Title of Invention	AN IMPROVED PROCESS FOR THE PREPARATION OF JATROPHA OIL - ACRYLIC CO-POLYMER FOR TANNING APPLICATIONS
Abstract	The present invention relates to an improved process for the preparation of jatropha oil-acrylic co-polymer for tanning applications. More particularly, the present invention relates to graft copolymerization of acrylic polymer onto jatropha oil to obtain a polymer for application in leather processing industry as tanning agent. The product developed under present invention is a tanning as well as lubricating agent for leather. It has also potential application in textile and surface coating industries.

Title of Invention

AN IMPROVED PROCESS FOR THE PREPARATION OF JATROPHA OIL - ACRYLIC CO-POLYMER FOR TANNING APPLICATIONS

Abstract

The present invention relates to an improved process for the preparation of jatropha oil-acrylic co-polymer for tanning applications. More particularly, the present invention relates to graft copolymerization of acrylic polymer onto jatropha oil to obtain a polymer for application in leather processing industry as tanning agent. The product developed under present invention is a tanning as well as lubricating agent for leather. It has also potential application in textile and surface coating industries.

Full Text	FIELD OF THE INVENTION The present invention relates to graft copolymerization of acrylic polymer onto jatropha oil to obtain a polymer for application in leather processing industry as tanning agent. The product developed under present invention is a tanning as well as lubricating agent for leather. It has also potential application in textile and surface coating industries. BACKGROUND OF THE INVENTION Tanning is associated with dehydration of skin fibres. This results in cohesion of fibre bundles resulting in hardening of the leather. Often such process necessitates use of large quantities of lubricating agents in the form of fatliquors, resulting in loading fibres and consequent strength reduction. Use of tanning cum lubricating agents obviates need for such excess use of lubricating agents. Anita Prezepiorkowska (Journal of Indian Leather Technologists Association, November, 1985, pp3-9) prepared a tanning cum lubricating agent by reacting chromium nitrate with palmitic acid. However the major limitation of the product prepared by Anita Prezepiorkowska was only soluble in Iso - propanal and the tanning had to be carried out in Iso-propanol whereas tanning is essentially carried out in aqueous medium. Subsequently Anita Prezepiorkowska developed products, these could be by reacting chromium (III) chloride with ethylene glycol and sulfated pig fat employed in aqueous medium, but this necessitated use of chromium salts for preparation of tanning cum fatliquoring agent (Journal of the Society of Leather Technologists and Chemists, pp82-85, 1993 and Journal of the Society of Leather Technologists and Chemists, pp109-114, 1994), which is a major limitation considering environmental factors. In an attempt to make tanning cum lubricating agent without using chromium Lakshminarayana etal (Journal of American Leather Chemists Association, pp 425-430, 1990) have developed a lubricating and filling agent using sulfated fish oil, alginic acid, acrylic ester and methacrylic acid. The process, however did not yield a tanning agent, but resulted only in retanning agent. The process methodology adopted adversely affected the tanning potential of oil used for polymerisation. The inventors therefore realized that there should be developed a process wherein the tanning potential of the oil should not be lost. Accordingly, the inventiveness of the present invention lies in in-situ polymerization of acrylic monomer and grafting the resulting polymer onto the oil backbone without losing the tanning activity of the oil. OBJECTS OF THE INVENTION The main objective of the present invention is to provide an improved process for the preparation of jatropha oil-acrylic polymer for tanning applications, which obviates the limitations as cited above. Another object of the present invention is to provide a process whereby the product obtained by the said process is aqueous based and hence eco-friendly. Still another object of the present invention is to provide a process which utilizes Jatropha oil as the main constituent, which is a naturally renewable resource. Yet another object of the present invention is to provide a process wherein because of the graft polymerization, consistency problems normally encountered in mixtures and blends of products of similar nature does not arise. SUMMARY OF THE INVENTION Accordingly, the present invention provides an improved process for the preparation of jatropha oil-acrylic co-polymer for tanning applications, which comprises: a) sulfonating jatropha oil using two to three moles of sulfuric acid per mole of jatropha oil at a temperature in the range of 20 to 50° C for 30 to 60 minutes; b) washing the product as obtained in step a) preferably using not more than 30% w/v, of chloride salt of alkali metal and /or alkali earth metal and subsequent adjustment of pH in the range of 6.0 to 8.0 to get sulfonated jatropha oil, c) treating the sulfonated jatropha oil, as obtained in step (b), with 0.5-1.5% of alkali meta bi sulfite, diluted in water in the range of 50-150% w/v, at a temperature of 50 to 80° C, preferably with stirring, for a period in the range of 15-30 minutes, d) reacting the treated sulfonated jatropha oil as obtained in step (c), with 50-100 mole percentage, based on sulfonated jatropha oil, of acrylic monomer having carbon chain length not exceeding C-5, in presence of 0.1 - 0.2 % by wt. of a known initiator, the weight of water being equal to the weight of the acrylic monomer, at a temperature in the range of 60-80 ° C for a period of not less than 2 hrs to get the jatropha oil- acrylic polymer. DETAILED DESCRIPTION OF THE INVENTION The process of the present invention is described below in detail. Jatropha oil is sulfonated using 2-3 moles of sulfuric acid per mole of jatropha oil at a temperature in the range of 20 to 50° C for 30 to 60 minutes by known method and the resulting mixture is subjected to aqueous washing, preferably using not more than 40% w/v, of chloride salt of alkali metal and /or alkali earth metal. pH of the mixture is adjusted in the range of 6.0 to 8.0 by conventional method to get sulfonated jatropha oil. This sulfonated oil is treated with 1-2% of alkali meta bi sulfite, diluted in water in the range of 100 -150 % w/v, at a temperature of 50 to 80° C, preferably with stirring, for a period in the range of 15 -30 mts. The resulting reaction mixture is treated with acrylic monomer having carbon chain length not exceeding C5. The amount of the acrylic monomer ranges between 50-100 mole percentage based on the sulfonated jatropha oil. The polymerization is continued in presence of 0.1 -0.2 % by weight of a known initiator based on the weight of water to dissolve the said initiator. The weight of water is equal to the weight of the acrylic monomer. The reaction is conducted at a temperature in the range of 60-80 ° C for a period not less than 2 hrs to get the jatropha oil- acrylic polymer. In an embodiment of the present invention, the chloride salt used may be selected from sodium chloride, potassium chloride, and calcium chloride. In another embodiment of the present invention, the alkali meta bisulfite used may be selected from sodium meta bi sulfite, potassium bi sulfite. In yet another embodiment of the present invention, the acrylic monomer used may be selected from Methacrylic acid, Acrylic acid, Methyl acrylate, Ethyl acrylate, Butyl acrylate, Methyl methacrylate. In still another embodiment of the present invention, the initiator used may be selected from potassium per sulfate, benzoyl peroxide. The following examples are given by way of illustration only and therefore should not be construed to limit the scope of the present invention Example -1 20 grams of concentrated sulphuric acid was added to 100 grams of Jatropha oil with constant stirring over a period of 30 minutes maintaining the temperature at 50°C. 100 ml of aqueous sodium chloride containing 20 gm of the salt was then added. The stirring was stopped and the contents were allowed to separate. The supernatant oil layer was collected in a beaker. Aqueous sodium hydroxide containing 20 gm of the alkali in 100 ml water was added to neutralize to pH 6.0 to get sulfonated Jatropha oil. 10 gram of sulfonated Jatropha oil was taken in a three necked flask. A mechanical stirrer was attached in the central neck with two dropping funnels on both sides. 0.5 gram of sodium metabisulphate dissolved in 50 ml of water was added to it at a temperature of 50 ° C and stirred for a period of 15 minutes. In one dropping funnel, 50 gm of Methacrylic acid was taken. In the other dropping funnel, 50 g of water containing 0.05 gm of potassium persulphate was taken. Both were added drop wise, with brisk stirring over a period of 60 minutes. The temperature was maintained at 50°C and the stirring was continued at the same temperature for another 60 minutes to get Jatropha oil acrylate co- polymer. Example 2 25 grams of concentrated sulphuric acid was added to 100 grams of Jatropha oil with constant stirring over a period of 40 minutes maintaining the temperature at 40°C. 100 ml of aqueous sodium chloride containing 25 grams of the salt was then added. The stirring was stopped and the contents were allowed to separate. The supernatant oil layer was collected in a beaker. Aqueous sodium hydroxide containing 25 gram of the alkali in 100 ml water was added to neutralize to pH 6.5 to get sulfonated Jatropha oil. 25 gram of sulfonated Jatropha oil was taken in a three necked flask. A mechanical stirrer was attached in the central neck with two dropping funnels on both sides. 1.25 gram of potassium metabisulphate dissolved in 125 ml of water was added to it at a temperature of 60°C and stirred for a period of 20 minutes. In one dropping funnel, 30 grams of Methacrylic acid and 30 gm of acrylic acid were taken. In the other dropping funnel, 60 g of water containing 0.1 gram of potassium persulphate was taken. Both were added drop wise, with brisk stirring over a period of 75 minutes. The temperature was maintained at 60°C and the stirring was continued at the same temperature for another 90 minutes to get Jatropha oil acrylate co-polymer. Example 3 30 grams of concentrated sulphuric acid was added to 100 grams of Jatropha oil with constant stirring over a period of 45 minutes maintaining the temperature at 35°C. 100 ml of aqueous sodium chloride containing 30 grams of the salt was then added. The stirring was stopped and the contents were allowed to separate. The supernatant oil layer was collected in a beaker. Aqueous sodium hydroxide containing 30 gram of the alkali in 100 ml water was added to neutralize to pH 7.0 to get sulfonated Jatropha oil. 30 gram of sulfonated Jatropha oil was taken in a three necked flask. A mechanical stirrer was attached in the central neck with two dropping funnels on both sides. 1.5 gram of sodium metabisulphate dissolved in 150 ml of water was added to it at a temperature of 70°C and stirred for a period of 25 minutes. In one dropping funnel, 30 grams of Methacrylic acid and 20 gms of butyl acrylate were taken. In the other dropping funnel, 50 g of water containing 0.1 gram of potassium persulphate was taken. Both were added drop wise, with brisk stirring over a period of 60 minutes. The temperature was maintained at 65°C and the stirring was continued at the same temperature for another 120 minutes to get Jatropha oil acrylate co-polymer. Example 4 30 grams of concentrated sulphuric acid was added to 100 grams of Jatropha oil with constant stirring over a period of 45 minutes maintaining the temperature at 30° C. 100 ml of aqueous sodium chloride containing 35 grams of the salt was then added. The stirring was stopped and the contents were allowed to separate. The supernatant oil layer was collected in a beaker. Aqueous sodium hydroxide containing 35 gram of the alkali in 100 ml water was added to neutralize to pH 7.5 to get sulfonated Jatropha oil, 50 gram of sulfonated Jatropha oil was taken in a three necked flask. A mechanical stirrer was attached in the central neck with two dropping funnels on both sides. 1.5 gram of potassium metabisulphate dissolved in 150 ml of water was added to it at a temperature of 80 ° C and stirred for a period of 30 minutes. In one dropping funnel, 60 gm of Methyl methacrylate was taken. In the other dropping funnel, 60 g of water containing 0.1 gram of potassium persulphate was taken. Both were added drop wise, with brisk stirring over a period of 60 minutes. The temperature was maintained at 70°C and the stirring was continued at the same temperature for another 90 minutes to get Jatropha oil acrylate co-polymer. Example 5 30 grams of concentrated sulphuric acid was added to 100 grams of Jatropha oil with constant stirring over a period of 60 minutes maintaining the temperature at 20°C. 100 ml of aqueous sodium chloride containing 30 grams of the salt was then added. The stirring was stopped and the contents were allowed to separate. The supernatant oil layer was collected in a beaker. Aqueous sodium hydroxide containing 40 gram of the alkali in 100 ml water was added to neutralize to pH 8.0 to get sulfonated Jatropha oil. 90 gram of the product was taken in a three necked flask. A mechanical stirrer was attached in the central neck with two dropping funnels on both sides. 1.5 gram of sodium metabisulphate dissolved in 150 ml of water was added to it at a temperature of 70 ° C and stirred for a period of 30 minutes. In one dropping funnel, 40 grams of Methacrylate, 20 gm of ethyl acrylate and 20 gm of butyl acrylate were taken. In the other dropping funnel, 80 g of water containing 0.15 gram of potassium persulphate was taken. Both were added drop wise, with brisk stirring over a period of 90 minutes. The temperature was maintained at 80°C and the stirring was continued at the same temperature for another 120 minutes to get Jatropha oil acrylate co-polymer. ADVANTAGES OF THE INVENTION 1. It is a simple process. 2. The product obtained by the process described is aqueous based and hence eco friendly. 3. Jatropha oil, the main constituent, is a naturally renewable resource. 4. Because of the graft polymerization, consistency problems normally encountered in mixtures and blends of products of similar nature does not arise. We claim: 1. An improved process for the preparation of jatropha oil-acrylic co-polymer for tanning applications, which comprises a) sulfonating jatropha oil using two to three moles of sulfuric acid per mole of jatropha oil at a temperature in the range of 20 to 50° C for 30 to 60 minutes; b) washing the product as obtained in step a) preferably using not more than 30% w/v, of chloride salt of alkali metal and /or alkali earth metal and subsequent adjustment of pH in the range of 6.0 to 8.0 to get sulfonated jatropha oil, c) treating the sulfonated jatropha oil, as obtained in step (b), with 0.5-1.5% of alkali meta bi sulfite, diluted in water in the range of 50-150% w/v, at a temperature of 50 to 80° C, preferably with stirring, for a period in the range of 15-30 minutes, d) reacting the treated sulfonated jatropha oil as obtained in step (c), with 50-100 mole percentage, based on sulfonated jatropha oil, of acrylic monomer having carbon chain length not exceeding C-5, in presence of 0.1 - 0.2 % by wt. of a known initiator, the weight of water being equal to the weight of the acrylic monomer, at a temperature in the range of 60-80 0 C for a period of not less than 2 hrs to get the jatropha oil- acrylic polymer. 2.An improved process as claimed in claim 1, wherein the chloride salt is selected from sodium chloride, potassium chloride, and calcium chloride. 3.An improved process as claimed in claims 1 and 2, wherein the alkali meta bisulfite is selected from sodium meta bi sulfite, potassium bi sulfite. 4.An improved process as claimed in claims 1 to 3, wherein the acrylic monomer is selected from Methacrylic acid, Acrylic acid, Methyl acrylate, Ethyl acrylate, Butyl acrylate, Methyl methacrylate. 5.An improved process as claimed in claims 1 to 4, wherein the initiator is selected from pottasium per sulfate, benzoyl peroxide

Full Text

FIELD OF THE INVENTION
The present invention relates to graft copolymerization of acrylic polymer onto jatropha oil to obtain a polymer for application in leather processing industry as tanning agent. The product developed under present invention is a tanning as well as lubricating agent for leather. It has also potential application in textile and surface coating industries.
BACKGROUND OF THE INVENTION
Tanning is associated with dehydration of skin fibres. This results in cohesion of fibre bundles resulting in hardening of the leather. Often such process necessitates use of large quantities of lubricating agents in the form of fatliquors, resulting in loading fibres and consequent strength reduction. Use of tanning cum lubricating agents obviates need for such excess use of lubricating agents.
Anita Prezepiorkowska (Journal of Indian Leather Technologists Association, November, 1985, pp3-9) prepared a tanning cum lubricating agent by reacting chromium nitrate with palmitic acid. However the major limitation of the product prepared by Anita Prezepiorkowska was only soluble in Iso - propanal and the tanning had to be carried out in Iso-propanol whereas tanning is essentially carried out in aqueous medium. Subsequently Anita Prezepiorkowska developed products, these could be by reacting chromium (III) chloride with ethylene glycol and sulfated pig fat employed in aqueous medium, but this necessitated use of chromium salts for preparation of tanning cum fatliquoring agent (Journal of the Society of Leather Technologists and Chemists, pp82-85, 1993 and Journal of the Society of Leather Technologists and Chemists, pp109-114, 1994), which is a major limitation considering environmental factors. In an attempt to make tanning cum lubricating agent without using chromium Lakshminarayana etal (Journal of American Leather Chemists Association, pp 425-430, 1990) have developed a lubricating and filling agent using sulfated fish oil, alginic acid, acrylic ester and methacrylic acid. The process, however did not yield a tanning agent, but resulted only in
retanning agent. The process methodology adopted adversely affected the tanning potential of oil used for polymerisation.
The inventors therefore realized that there should be developed a process wherein the tanning potential of the oil should not be lost. Accordingly, the inventiveness of the present invention lies in in-situ polymerization of acrylic monomer and grafting the resulting polymer onto the oil backbone without losing the tanning activity of the oil.
OBJECTS OF THE INVENTION
The main objective of the present invention is to provide an improved process for the preparation of jatropha oil-acrylic polymer for tanning applications, which obviates the limitations as cited above.
Another object of the present invention is to provide a process whereby the
product obtained by the said process is aqueous based and hence eco-friendly. Still another object of the present invention is to provide a process which utilizes Jatropha oil as the main constituent, which is a naturally renewable resource. Yet another object of the present invention is to provide a process wherein because of the graft polymerization, consistency problems normally encountered in mixtures and blends of products of similar nature does not arise.
SUMMARY OF THE INVENTION Accordingly, the present invention provides an improved process for the preparation of jatropha oil-acrylic co-polymer for tanning applications, which comprises: a) sulfonating jatropha oil using two to three moles of sulfuric acid per mole of jatropha oil at a temperature in the range of 20 to 50° C for 30 to 60 minutes;
b) washing the product as obtained in step a) preferably using not more
than 30% w/v, of chloride salt of alkali metal and /or alkali earth metal

and subsequent adjustment of pH in the range of 6.0 to 8.0 to get sulfonated jatropha oil,
c) treating the sulfonated jatropha oil, as obtained in step (b), with 0.5-1.5% of alkali meta bi sulfite, diluted in water in the range of 50-150% w/v, at a temperature of 50 to 80° C, preferably with stirring, for a period in the range of 15-30 minutes,
d) reacting the treated sulfonated jatropha oil as obtained in step (c), with 50-100 mole percentage, based on sulfonated jatropha oil, of acrylic monomer having carbon chain length not exceeding C-5, in presence of 0.1 - 0.2 % by wt. of a known initiator, the weight of water being equal to the weight of the acrylic monomer, at a temperature in the range of 60-80 ° C for a period of not less than 2 hrs to get the jatropha oil- acrylic polymer.
DETAILED DESCRIPTION OF THE INVENTION
The process of the present invention is described below in detail. Jatropha oil is sulfonated using 2-3 moles of sulfuric acid per mole of jatropha oil at a temperature in the range of 20 to 50° C for 30 to 60 minutes by known method and the resulting mixture is subjected to aqueous washing, preferably using not more than 40% w/v, of chloride salt of alkali metal and /or alkali earth metal. pH of the mixture is adjusted in the range of 6.0 to 8.0 by conventional method to get sulfonated jatropha oil. This sulfonated oil is treated with 1-2% of alkali meta bi sulfite, diluted in water in the range of 100 -150 % w/v, at a temperature of 50 to 80° C, preferably with stirring, for a period in the range of 15 -30 mts. The resulting reaction mixture is treated with acrylic monomer having carbon chain length not exceeding C5. The amount of the acrylic monomer ranges between 50-100 mole percentage based on the
sulfonated jatropha oil. The polymerization is continued in presence of 0.1 -0.2 % by weight of a known initiator based on the weight of water to dissolve the said initiator. The weight of water is equal to the weight of the acrylic monomer. The reaction is conducted at a temperature in the range of 60-80 ° C for a period not less than 2 hrs to get the jatropha oil- acrylic polymer.
In an embodiment of the present invention, the chloride salt used may be selected from sodium chloride, potassium chloride, and calcium chloride.
In another embodiment of the present invention, the alkali meta bisulfite used may be selected from sodium meta bi sulfite, potassium bi sulfite.
In yet another embodiment of the present invention, the acrylic monomer used may be selected from Methacrylic acid, Acrylic acid, Methyl acrylate, Ethyl acrylate, Butyl acrylate, Methyl methacrylate.
In still another embodiment of the present invention, the initiator used may be selected from potassium per sulfate, benzoyl peroxide.
The following examples are given by way of illustration only and therefore should not be construed to limit the scope of the present invention
Example -1
20 grams of concentrated sulphuric acid was added to 100 grams of Jatropha oil with constant stirring over a period of 30 minutes maintaining the temperature at 50°C. 100 ml of aqueous sodium chloride containing 20 gm of the salt was then added. The stirring was stopped and the contents were allowed to separate. The supernatant oil layer was collected in a beaker. Aqueous sodium hydroxide containing 20 gm of the alkali in 100 ml water was added to neutralize to pH 6.0 to get sulfonated Jatropha oil.
10 gram of sulfonated Jatropha oil was taken in a three necked flask. A mechanical stirrer was attached in the central neck with two dropping funnels on both sides. 0.5 gram of sodium metabisulphate dissolved in 50 ml of water

was added to it at a temperature of 50 ° C and stirred for a period of 15 minutes. In one dropping funnel, 50 gm of Methacrylic acid was taken. In the other dropping funnel, 50 g of water containing 0.05 gm of potassium persulphate was taken. Both were added drop wise, with brisk stirring over a period of 60 minutes. The temperature was maintained at 50°C and the stirring was continued at the same temperature for another 60 minutes to get Jatropha oil acrylate co- polymer.
Example 2
25 grams of concentrated sulphuric acid was added to 100 grams of Jatropha oil with constant stirring over a period of 40 minutes maintaining the temperature at 40°C. 100 ml of aqueous sodium chloride containing 25 grams of the salt was then added. The stirring was stopped and the contents were allowed to separate. The supernatant oil layer was collected in a beaker. Aqueous sodium hydroxide containing 25 gram of the alkali in 100 ml water was added to neutralize to pH 6.5 to get sulfonated Jatropha oil.
25 gram of sulfonated Jatropha oil was taken in a three necked flask. A mechanical stirrer was attached in the central neck with two dropping funnels on both sides. 1.25 gram of potassium metabisulphate dissolved in 125 ml of water was added to it at a temperature of 60°C and stirred for a period of 20 minutes. In one dropping funnel, 30 grams of Methacrylic acid and 30 gm of acrylic acid were taken. In the other dropping funnel, 60 g of water containing 0.1 gram of potassium persulphate was taken. Both were added drop wise, with brisk stirring over a period of 75 minutes. The temperature was maintained at 60°C and the stirring was continued at the same temperature for another 90 minutes to get Jatropha oil acrylate co-polymer.
Example 3
30 grams of concentrated sulphuric acid was added to 100 grams of Jatropha oil with constant stirring over a period of 45 minutes maintaining the temperature at 35°C. 100 ml of aqueous sodium chloride containing 30 grams of the salt was then added. The stirring was stopped and the contents were

allowed to separate. The supernatant oil layer was collected in a beaker. Aqueous sodium hydroxide containing 30 gram of the alkali in 100 ml water was added to neutralize to pH 7.0 to get sulfonated Jatropha oil.
30 gram of sulfonated Jatropha oil was taken in a three necked flask. A mechanical stirrer was attached in the central neck with two dropping funnels on both sides. 1.5 gram of sodium metabisulphate dissolved in 150 ml of water was added to it at a temperature of 70°C and stirred for a period of 25 minutes. In one dropping funnel, 30 grams of Methacrylic acid and 20 gms of butyl acrylate were taken. In the other dropping funnel, 50 g of water containing 0.1 gram of potassium persulphate was taken. Both were added drop wise, with brisk stirring over a period of 60 minutes. The temperature was maintained at 65°C and the stirring was continued at the same temperature for another 120 minutes to get Jatropha oil acrylate co-polymer.
Example 4
30 grams of concentrated sulphuric acid was added to 100 grams of Jatropha oil with constant stirring over a period of 45 minutes maintaining the temperature at 30° C. 100 ml of aqueous sodium chloride containing 35 grams of the salt was then added. The stirring was stopped and the contents were allowed to separate. The supernatant oil layer was collected in a beaker. Aqueous sodium hydroxide containing 35 gram of the alkali in 100 ml water was added to neutralize to pH 7.5 to get sulfonated Jatropha oil,
50 gram of sulfonated Jatropha oil was taken in a three necked flask. A mechanical stirrer was attached in the central neck with two dropping funnels on both sides. 1.5 gram of potassium metabisulphate dissolved in 150 ml of water was added to it at a temperature of 80 ° C and stirred for a period of 30 minutes. In one dropping funnel, 60 gm of Methyl methacrylate was taken. In the other dropping funnel, 60 g of water containing 0.1 gram of potassium persulphate was taken. Both were added drop wise, with brisk stirring over a period of 60 minutes. The temperature was maintained at 70°C and the stirring

was continued at the same temperature for another 90 minutes to get Jatropha oil acrylate co-polymer.
Example 5
30 grams of concentrated sulphuric acid was added to 100 grams of Jatropha oil with constant stirring over a period of 60 minutes maintaining the temperature at 20°C. 100 ml of aqueous sodium chloride containing 30 grams of the salt was then added. The stirring was stopped and the contents were allowed to separate. The supernatant oil layer was collected in a beaker. Aqueous sodium hydroxide containing 40 gram of the alkali in 100 ml water was added to neutralize to pH 8.0 to get sulfonated Jatropha oil.
90 gram of the product was taken in a three necked flask. A mechanical stirrer was attached in the central neck with two dropping funnels on both sides. 1.5 gram of sodium metabisulphate dissolved in 150 ml of water was added to it at a temperature of 70 ° C and stirred for a period of 30 minutes. In one dropping funnel, 40 grams of Methacrylate, 20 gm of ethyl acrylate and 20 gm of butyl acrylate were taken. In the other dropping funnel, 80 g of water containing 0.15 gram of potassium persulphate was taken. Both were added drop wise, with brisk stirring over a period of 90 minutes. The temperature was maintained at 80°C and the stirring was continued at the same temperature for another 120 minutes to get Jatropha oil acrylate co-polymer.
ADVANTAGES OF THE INVENTION
1. It is a simple process.
2. The product obtained by the process described is aqueous based and
hence eco friendly.
3. Jatropha oil, the main constituent, is a naturally renewable resource.
4. Because of the graft polymerization, consistency problems normally
encountered in mixtures and blends of products of similar nature does
not arise.

We claim:
1. An improved process for the preparation of jatropha oil-acrylic co-polymer
for tanning applications, which comprises
a) sulfonating jatropha oil using two to three moles of sulfuric acid per mole of
jatropha oil at a temperature in the range of 20 to 50° C for 30 to 60
minutes;
b) washing the product as obtained in step a) preferably using not more than 30% w/v, of chloride salt of alkali metal and /or alkali earth metal and subsequent adjustment of pH in the range of 6.0 to 8.0 to get sulfonated jatropha oil,
c) treating the sulfonated jatropha oil, as obtained in step (b), with 0.5-1.5% of alkali meta bi sulfite, diluted in water in the range of 50-150% w/v, at a temperature of 50 to 80° C, preferably with stirring, for a period in the range of 15-30 minutes,
d) reacting the treated sulfonated jatropha oil as obtained in step (c), with 50-100 mole percentage, based on sulfonated jatropha oil, of acrylic monomer having carbon chain length not exceeding C-5, in presence of 0.1 - 0.2 % by wt. of a known initiator, the weight of water being equal to the weight of the acrylic monomer, at a temperature in the range of 60-80 0 C for a period of not less than 2 hrs to get the jatropha oil- acrylic polymer.
2.An improved process as claimed in claim 1, wherein the chloride salt is selected from sodium chloride, potassium chloride, and calcium chloride.

3.An improved process as claimed in claims 1 and 2, wherein the alkali meta
bisulfite is selected from sodium meta bi sulfite, potassium bi sulfite.
4.An improved process as claimed in claims 1 to 3, wherein the acrylic
monomer is selected from Methacrylic acid, Acrylic acid, Methyl acrylate,
Ethyl acrylate, Butyl acrylate, Methyl methacrylate.
5.An improved process as claimed in claims 1 to 4, wherein the initiator is
selected from pottasium per sulfate, benzoyl peroxide

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Patent Number

258248

Indian Patent Application Number

663/DEL/2006

PG Journal Number

52/2013

Publication Date

27-Dec-2013

Grant Date

20-Dec-2013

Date of Filing

10-Mar-2006

Name of Patentee

COUNCIL OF SCIENTIFIC & INDUSTRIAL RESEARCH

Applicant Address

ANUSANDHAN BHAWAN, RAFI MARG, NEW DELHI-110001, INDIA.

Inventors:

#	Inventor's Name	Inventor's Address
1	POLUR KRISHNIAH	CENTRAL LEATHER RESEARCH INSTITUTE, CHENNAI.
2	VENKATESWARAN HARI BABU	CENTRAL LEATHER RESEARCH INSTITUTE, CHENNAI.
3	CHELIAPPA MURALIDHARAN	CENTRAL LEATHER RESEARCH INSTITUTE, CHENNAI..
4	BOREDDY SIVA RAMI REDDY	CENTRAL LEATHER RESEARCH INSTITUTE, CHENNAI.

PCT International Classification Number

C08F 2/00

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1			NA