Title of Invention

PROCESS FOR THE EXTRACTION OF HIGH GRADE SOY LECITHIN IN POWDER AND LIQUID FORM

Abstract An improved process for the preparation of high grade Igcithin in powder and liquid form comprising the steps of, (a) solvent extraction of crude oil, from the seed material, using hexane as solvent; ^^ (b) removal of hexane by distillation; (c) "deoiling" the product of step (b) by treating with a first solvent in a centrifugal mixer under agitation with a bladed agitator to precipitate lecithin sludge with reduced particle size; (d) allowing the product of step (c) to stand for atleast one hour to separate into two layers; (e) separating the layers by decantation to obtain the solvent wet "deoiled lecithin"; (f) treating the "deoiled lecithin" obtained from step (e)' to a second solvent to obtain a phosphatidylcholine enriched fraction; (g) centrifuging to separate the soluble and insoluble fractions in a "disc bowl" in a manner well known in industry; (h) obtaining a phosphatidylcholine enriched soluble fraction and removing solvent and moisture by distillation and vacuum drying to obtain the phosphatidylcholine enriched high grade lecithin in powder form; and (i) adding diluents to fluidize the product obtained in step(K) (j) and blending to obtain high grade lecithin in liquid form. An improved process for the preparation of high grade Igcithin in powder and liquid form comprising the steps of, (a) solvent extraction of crude oil, from the seed material, using hexane as solvent; ^^ (b) removal of hexane by distillation; (c) "deoiling" the product of step (b) by treating with a first solvent in a centrifugal mixer under agitation with a bladed agitator to precipitate lecithin sludge with reduced particle size; (d) allowing the product of step (c) to stand for atleast one hour to separate into two layers; (e) separating the layers by decantation to obtain the solvent wet "deoiled lecithin"; (f) treating the "deoiled lecithin" obtained from step (e)' to a second solvent to obtain a phosphatidylcholine enriched fraction; (g) centrifuging to separate the soluble and insoluble fractions in a "disc bowl" in a manner well known in industry; (h) obtaining a phosphatidylcholine enriched soluble fraction and removing solvent and moisture by distillation and vacuum drying to obtain the phosphatidylcholine enriched high grade lecithin in powder form; and (i) adding diluents to fluidize the product obtained in step(K) (j) and blending to obtain high grade lecithin in liquid form
Full Text FORM 2
THE PATENTS ACT, 1970 (39ofl970)
COMPLETE SPECIFICATION (See Section 10)
TITLE

PROCESS FOR THE EXTRACTION OF HIGH GRADE SOY
LECITHIN IN POWDER AND LIQUID FORM

APPLICANT
KHANDELWAL SHYAM SUNDER of 11/4 MANORAMA GANJ, INDORE 452 001, MADHYA PRADESH
INDIA. A CITIZEN OF INDIA.

FIELD OF INVENTION
The present invention relates to an improved process for the preparation of high grade lecithin in powder and liquid form.
BACKGROUND OF THE INVENTION
Lecithin is a mixture of polar lipids available from vegetable and animal sources. The polar lipids are a mixture of glycolipids and phospholipids.
Commercial lecithin is a wetting and emulsifying agent. Lecithin is used in paints and plastics as it facilitates rapid pigment wetting and dispersion. Lecithin is used in fertilizers, textiles, etc. as an emulsifi'er.
The primary commercial source of lecithin is plant seed, the source of vegetable oils. Soybean forms a major source of commercial lecithin. The percentage composition of soylecithin is*
Phosphatidylcholine 20-22
Phosphatidylethanolamine 21-23
Phosphatidylinositol 18-20
Phosphatidic acid 4-8
Other phospholipids 15
Glycolipids 9-12

In the commercial extraction of lecithin from soybean, crude soybean oil, is extracted using hot hexane as solvent from the soybeans and the oil- hexane fraction obtained is termed as "miscella".
The "miscella" is filtered to remove minute particles of flaked seed called "fines" and the hexane is then removed by distillation to obtain the crude oil.
Lecithin is obtained from the crude oil by various purification processes, the most important being by the "deoiling process" when the neutral lipids and polar lipids are separated.
The crude oil is subjected to "deoiling process" by the addition of acetone when the pdlar lipids are thrown out of solution as an acetone insoluble whereas the neutral lipids are soluble in acetone. Extraction with acetone has to be repeated and the mixture subjected to intense agitation to enhance the extent of "deoiling". The polar lipids thrown out of solution as an acetone insoluble are in the form of a "slurry" and the top layer of acetone with neutral lipids must be removed in order to obtain acetone wet "lecithin sludge". The acetone insoluble, polar lipids separated out as acetone wet "lecithin sludge" must be dried to ob»tain "deoiled lecithin".
The "deoiled lecithin" obtained is subsequently treated with another solvent such as ethanol to obtain an ethanol

soluble phosphatidylcholine enriched fraction. The solvent is removed by distillation from the ethanol soluble phosphatidylcholine enriched fraction to obtain the powder form of lecithin and suitable diluents are added to it such as calcium chloride, fatty acids, vegetable oils, etc. and they are blended in order to obtain the liquid form of lecithin.
SUMMARY OF THE INVENTION
The object of the present invention is to provide an improved process for the preparation of high grade lecithin in powder and liquid form.
Accordingly, the present invention provides an improved process for the preparation of high grade lecithin in powder and liquid form comprising the steps of,
(a) solvent extraction of crude oil, from the seed material, using hexane as solvent;
(b) removal of hexane by distillation;
(c) "deoiling" the product of step (b) by treating with a first solvent in a centrifugal mixer under-agitation with a bladed agitator to precipitate lecithin sludge with reduced particle size;

(d) allowing the product of step (c) to stand for atleast one hour to separate into two layers;
(e) separating the layers by decantation to obtain the solvent wet "deoiled lecithin";

(f) treating the "deoiled lecithin" obtained from step (e)' to a second solvent to obtain a phosphatidylcholine enriched fraction;
(g) centrifuging to separate the soluble and insoluble fractions in a "disc bowl" in a manner well known in industry;
(h) obtaining a phosphatidYlcholine enriched soluble fraction
and removing solvent and moisture by distillation and vacuum
drying to obtain the phosphatidylcholine enriched high grade
lecithin in powder form; and
(i) adding diluents to fluidize the product obtained in step(Vi)
(j) and blending to obtain high grade lecithin in liquid
form.
DETAILED DESCRIPTION OF THE INVENTION
In the extraction of lecithin from soybean by the process of the invention, the crude oil, neutral lipids and phospholipids are coextracted by solvent extraction using hexane as solvent from the seed material. The seed quality is important for obtaining good quality lecithin. The better the seed quality and the lower the free fatty acids (FFA) present, the better is it for lecithin.
The crude oil- hexane solution containing lecithin extracted from the seed and termed as miscella is filtered to remove the residual meal and "fines" present as suspended impurities. The miscella is then, subjected to distillation for the removal of solvent hexane.

The crude soybean oil obtained is subjected to the "deoiling process" using acetone as solvent. Since intense agitation is important to enhance the extent of "deoiling" hence agitation using a bladed agitator in a centrifugal mixer is used to reduce particle size and thus lower crude oil entrainment in the lecithin sludge. The two layers formed are allowed to stand for atleast one hour in order to ensure good separation, when two separate layers are clearly formed, before the layers are separated by decantation. The lecithin sludge is bleached to remove the color by the action of hydrogen peroxide or benzoyl peroxide. The crude lecithin is dried. The dried lecithin termed as "deoiled lecithin" is a fine free flowing powder. It is a mixture of phospholipids (85%) and glycolipids (10%) with 5% of other substances. The phospholipids present are phosphatidylcholine (PC), phosphatidylethanolamine (PE), phosphatidic acid (PA) and phosphatidylinositol (PI).
The "deoiled lecithin" is further fractionated to obtain a phosphatidylcholine (PC) enriched fraction, Ethanol is added to the "deoiled lecithin" for the recovery of the phosphotidylcholine enriched fraction.
The ethanol soluble part is enriched in phosphatidylcholine whereas the ethanol insoluble part contains the acidic phospholipids such as phosphatidic acid and phosphatidylinositol with phosphatidyl ethanolamine being

distributed almost evenly between the ethanol soluble and the ethanol insoluble parts.
Starting material Soluble (A) Insoluble(B)
PC 22
PE 24
PI 16
PA 12
48 11
22 18
3 16
2 15
After treatment with ethanol, the solid obtained has the composition (B) whereas the solution obtained has the composition (A).
Centrifugal separation of soluble and insoluble lecithin is carried out in a "disc bowl" in a manner known per se.
The ethanol soluble phosphatidylcholine enriched fraction is distilled to remove the solvent and vacuum dried to obtain the high grade powder form of lecithin.
Suitable diluents such as vegetable oils and fatty acids are added to the powder form of lecithin and blending is carried out at 55°C to 90°C for a minimum of 2 hours to obtain the high grade liquid form of lecithin having a viscosity in the range of 7,500 to 10,500 centipoise at 25°C.
The following example is included by way of illustration and does not in any way restrict the scope of the invention.
Example
The soybean seed material was treated with hot hexane as solvent and extracted repeatedly. Atleast three extractions

were required. Filtration of the hexane- crude oil extract to remove the fines was carried out and the hexane was subsequently removed .by distillation. '
The crude oil was introduced into a centrifugal mixer and charged with acetone until a acetone: crude oil ratio of 5:1 is obtained. Two to four extractions were required. Agitation using a bladed agitator was used.
The crude lecithin sludge was allowed to stand for one hour and separated by decantation. The lecithin sludge as a filter cake was acetone wet "deoiled lecithin". Acetone was removed in a moving bed forced air dryer.
The deoiled lecithin was treated with ethanol to obtain phosphatidylcholine enriched soluble fraction. Ethanol was removed by distillation and the product was vacuum dried to obtain the powder form of lecithin. The powder form was blended with diluents such as vegetable oils and fatty acids to fluidize it and obtain lecithin in liquid form with a viscosity of 9,000 centipoise at 25°C .

I CLAIM
1. An improved process for the preparation of high grade Igcithin in powder and liquid form comprising the steps of,
(a) solvent extraction of crude oil, from the seed material, using hexane as solvent; ^^
(b) removal of hexane by distillation;

(c) "deoiling" the product of step (b) by treating with a first solvent in a centrifugal mixer under agitation with a bladed agitator to precipitate lecithin sludge with reduced particle size;
(d) allowing the product of step (c) to stand for atleast one hour to separate into two layers;
(e) separating the layers by decantation to obtain the solvent wet "deoiled lecithin";

(f) treating the "deoiled lecithin" obtained from step (e)' to a second solvent to obtain a phosphatidylcholine enriched fraction;
(g) centrifuging to separate the soluble and insoluble fractions in a "disc bowl" in a manner well known in industry;
(h) obtaining a phosphatidylcholine enriched soluble fraction and removing solvent and moisture by distillation and vacuum drying to obtain the phosphatidylcholine enriched high grade lecithin in powder form; and
(i) adding diluents to fluidize the product obtained in step(K) (j) and blending to obtain high grade lecithin in liquid form.

2. A process as claimed in claim 1, wherein the first solvent is acetone.
3. A process as claimed in claims l and 2, wherein the acetone: crude oil ratio is 5:1.
4. A process as claimed in any of the preceding claims wherein the "deoiled lecithin" obtained in step (e) is a mixture of phospholipids (85%) and glycolipids (10%) with 5% of other substances.
5. A process as claimed in claim 4, wherein the "deoiled lecithin" obtained in step (e) is bleached to remove the color by the action of hydrogen peroxide or benzoyl peroxide.
6. A process as claimed in claim 4, wherein the phospholipids present are phosphatidylcholine (PC), phosphatidylethanolamine (PE), phosphatidic acid (PA) and phosphatidylinositol (PI).

7. A process as claimed in claim 1, wherein the second solvent is ethanol.
8. A process as claimed in claim 1, wherein the ethanol soluble phosphatidylcholine enriched fraction of step (h) has a composition of 48% phosphotidylcholine, 22% phosphatidylethanolamine, 3% phosphatidylinositol and 2% phosphatidic acid.
9. A process as claimed in claim 1, wherein the blending in step (h) is carried out with diluents selected from the group consisting of calcium chloride, fatty acids and vegetable oils.

10. A process as claimed in claim 1, wherein the blending
in step (h) is carried out at 55°C to 90°C for a minimum of 2
hours.
11. A process as claimed in claim 1, wherein the high grade liquid form of lecithin has a viscosity in the range of 7,500 to 10,500 centipoise at 25°C.
12. An improved process for the preparation of high grade lecithin in powder and liquid form, substantially as herein described particularly with reference to the foregoing example.
Dated this Znd day of May, 2001.

FORM 2
THE PATENTS ACT, 1970 (39ofl970)
COMPLETE SPECIFICATION (See Section 10)
TITLE

PROCESS FOR THE EXTRACTION OF HIGH GRADE SOY
LECITHIN IN POWDER AND LIQUID FORM

APPLICANT
KHANDELWAL SHYAM SUNDER of 11/4 MANORAMA GANJ, INDORE 452 001, MADHYA PRADESH
INDIA. A CITIZEN OF INDIA.

FIELD OF INVENTION
The present invention relates to an improved process for the preparation of high grade lecithin in powder and liquid form.
BACKGROUND OF THE INVENTION
Lecithin is a mixture of polar lipids available from vegetable and animal sources. The polar lipids are a mixture of glycolipids and phospholipids.
Commercial lecithin is a wetting and emulsifying agent. Lecithin is used in paints and plastics as it facilitates rapid pigment wetting and dispersion. Lecithin is used in fertilizers, textiles, etc. as an emulsifi'er.
The primary commercial source of lecithin is plant seed, the source of vegetable oils. Soybean forms a major source of commercial lecithin. The percentage composition of soylecithin is*
Phosphatidylcholine 20-22
Phosphatidylethanolamine 21-23
Phosphatidylinositol 18-20
Phosphatidic acid 4-8
Other phospholipids 15
Glycolipids 9-12

In the commercial extraction of lecithin from soybean, crude soybean oil, is extracted using hot hexane as solvent from the soybeans and the oil- hexane fraction obtained is termed as "miscella".
The "miscella" is filtered to remove minute particles of flaked seed called "fines" and the hexane is then removed by distillation to obtain the crude oil.
Lecithin is obtained from the crude oil by various purification processes, the most important being by the "deoiling process" when the neutral lipids and polar lipids are separated.
The crude oil is subjected to "deoiling process" by the addition of acetone when the pdlar lipids are thrown out of solution as an acetone insoluble whereas the neutral lipids are soluble in acetone. Extraction with acetone has to be repeated and the mixture subjected to intense agitation to enhance the extent of "deoiling". The polar lipids thrown out of solution as an acetone insoluble are in the form of a "slurry" and the top layer of acetone with neutral lipids must be removed in order to obtain acetone wet "lecithin sludge". The acetone insoluble, polar lipids separated out as acetone wet "lecithin sludge" must be dried to ob»tain "deoiled lecithin".
The "deoiled lecithin" obtained is subsequently treated with another solvent such as ethanol to obtain an ethanol

soluble phosphatidylcholine enriched fraction. The solvent is removed by distillation from the ethanol soluble phosphatidylcholine enriched fraction to obtain the powder form of lecithin and suitable diluents are added to it such as calcium chloride, fatty acids, vegetable oils, etc. and they are blended in order to obtain the liquid form of lecithin.
SUMMARY OF THE INVENTION
The object of the present invention is to provide an improved process for the preparation of high grade lecithin in powder and liquid form.
Accordingly, the present invention provides an improved process for the preparation of high grade lecithin in powder and liquid form comprising the steps of,
(a) solvent extraction of crude oil, from the seed material, using hexane as solvent;
(b) removal of hexane by distillation;
(c) "deoiling" the product of step (b) by treating with a first solvent in a centrifugal mixer under-agitation with a bladed agitator to precipitate lecithin sludge with reduced particle size;

(d) allowing the product of step (c) to stand for atleast one hour to separate into two layers;
(e) separating the layers by decantation to obtain the solvent wet "deoiled lecithin";

(f) treating the "deoiled lecithin" obtained from step (e)' to a second solvent to obtain a phosphatidylcholine enriched fraction;
(g) centrifuging to separate the soluble and insoluble fractions in a "disc bowl" in a manner well known in industry;
(h) obtaining a phosphatidYlcholine enriched soluble fraction
and removing solvent and moisture by distillation and vacuum
drying to obtain the phosphatidylcholine enriched high grade
lecithin in powder form; and
(i) adding diluents to fluidize the product obtained in step(Vi)
(j) and blending to obtain high grade lecithin in liquid
form.
DETAILED DESCRIPTION OF THE INVENTION
In the extraction of lecithin from soybean by the process of the invention, the crude oil, neutral lipids and phospholipids are coextracted by solvent extraction using hexane as solvent from the seed material. The seed quality is important for obtaining good quality lecithin. The better the seed quality and the lower the free fatty acids (FFA) present, the better is it for lecithin.
The crude oil- hexane solution containing lecithin extracted from the seed and termed as miscella is filtered to remove the residual meal and "fines" present as suspended impurities. The miscella is then, subjected to distillation for the removal of solvent hexane.

The crude soybean oil obtained is subjected to the "deoiling process" using acetone as solvent. Since intense agitation is important to enhance the extent of "deoiling" hence agitation using a bladed agitator in a centrifugal mixer is used to reduce particle size and thus lower crude oil entrainment in the lecithin sludge. The two layers formed are allowed to stand for atleast one hour in order to ensure good separation, when two separate layers are clearly formed, before the layers are separated by decantation. The lecithin sludge is bleached to remove the color by the action of hydrogen peroxide or benzoyl peroxide. The crude lecithin is dried. The dried lecithin termed as "deoiled lecithin" is a fine free flowing powder. It is a mixture of phospholipids (85%) and glycolipids (10%) with 5% of other substances. The phospholipids present are phosphatidylcholine (PC), phosphatidylethanolamine (PE), phosphatidic acid (PA) and phosphatidylinositol (PI).
The "deoiled lecithin" is further fractionated to obtain a phosphatidylcholine (PC) enriched fraction, Ethanol is added to the "deoiled lecithin" for the recovery of the phosphotidylcholine enriched fraction.
The ethanol soluble part is enriched in phosphatidylcholine whereas the ethanol insoluble part contains the acidic phospholipids such as phosphatidic acid and phosphatidylinositol with phosphatidyl ethanolamine being

distributed almost evenly between the ethanol soluble and the ethanol insoluble parts.
Starting material Soluble (A) Insoluble(B)
PC 22
PE 24
PI 16
PA 12
48 11
22 18
3 16
2 15
After treatment with ethanol, the solid obtained has the composition (B) whereas the solution obtained has the composition (A).
Centrifugal separation of soluble and insoluble lecithin is carried out in a "disc bowl" in a manner known per se.
The ethanol soluble phosphatidylcholine enriched fraction is distilled to remove the solvent and vacuum dried to obtain the high grade powder form of lecithin.
Suitable diluents such as vegetable oils and fatty acids are added to the powder form of lecithin and blending is carried out at 55°C to 90°C for a minimum of 2 hours to obtain the high grade liquid form of lecithin having a viscosity in the range of 7,500 to 10,500 centipoise at 25°C.
The following example is included by way of illustration and does not in any way restrict the scope of the invention.
Example
The soybean seed material was treated with hot hexane as solvent and extracted repeatedly. Atleast three extractions

were required. Filtration of the hexane- crude oil extract to remove the fines was carried out and the hexane was subsequently removed .by distillation. '
The crude oil was introduced into a centrifugal mixer and charged with acetone until a acetone: crude oil ratio of 5:1 is obtained. Two to four extractions were required. Agitation using a bladed agitator was used.
The crude lecithin sludge was allowed to stand for one hour and separated by decantation. The lecithin sludge as a filter cake was acetone wet "deoiled lecithin". Acetone was removed in a moving bed forced air dryer.
The deoiled lecithin was treated with ethanol to obtain phosphatidylcholine enriched soluble fraction. Ethanol was removed by distillation and the product was vacuum dried to obtain the powder form of lecithin. The powder form was blended with diluents such as vegetable oils and fatty acids to fluidize it and obtain lecithin in liquid form with a viscosity of 9,000 centipoise at 25°C .

I CLAIM
1. An improved process for the preparation of high grade Igcithin in powder and liquid form comprising the steps of,
(a) solvent extraction of crude oil, from the seed material, using hexane as solvent; ^^
(b) removal of hexane by distillation;

(c) "deoiling" the product of step (b) by treating with a first solvent in a centrifugal mixer under agitation with a bladed agitator to precipitate lecithin sludge with reduced particle size;
(d) allowing the product of step (c) to stand for atleast one hour to separate into two layers;
(e) separating the layers by decantation to obtain the solvent wet "deoiled lecithin";

(f) treating the "deoiled lecithin" obtained from step (e)' to a second solvent to obtain a phosphatidylcholine enriched fraction;
(g) centrifuging to separate the soluble and insoluble fractions in a "disc bowl" in a manner well known in industry;
(h) obtaining a phosphatidylcholine enriched soluble fraction and removing solvent and moisture by distillation and vacuum drying to obtain the phosphatidylcholine enriched high grade lecithin in powder form; and
(i) adding diluents to fluidize the product obtained in step(K) (j) and blending to obtain high grade lecithin in liquid form.

2. A process as claimed in claim 1, wherein the first solvent is acetone.
3. A process as claimed in claims l and 2, wherein the acetone: crude oil ratio is 5:1.
4. A process as claimed in any of the preceding claims wherein the "deoiled lecithin" obtained in step (e) is a mixture of phospholipids (85%) and glycolipids (10%) with 5% of other substances.
5. A process as claimed in claim 4, wherein the "deoiled lecithin" obtained in step (e) is bleached to remove the color by the action of hydrogen peroxide or benzoyl peroxide.
6. A process as claimed in claim 4, wherein the phospholipids present are phosphatidylcholine (PC), phosphatidylethanolamine (PE), phosphatidic acid (PA) and phosphatidylinositol (PI).

7. A process as claimed in claim 1, wherein the second solvent is ethanol.
8. A process as claimed in claim 1, wherein the ethanol soluble phosphatidylcholine enriched fraction of step (h) has a composition of 48% phosphotidylcholine, 22% phosphatidylethanolamine, 3% phosphatidylinositol and 2% phosphatidic acid.
9. A process as claimed in claim 1, wherein the blending in step (h) is carried out with diluents selected from the group consisting of calcium chloride, fatty acids and vegetable oils.

10. A process as claimed in claim 1, wherein the blending
in step (h) is carried out at 55°C to 90°C for a minimum of 2
hours.
11. A process as claimed in claim 1, wherein the high grade liquid form of lecithin has a viscosity in the range of 7,500 to 10,500 centipoise at 25°C.
12. An improved process for the preparation of high grade lecithin in powder and liquid form, substantially as herein described particularly with reference to the foregoing example.
Dated this Znd day of May, 2001.


Documents:

424-mum-2001-cancelled page(5-10-2006).pdf

424-mum-2001-claim(granted)-(5-10-2006).pdf

424-mum-2001-claims(granted)-(5-10-2006).doc

424-mum-2001-correspondence(30-10-2006).pdf

424-mum-2001-correspondence(ipo)-(7-10-2005).pdf

424-mum-2001-form 1(3-5-2001).pdf

424-mum-2001-form 13(5-10-2006).pdf

424-mum-2001-form 18(2-5-2005).pdf

424-mum-2001-form 2(granted)-(5-10-2006).doc

424-mum-2001-form 2(granted)-(5-10-2006).pdf

424-mum-2001-form 3(3-5-2001).pdf

424-mum-2001-form 4(3-5-2006).pdf

424-mum-2001-power of authority(28-9-2001).pdf


Patent Number 203177
Indian Patent Application Number 424/MUM/2001
PG Journal Number 40/2008
Publication Date 03-Oct-2008
Grant Date 31-Oct-2006
Date of Filing 03-May-2001
Name of Patentee KHANDELWAL SHYAM SUNDER
Applicant Address 11/4 MANORAMA GANJ, INDORE
Inventors:
# Inventor's Name Inventor's Address
1 KHANDELWAL SHYAM SUNDER 11/4 MANORAMA GANJ, INDORE 452001
PCT International Classification Number N/A
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA