Title of Invention	A PROCESS FOR REMOVAL OF NON-FATTY ACID FROM FATTY ACID
Abstract	The present invention relates to process for removal of non-fatty acid from fatty acid comprising the steps of:a)reacting said fatty acid with sodium Hydroxide at 70ºC to form a sodium soap solution;b)reacting Sodium Soap solution prepared at step(a)with solution of calcium nitrate at ambient temperatures to obtain calcium salt solution;c)filtering said calcium salt solution,d)extracting traces of non fatty acid from said calcium salt;e)splitting calcium salt cake with acid.

Title of Invention

A PROCESS FOR REMOVAL OF NON-FATTY ACID FROM FATTY ACID

Abstract

The present invention relates to process for removal of non-fatty acid from fatty acid comprising the steps of:a)reacting said fatty acid with sodium Hydroxide at 70ºC to form a sodium soap solution;b)reacting Sodium Soap solution prepared at step(a)with solution of calcium nitrate at ambient temperatures to obtain calcium salt solution;c)filtering said calcium salt solution,d)extracting traces of non fatty acid from said calcium salt;e)splitting calcium salt cake with acid.

Full Text	FORM 2 THE PATENTS ACT, 1970 (39 OF 1970) & THE PATENT RULES, 2003 COMPLETE SPECIFICATION [SECTION 10 ; RULE 13 ] "A PROCESS FOR REMOVAL OF NON-FATTY ACID FROM FATTY ACID" APPLICANT: GODREJ CONSUMERS PRODUCT LTD. NATIONALITY: COMPANY INCORPORATED UNDER THE ADDRESS: EASTERN EXPRESS COMPANIES ACT, 1956. PIROJSHANAGAR, HIGHWAY, VIKHROLI, MUMBAI- 400 079, MAHARASHTRA STATE, INDIA THE FOLLOWING SPECIFICATION DESCRIBES THE NATURE OF THIS INVENTION AND THE MANNER IN WHICH IT IS TO BE PERFORMED: - FIELD OF INVENTION: The present invention relates to a process for removal of non-fatty acid from fatty acids. More particularly, the present invention relates to a process for removal of non-fatty acid from fatty acids having carbon atoms ranging from C6 to C12 (low and medium weight). BACKGROUND OF THE INVENTION: The non-fatty acid materials are quantified by two analytical methods - 1. Unsaponifiable Matter 2. Non-Fatty Acid peaks in the GC of the Fatty Acid The process for removal of non-fatty acid is mainly done for low grade fatty acids, which contain around 7-10 % of non-fatty acid material, thus making this type of fatty acid unacceptable. The fatty acids used in premium quality products like foods, pharmaceuticals and cosmetics have to be of a high grade. The presence of non-fatty acid material diminishes the market value of the fatty acid as well as its use in high value products. These non-fatty acid materials are originally present in the vegetable oils, and are formed by enzymatic degradation of the oil, while it is still in the seed or fruit, from which it is extracted. These non-fatty acid materials basically include Aldehydes, Ketones and Hydrocarbons. In the case of lower quality fatty acids the percentage of non-fatty acid materials is higher than in the good quality fatty acids. The percentage of the non-fatty acid materials is further pronounced in the case of inferior low & medium molecular weight fatty acids - C6, C8, CIO and CI2. Since non-fatty acid materials are Aldehydes, Ketones and Hydrocarbons, their volatility is almost the same as that of the low & medium molecular weight fatty acids. 2 Since the amount of non-fatty acid materials is very high, simple chemical treatments will not be able to upgrade these fatty acids. Therefore physical processes would help in upgrading these fatty acids. The most common and well documented physical separation & purification process is that of Distillation. As is well known in the art, the separation efficiency of Distillation is dependent upon the boiling point and vapour pressure differences between two liquids. Unfortunately these non-fatty acid materials have the same boiling points & vapour pressures as that of low & medium molecular weight fatty acids. Hence both these liquids co-distill with each other and hence cannot be separated by Distillation. Prior Art US Patent No. 3965085 describes a process where in tall oil resins are converted to potassium soap and the aqueous soap mixture is extracted with organic solvents such as petroleum ether and acetone to remove non fatty acid neutral material. The soap is then split with sulphuric acid to give fatty acid. Here, the problem is that potassium soap being a good emulsifier; it prevents extraction of all the non-fatty acid materials into the organic layer. Hence a complete separation of these non-fatty acid materials at this stage itself is not possible unless it is converted to non emulsifying and water insoluble calcium soap. US Patent No. 4,151,160 describes a process where a tall oil fraction was heated to about 80°C and zinc oxide added to form molten zinc soap. The mixture was then distilled under vacuum to remove non soap material form molten zinc soap. Zinc soap was split to get fatty acid. Similarly, US Patent No. 4,483,791 describes a process where a tall oil fraction was treated with magnesium hydroxide to form magnesium soap magnesium soap. The mixture was then distilled under vacuum to remove non soap material form molten magnesium soap. Magnesium soap was split to get fatty acid. But here decomposition of Zn soap or Mg soap takes place due to high temperature and high 3 vacuum during processing i.e. during removal of unsaponified material, thereby degrading the color of fatty acid generating more unsaponified material in the final product. US Patent No. 4,076,700 describes a process wherein tall oil fatty acid is converted to sodium soap. The sodium soap slurry is then passed through thin film continuous reactor. A vacuum arrangement is present in the reactor to remove unsaponified material from top while soap is collected at the bottom of the reactor. The soap is split with sulphuric acid and subjected to vacuum distillation to get fatty acid free of unsaponified material. Here also due to high temperature and pressure the sodium soap is subjected to, there is decomposition of fatty soap taking place, thereby giving color and increase in unsaponified products after splitting of soap. OBJECT OF INVENTION: It is the object of the present invention to obviate the aforesaid drawbacks and provide an improved process for removal of non-fatty acid from fatty acid. Since physical methods alone will not help, physicochemical methods would be needed for the removal of non-fatty acid material. Since the fatty acids are a subset of a carboxylic acid group, they all have the -COOH group. One of the well known chemical reaction involving carboxylic acid is Saponification i.e. formation of soap by reacting with alkalis. Soaps (alkali salts of fatty acids) are soluble in water. The soap solution of the low & medium molecular weight fatty acids is a clear at 50% concentration even at room temperature. The preferred alkali metal to form water soluble soap is Sodium (Na). So we now have a 50% Na soap solution of the low & medium molecular weight fatty acids. In contrast to the fatty acids, the non-fatty acid materials described previously such as aldehydes, ketones, hydrocarbons do not react with alkalis nor are they soluble 4 in water. After this chemical treatment, the physical separation between the fatty acids, now present in the form of soap, and non-fatty acid materials is possible. But soap, being a good emulsifier, it prevents all the non-fatty acid materials from forming a separate layer above the soap solution and some of it gets dispersed into the above mentioned 50% soap solution. Hence a complete separation of these non-fatty acid materials at this stage itself is not possible. In order to remove the emulsified non-fatty material from the soap solution, an organic solvent like hexane would be needed for extraction. Liquid-Liquid extractions require large volumes of the organic extractant to completely remove the non-fatty acid material. More advantageously, if instead, the water soluble Na soap was converted into a water insoluble Calcium (Ca) soap it could be washed, filtered and dried. This would simplify the separation process, as well as increase the amount of non-fatty acid material removed. A further advantage is that, even the solvent extraction process will be simplified and lower operational volumes will be required. Additionally, isolating the fatty acid as its Ca soap would make the process of recycling the organic extracting solvent also easier. This is the principle behind the process of lowering the non-fatty acid material in the low & medium molecular weight fatty acids. Hence the present invention discloses a process to make fatty acids having a lower percentage of non-fatty acid material, obtained from vegetable oils and fats, having even chained carbon atoms ranging from C6 to C24. SUMMARY OF THE INVENTION: The present invention relates to process for removal of non-fatty acid from fatty acid comprising the steps of: - 5 a) reacting said fatty acid with Sodium Hydroxide at 70°C to form a Sodium Soap solution; b) reacting Sodium Soap solution prepared at step (a) with solution of calcium nitrate at ambient temperatures to obtain calcium salt solution; c) filtering said calcium salt solution; d) extracting traces of non fatty acid from said calcium salt; e) splitting calcium salt cake with acid. DETAILED DESCRIPTION OF THE INVENTION: The present invention envisages a process for removing non fatty acid material from the fatty acid comprising the following steps: a) reacting said fatty acid with Sodium Hydroxide at 70°C to form a Sodium Soap solution; The Sodium Soap solution is diluted with water to 30 - 60 %, preferably 50%. b) reacting Sodium Soap solution prepared at step (a) with solution of calcium nitrate at ambient temperatures to obtain calcium salt solution; The Calcium salt is insoluble in water and thus settles at the bottom. c) filtering said calcium salt solution. The Calcium salt is filtered using a Buchner funnel and washed with enough water to free it of Calcium Nitrate and Sodium Hydroxide. d) extracting traces of non fatty acid from said calcium salt using hexane at 68°C to 70°C using known soxhlet apparatus for 4 to 8 hours, preferably 6 hours; e) splitting calcium salt cake using 50% H2SO4 at ambient temperatures. The next step involves washing the above fatty acid free of sulphuric acid and dried. The present invention involves removal of non-fatty acid material at every step. 6 The present invention will now be described with reference to the following examples. However, the examples in no way limit the scope of the invention. Examples Example I 500 grams of Low & Medium Chain Fatty Acids (fraction containing C6 to C12 fatty acids) having Unsaponifiable Matter = 3.5% and Non Fatty Acids (by GC) = 6.5%, is distilled by the normal distillation technique. The distilled fatty acid obtained is analyzed for percentage non fatty acid material as % Unsaponifiable Matter and % Non Fatty Acids (by GC). Although the distilled fatty acid had a much lighter color, the % of unsaponifiable matter and the non fatty acids (by GC) has not been lowered. Example II 500 grams of Low & Medium Chain Fatty Acids (fraction containing C6 to C12 fatty acids) having Unsaponifiable Matter = 3.5% and Non Fatty Acids (by GC) = 6.5%, is converted to a 50% Sodium Soap solution with dilute Sodium Hydroxide by the known soap making methods. This 50% solution is clear liquid at room temperature. The Sodium soap solution is then extracted thrice with 50ml portions of hexane each and the unsaponifiable material is separated. The extraction took 48 hrs due heavy emulsion formation. The aqueous layer is separated and acidified with 50% sulphuric acid and the fatty acid being a liquid separates out above the aqueous layer. Fatty acid is washed with water till free of sulphuric acid. The fatty acid obtained is dried and analyzed for percentage non fatty acid material as % Unsaponifiable Matter and % Non Fatty Acids (by GC). Example III 7 500 grams of Low & Medium Chain Fatty Acids (fraction containing C6 to C12 fatty acids) having Unsaponifiable Matter = 3.5% and Non Fatty Acids (by GC) = 6.5%, is converted to a 50% Sodium Soap solution with dilute Sodium Hydroxide by the known soap making methods. This 50% solution is clear liquid at room temperature. A clear solution of Calcium Nitrate is prepared and is added to the Sodium soap solution to give a 50% water insoluble Calcium soap solution. The Calcium soap formed precipitates put as a fine, pale, cream solid. After ensuring complete conversion to the Calcium soap the solution is filtered using a Buchner funnel and washed with enough water to free it of Calcium Nitrate and Sodium Hydroxide. The Calcium salt cake thus obtained is split with 50% sulphuric acid and the fatty acid separated. Fatty acid is washed with water till free of sulphuric acid. The fatty acid obtained is dried and analyzed for percentage non fatty acid material as % Unsaponifiable Matter and % Non Fatty Acids (by GC). Example IV showing Inventive Step 500 grams of Low & Medium Chain Fatty Acids (fraction containing C6 to C12 fatty acids) having Unsaponifiable Matter = 3.5% and Non Fatty Acids (by GC) = 6.5%, is converted to a 50% Sodium Soap solution with dilute Sodium Hydroxide by the known soap making methods. This 50% solution is clear liquid at room temperature. A clear solution of Calcium Nitrate is prepared and is added to the Sodium soap solution to give a 50% water insoluble Calcium soap solution. The Calcium soap formed precipitates out as a fine, pale, cream solid. After ensuring complete conversion to the Calcium soap the solution is filtered using a Buchner funnel and washed with enough water to free it of Calcium Nitrate and Sodium Hydroxide. The Calcium soap thus obtained is extracted with Hexane using soxhlet apparatus, where only 500ml of solvent can be used for each lot. The Calcium salt cake is then split with 50% sulphuric acid to obtain fatty acid. Fatty acid is washed with water till free of sulphuric acid. The fatty acid obtained is dried and analyzed for percentage non fatty acid material as % Unsaponifiable Matter and % Non Fatty Acids (by GC). 8 Measurement The fatty acid is analyzed for percentage of non fatty acid material by the usual methods of % unsaponifiable matter as well as % non fatty acid peaks by gas chromatography. Results Table Unsaponifiable Matter % Non-Fatty-Acid (by GC) % Example I 3.5 6.5 Example II 1.5 1.8 Example III 0.8 0.8 Example IV 0.14 0.2 9 We Claim: 1. A process for removal of non-fatty acid from fatty acid comprising the steps of: - a) reacting said fatty acid with Sodium Hydroxide at 70°C to form a Sodium Soap solution; b) reacting Sodium Soap solution prepared at step (a) with solution of calcium nitrate at ambient temperatures to obtain calcium salt solution; c) filtering said calcium salt solution; d) extracting traces of non fatty acid from said calcium salt; e) splitting calcium salt cake with acid. 2. A process as claimed in Claim 1, wherein said fatty acids are selected from C6 to C12. 3. A process as claimed in Claim 1, wherein said extraction in step (d) is carried out using hexane at 68°C to 70°C using known soxhlet apparatus for 4 to 8 hours. 4. A process as claimed in Claim 3, wherein said extraction is carried out for 6 hours. 5. A process as claimed in Claim 1, wherein said splitting in step (e) is done using 50% H2SO4 at ambient temperatures. 6. A process as claimed in Claim 1, wherein said Sodium Soap solution in step (a) is diluted to 30 - 60 %. 7. A process as claimed in Claim 6, wherein said Sodium Soap solution is diluted to 50%. 10 8. A process for removal of non-fatty acid from fatty acid substantially described herein with reference to examples. Dated this 29™ day of March ,2006. Himanshu W. Kane (Applicants' Patent Agent) S-3/PATENT/GODREJ/NEW PATENT/REMOVAL OF NON-FATTY ACID/CS NFM REMOVAL FA FINAL 11 ABSTRACT The present invention relates to process for removal of non-fatty acid from fatty acid comprising the steps of: a) reacting said fatty acid with Sodium Hydroxide at 70°C to form a Sodium Soap solution; b) reacting Sodium Soap solution prepared at step (a) with solution of calcium nitrate at ambient temperatures to obtain calcium salt solution; c) filtering said calcium salt solution; d) extracting traces of non fatty acid from said calcium salt; e) splitting calcium salt cake with acid. S-3/PATENT/GODREJ/NEW PATENT/REMOVAL OF NON-FATTY ACID/CS NFM REMOVAL FA FINAL 12

Full Text

FORM 2
THE PATENTS ACT, 1970
(39 OF 1970)
&
THE PATENT RULES, 2003

COMPLETE SPECIFICATION

[SECTION 10 ; RULE 13 ]

"A PROCESS FOR REMOVAL OF NON-FATTY ACID FROM FATTY
ACID"

APPLICANT:

GODREJ CONSUMERS PRODUCT LTD.

NATIONALITY: COMPANY INCORPORATED UNDER THE

ADDRESS:

EASTERN
EXPRESS
COMPANIES ACT, 1956. PIROJSHANAGAR,
HIGHWAY, VIKHROLI, MUMBAI- 400 079, MAHARASHTRA STATE, INDIA

THE FOLLOWING SPECIFICATION DESCRIBES THE NATURE OF THIS INVENTION AND THE MANNER IN WHICH IT IS TO BE PERFORMED: -

FIELD OF INVENTION:
The present invention relates to a process for removal of non-fatty acid from fatty acids. More particularly, the present invention relates to a process for removal of non-fatty acid from fatty acids having carbon atoms ranging from C6 to C12 (low and medium weight).
BACKGROUND OF THE INVENTION:
The non-fatty acid materials are quantified by two analytical methods -
1. Unsaponifiable Matter
2. Non-Fatty Acid peaks in the GC of the Fatty Acid
The process for removal of non-fatty acid is mainly done for low grade fatty acids, which contain around 7-10 % of non-fatty acid material, thus making this type of fatty acid unacceptable. The fatty acids used in premium quality products like foods, pharmaceuticals and cosmetics have to be of a high grade. The presence of non-fatty acid material diminishes the market value of the fatty acid as well as its use in high value products.
These non-fatty acid materials are originally present in the vegetable oils, and are formed by enzymatic degradation of the oil, while it is still in the seed or fruit, from which it is extracted. These non-fatty acid materials basically include Aldehydes, Ketones and Hydrocarbons. In the case of lower quality fatty acids the percentage of non-fatty acid materials is higher than in the good quality fatty acids. The percentage of the non-fatty acid materials is further pronounced in the case of inferior low & medium molecular weight fatty acids - C6, C8, CIO and CI2. Since non-fatty acid materials are Aldehydes, Ketones and Hydrocarbons, their volatility is almost the same as that of the low & medium molecular weight fatty acids.
2

Since the amount of non-fatty acid materials is very high, simple chemical treatments will not be able to upgrade these fatty acids. Therefore physical processes would help in upgrading these fatty acids. The most common and well documented physical separation & purification process is that of Distillation. As is well known in the art, the separation efficiency of Distillation is dependent upon the boiling point and vapour pressure differences between two liquids. Unfortunately these non-fatty acid materials have the same boiling points & vapour pressures as that of low & medium molecular weight fatty acids. Hence both these liquids co-distill with each other and hence cannot be separated by Distillation.
Prior Art
US Patent No. 3965085 describes a process where in tall oil resins are converted to potassium soap and the aqueous soap mixture is extracted with organic solvents such as petroleum ether and acetone to remove non fatty acid neutral material. The soap is then split with sulphuric acid to give fatty acid. Here, the problem is that potassium soap being a good emulsifier; it prevents extraction of all the non-fatty acid materials into the organic layer. Hence a complete separation of these non-fatty acid materials at this stage itself is not possible unless it is converted to non emulsifying and water insoluble calcium soap.
US Patent No. 4,151,160 describes a process where a tall oil fraction was heated to about 80°C and zinc oxide added to form molten zinc soap. The mixture was then distilled under vacuum to remove non soap material form molten zinc soap. Zinc soap was split to get fatty acid.
Similarly, US Patent No. 4,483,791 describes a process where a tall oil fraction was treated with magnesium hydroxide to form magnesium soap magnesium soap. The mixture was then distilled under vacuum to remove non soap material form molten magnesium soap. Magnesium soap was split to get fatty acid. But here decomposition of Zn soap or Mg soap takes place due to high temperature and high
3

vacuum during processing i.e. during removal of unsaponified material, thereby degrading the color of fatty acid generating more unsaponified material in the final product.
US Patent No. 4,076,700 describes a process wherein tall oil fatty acid is converted to sodium soap. The sodium soap slurry is then passed through thin film continuous reactor. A vacuum arrangement is present in the reactor to remove unsaponified material from top while soap is collected at the bottom of the reactor. The soap is split with sulphuric acid and subjected to vacuum distillation to get fatty acid free of unsaponified material. Here also due to high temperature and pressure the sodium soap is subjected to, there is decomposition of fatty soap taking place, thereby giving color and increase in unsaponified products after splitting of soap.
OBJECT OF INVENTION:
It is the object of the present invention to obviate the aforesaid drawbacks and provide an improved process for removal of non-fatty acid from fatty acid.
Since physical methods alone will not help, physicochemical methods would be needed for the removal of non-fatty acid material. Since the fatty acids are a subset of a carboxylic acid group, they all have the -COOH group. One of the well known chemical reaction involving carboxylic acid is Saponification i.e. formation of soap by reacting with alkalis. Soaps (alkali salts of fatty acids) are soluble in water. The soap solution of the low & medium molecular weight fatty acids is a clear at 50% concentration even at room temperature. The preferred alkali metal to form water soluble soap is Sodium (Na). So we now have a 50% Na soap solution of the low & medium molecular weight fatty acids.
In contrast to the fatty acids, the non-fatty acid materials described previously such as aldehydes, ketones, hydrocarbons do not react with alkalis nor are they soluble
4

in water. After this chemical treatment, the physical separation between the fatty acids, now present in the form of soap, and non-fatty acid materials is possible. But soap, being a good emulsifier, it prevents all the non-fatty acid materials from forming a separate layer above the soap solution and some of it gets dispersed into the above mentioned 50% soap solution. Hence a complete separation of these non-fatty acid materials at this stage itself is not possible. In order to remove the emulsified non-fatty material from the soap solution, an organic solvent like hexane would be needed for extraction. Liquid-Liquid extractions require large volumes of the organic extractant to completely remove the non-fatty acid material.
More advantageously, if instead, the water soluble Na soap was converted into a water insoluble Calcium (Ca) soap it could be washed, filtered and dried. This would simplify the separation process, as well as increase the amount of non-fatty acid material removed.
A further advantage is that, even the solvent extraction process will be simplified and lower operational volumes will be required. Additionally, isolating the fatty acid as its Ca soap would make the process of recycling the organic extracting solvent also easier. This is the principle behind the process of lowering the non-fatty acid material in the low & medium molecular weight fatty acids.
Hence the present invention discloses a process to make fatty acids having a lower percentage of non-fatty acid material, obtained from vegetable oils and fats, having even chained carbon atoms ranging from C6 to C24.
SUMMARY OF THE INVENTION:
The present invention relates to process for removal of non-fatty acid from fatty acid comprising the steps of: -
5

a) reacting said fatty acid with Sodium Hydroxide at 70°C to form a Sodium Soap solution;
b) reacting Sodium Soap solution prepared at step (a) with solution of calcium nitrate at ambient temperatures to obtain calcium salt solution;
c) filtering said calcium salt solution;
d) extracting traces of non fatty acid from said calcium salt;
e) splitting calcium salt cake with acid.
DETAILED DESCRIPTION OF THE INVENTION:
The present invention envisages a process for removing non fatty acid material from the fatty acid comprising the following steps:
a) reacting said fatty acid with Sodium Hydroxide at 70°C to form a Sodium Soap solution; The Sodium Soap solution is diluted with water to 30 - 60 %, preferably 50%.
b) reacting Sodium Soap solution prepared at step (a) with solution of calcium nitrate at ambient temperatures to obtain calcium salt solution; The Calcium salt is insoluble in water and thus settles at the bottom.
c) filtering said calcium salt solution. The Calcium salt is filtered using a Buchner funnel and washed with enough water to free it of Calcium Nitrate and Sodium Hydroxide.
d) extracting traces of non fatty acid from said calcium salt using hexane at 68°C to 70°C using known soxhlet apparatus for 4 to 8 hours, preferably 6 hours;
e) splitting calcium salt cake using 50% H2SO4 at ambient temperatures.
The next step involves washing the above fatty acid free of sulphuric acid and dried.
The present invention involves removal of non-fatty acid material at every step.
6

The present invention will now be described with reference to the following examples. However, the examples in no way limit the scope of the invention.
Examples
Example I
500 grams of Low & Medium Chain Fatty Acids (fraction containing C6 to C12 fatty acids) having Unsaponifiable Matter = 3.5% and Non Fatty Acids (by GC) = 6.5%, is distilled by the normal distillation technique. The distilled fatty acid obtained is analyzed for percentage non fatty acid material as % Unsaponifiable Matter and % Non Fatty Acids (by GC). Although the distilled fatty acid had a much lighter color, the % of unsaponifiable matter and the non fatty acids (by GC) has not been lowered.
Example II
500 grams of Low & Medium Chain Fatty Acids (fraction containing C6 to C12 fatty acids) having Unsaponifiable Matter = 3.5% and Non Fatty Acids (by GC) = 6.5%, is converted to a 50% Sodium Soap solution with dilute Sodium Hydroxide by the known soap making methods. This 50% solution is clear liquid at room temperature. The Sodium soap solution is then extracted thrice with 50ml portions of hexane each and the unsaponifiable material is separated. The extraction took 48 hrs due heavy emulsion formation. The aqueous layer is separated and acidified with 50% sulphuric acid and the fatty acid being a liquid separates out above the aqueous layer. Fatty acid is washed with water till free of sulphuric acid. The fatty acid obtained is dried and analyzed for percentage non fatty acid material as % Unsaponifiable Matter and % Non Fatty Acids (by GC).
Example III
7

500 grams of Low & Medium Chain Fatty Acids (fraction containing C6 to C12 fatty acids) having Unsaponifiable Matter = 3.5% and Non Fatty Acids (by GC) = 6.5%, is converted to a 50% Sodium Soap solution with dilute Sodium Hydroxide by the known soap making methods. This 50% solution is clear liquid at room temperature. A clear solution of Calcium Nitrate is prepared and is added to the Sodium soap solution to give a 50% water insoluble Calcium soap solution. The Calcium soap formed precipitates put as a fine, pale, cream solid. After ensuring complete conversion to the Calcium soap the solution is filtered using a Buchner funnel and washed with enough water to free it of Calcium Nitrate and Sodium Hydroxide. The Calcium salt cake thus obtained is split with 50% sulphuric acid and the fatty acid separated. Fatty acid is washed with water till free of sulphuric acid. The fatty acid obtained is dried and analyzed for percentage non fatty acid material as % Unsaponifiable Matter and % Non Fatty Acids (by GC).
Example IV showing Inventive Step
500 grams of Low & Medium Chain Fatty Acids (fraction containing C6 to C12 fatty acids) having Unsaponifiable Matter = 3.5% and Non Fatty Acids (by GC) = 6.5%, is converted to a 50% Sodium Soap solution with dilute Sodium Hydroxide by the known soap making methods. This 50% solution is clear liquid at room temperature. A clear solution of Calcium Nitrate is prepared and is added to the Sodium soap solution to give a 50% water insoluble Calcium soap solution. The Calcium soap formed precipitates out as a fine, pale, cream solid. After ensuring complete conversion to the Calcium soap the solution is filtered using a Buchner funnel and washed with enough water to free it of Calcium Nitrate and Sodium Hydroxide. The Calcium soap thus obtained is extracted with Hexane using soxhlet apparatus, where only 500ml of solvent can be used for each lot. The Calcium salt cake is then split with 50% sulphuric acid to obtain fatty acid. Fatty acid is washed with water till free of sulphuric acid. The fatty acid obtained is dried and analyzed for percentage non fatty acid material as % Unsaponifiable Matter and % Non Fatty Acids (by GC).
8

Measurement
The fatty acid is analyzed for percentage of non fatty acid material by the usual methods of % unsaponifiable matter as well as % non fatty acid peaks by gas chromatography.
Results Table

Unsaponifiable Matter % Non-Fatty-Acid (by GC) %
Example I 3.5 6.5
Example II 1.5 1.8
Example III 0.8 0.8
Example IV 0.14 0.2
9

We Claim:
1. A process for removal of non-fatty acid from fatty acid comprising
the steps of: -
a) reacting said fatty acid with Sodium Hydroxide at 70°C to form a Sodium Soap solution;
b) reacting Sodium Soap solution prepared at step (a) with solution of calcium nitrate at ambient temperatures to obtain calcium salt solution;
c) filtering said calcium salt solution;
d) extracting traces of non fatty acid from said calcium salt;
e) splitting calcium salt cake with acid.

2. A process as claimed in Claim 1, wherein said fatty acids are selected from C6 to C12.
3. A process as claimed in Claim 1, wherein said extraction in step (d) is carried out using hexane at 68°C to 70°C using known soxhlet apparatus for 4 to 8 hours.
4. A process as claimed in Claim 3, wherein said extraction is carried out for 6 hours.
5. A process as claimed in Claim 1, wherein said splitting in step (e) is done using 50% H2SO4 at ambient temperatures.
6. A process as claimed in Claim 1, wherein said Sodium Soap solution in step (a) is diluted to 30 - 60 %.
7. A process as claimed in Claim 6, wherein said Sodium Soap solution is diluted to 50%.
10

8. A process for removal of non-fatty acid from fatty acid substantially described herein with reference to examples.

Dated this 29™ day of March ,2006.

Himanshu W. Kane (Applicants' Patent Agent)
S-3/PATENT/GODREJ/NEW PATENT/REMOVAL OF NON-FATTY ACID/CS NFM REMOVAL FA FINAL
11

ABSTRACT
The present invention relates to process for removal of non-fatty acid from
fatty acid comprising the steps of: a) reacting said fatty acid with Sodium
Hydroxide at 70°C to form a Sodium Soap solution; b) reacting
Sodium Soap solution prepared at step (a) with solution of calcium nitrate
at ambient temperatures to obtain calcium salt solution; c) filtering said
calcium salt solution; d) extracting traces of non fatty acid from said
calcium salt; e) splitting calcium salt cake with acid.
S-3/PATENT/GODREJ/NEW PATENT/REMOVAL OF NON-FATTY ACID/CS NFM REMOVAL FA FINAL
12

Documents:

359-MUM-2005-ABSTRACT 29-3-2005.pdf

359-mum-2005-abstract.doc

359-mum-2005-abstract.pdf

359-MUM-2005-CLAIMS 29-3-2005.pdf

359-mum-2005-claims(granted)-(29-03-2006).doc

359-mum-2005-claims.doc

359-mum-2005-claims.pdf

359-MUM-2005-CORRESPONDENCE 3-7-2008.pdf

359-mum-2005-correspondence(ipo)-(03-12-2008).pdf

359-mum-2005-corrrespondence-received-ver-250405.pdf

359-mum-2005-corrrespondence-received-ver-290305.pdf

359-mum-2005-corrrespondence-received-ver-290306.pdf

359-mum-2005-descripiton (complete).pdf

359-MUM-2005-DESCRIPTION(COMPLETE) 29-3-2005.pdf

359-MUM-2005-FORM 1 29-3-2005.pdf

359-MUM-2005-FORM 18 3-7-2008.pdf

359-mum-2005-form 18(12-09-2006).pdf

359-mum-2005-form 2(granted)-(29-03-2006).doc

359-mum-2005-form 2(granted)-(29-03-2006).pdf

359-MUM-2005-FORM 2(TITLE PAGE) 29-3-2005.pdf

359-mum-2005-form 3(29-03-2005).pdf

359-mum-2005-form 5(29-03-2006).pdf

359-mum-2005-form-1.pdf

359-mum-2005-form-2.doc

359-mum-2005-form-2.pdf

359-mum-2005-form-26.pdf

359-mum-2005-form-3.pdf

359-mum-2005-form-5.pdf

359-MUM-2005-POWER OF ATTORNEY 3-7-2008.pdf

359-mum-2005-power of authority(29-03-2005).pdf

« Previous Patent

Next Patent »

Patent Number

226301

Indian Patent Application Number

359/MUM/2005

PG Journal Number

07/2009

Publication Date

13-Feb-2009

Grant Date

17-Dec-2008

Date of Filing

29-Mar-2005

Name of Patentee

GODREJ CONSUMER PRODUCTS LIMITED

Applicant Address

PIROJSHANAGAR,EASTERN EXPRESS HIGHWAY,VIKHROLI,MUMBAI-400 079.

Inventors:

#	Inventor's Name	Inventor's Address
1	DORDI JIMMY RUSTOM	PIROJSHANAGAR,EASTERN,EXPRESS HIGHWAY,VIKHROLI,MUMBAI-400 079

PCT International Classification Number

C09F8/07

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1			NA