleo
chemicals as claimed in claim 1, wherein the reaction is preferably carried under
vacuum which should be 700 to 760 mm (minimum) and temperature of the
process is carried out at around 100°C to 200°C for atleast 4 hours under
vacuum.
3. An improved process for the preparation of fatty acid derivatives and oleo
chemicals as claimed in claim 1, in the above mentioned process the acid value
should be below 3.0.
4. An improved process for the preparation of fatty acid derivatives and oleo
chemicals as claimed in claim 1, if desired, vicinonl palmitic acid, mixed ethyl
glycol, Finanox-8, ceto stearyl alcohol Tego 233, sorbitol is added to the
reaction product while stirring.
5. An improved process for the preparation of fatty acid derivatives and oleo
chemicals as claimed in claim 1, wherein penta erythritol is added to the
reactants for 5-6 hours and sodium borohydride is added to the reactants and
heated to the temperatue of 150°C and then treated with lime and amide ester.

An improved process for the preparation of fatty acid derivatives and oleo chemicals comprising reacting stearates such as glycerol tristreate, stearic acid with glycerine in a reactor at a temperature of 80°C-160°C while stirring the
both components and slowly adding caustic soda and visinol palmitic acid to obtain glycerol mono stearate and the mass is melted with mixed ethyl alcohol to obtain ethylene glycol mono stearat and ethylene glycol di stearate, reacting
stearyl alcohol/ ceto stearyl alcohol and stearic acid at a temperature of 100°C- 160°C while stirring both components and slowly adding visinol palmitic acid and caustic soda NaOH to obtain stearyl stearate/ceto stearyl stearate, reacting penta erythritol and stearic acid at a temperature of 200°C-260°C while stirring
both components and slowly adding visinol palmitic acid and caustic soda NaOH to obtain penta distearate/penta tetrastearate,

Documents

Application Documents

# Name Date
1 1114-kol-2009-abstract.pdf 2011-10-07
1 1114-kol-2009-specification.pdf 2011-10-07
2 1114-kol-2009-claims.pdf 2011-10-07
2 1114-kol-2009-pa.pdf 2011-10-07
3 1114-kol-2009-correspondence.pdf 2011-10-07
3 1114-kol-2009-form 5.pdf 2011-10-07
4 1114-kol-2009-description (complete).pdf 2011-10-07
4 1114-kol-2009-form 3.pdf 2011-10-07
5 1114-kol-2009-form 2.pdf 2011-10-07
5 1114-kol-2009-form 1.pdf 2011-10-07
6 1114-kol-2009-form 1.pdf 2011-10-07
6 1114-kol-2009-form 2.pdf 2011-10-07
7 1114-kol-2009-description (complete).pdf 2011-10-07
7 1114-kol-2009-form 3.pdf 2011-10-07
8 1114-kol-2009-correspondence.pdf 2011-10-07
8 1114-kol-2009-form 5.pdf 2011-10-07
9 1114-kol-2009-claims.pdf 2011-10-07
9 1114-kol-2009-pa.pdf 2011-10-07
10 1114-kol-2009-specification.pdf 2011-10-07
10 1114-kol-2009-abstract.pdf 2011-10-07