Title of Invention	A PROCESS FOR THE PREPARATION OF A PROTEINOID-ACRYLATE COMPOSITE HAVING MOLECULAR WEIGHT IN THE RANGE OF 15000-20000 KD
Abstract	The process provides a method of copolymerisation of protein hydrolysate with acrylic resin of molecular weight in the range of 12000-15000 KD to prepare a composite of molecular weight in the range of 15000-20000 KD, having enormous potential application as high exhaustion syntan in leather processing, thereby suggesting not only an economical option for utilising the proteinous wastes of different industries including leather industry in useful way, but also an eco-friendly measure for leather processing using the resulting product of the present invention.

Title of Invention

A PROCESS FOR THE PREPARATION OF A PROTEINOID-ACRYLATE COMPOSITE HAVING MOLECULAR WEIGHT IN THE RANGE OF 15000-20000 KD

Abstract

The process provides a method of copolymerisation of protein hydrolysate with acrylic resin of molecular weight in the range of 12000-15000 KD to prepare a composite of molecular weight in the range of 15000-20000 KD, having enormous potential application as high exhaustion syntan in leather processing, thereby suggesting not only an economical option for utilising the proteinous wastes of different industries including leather industry in useful way, but also an eco-friendly measure for leather processing using the resulting product of the present invention.

Full Text	The present invention relates to a process for the preparation of a proteinoid-acrylate composite having molecular weight in the range of 15000-20000 KD. More particularly, the present invention relates to a process for the preparation of a proteinoid-acrylate composite for application as filler-cum-syntan in leather processing industry. The syntan of the present invention has potential application in post tanning wet processing section of leather processing industry to get filling effect, grain tightness and softness in the processed leather. The composite may also be used as filler in cardboard industry. One of the important operations, leathers are subjected to during the post tanning wet operations is retanning, which has a major role to play in connection with tightness, fullness and softness of the final leather. Different syntans are conventionally used for this purpose depending on the requirement of properties and end uses of the final leather. Retanning syntans have usually been of non-proteinous nature. They may in general be classified into two broad categories - phenolic syntan and resin syntan. Phenolic syntans are essentially phenol/ cresol/napthol/formaldehyde containing acid derivatives, which can partially or completely replace vegetable tanning materials for imparting tanning effect. Hence, they are also known as replacement syntans. The phenolic syntans exhibit better filling effect in leather and also result in better nap in suede leather. The main limitation of these syntans lies in poor degradability as well as poor exhaustion in the range of 50-60% during dyeing, thereby adding to the effluent problem by way of increasing total dissolved solids of the waste water. Resin syntans are essentially the sodium or ammonium salts of different resins, other than those, of phenol formaldehyde types. Resins of urea, dicyanamide, melamine etc., with formaldehyde or resins of acrylic and methacrylic acids, di-isocyanates, dialdehyde have generally been of much use. These syntans not only posses tanning properties, but also exhibit selective filling effect to ensure that the looseness of the leathers is removed. Thus these syntans provide uniformity, softness and grain tightness to the leather. As reported by Ludvik, (United Nations Industrial Development Organization, Report, 1,24,1996), the limitation associated with these syntans of poor exhaustion to the tune of maximum 60% during dyeing of leather, thereby adding to the effluent problem. Another major limitation associated with the resin syntans is that they are not stable at a temperature of more than 80°C, thereby rendering them unsuitable for producing leathers to be glaze finished. The above limitations of the conventional resin syntans have prompted the researchers to look for better option in the realm of leather syntan. Ramamurthy et al (Journal of Society of Leather Technologists and Chemists, 73,168,1989) provided a process for preparing keratin hydrolysate for using as protein based syntan in leather processing, whereby the keratinous protein is hydrolysed by using acid or alkali. Conventionally, the acid hydrolysis of protein is carried out at a pH in the range of 1-2, while alkali hydrolysis is done at a pH in the range of 10-12. While the keratin hydrolysate, as prepared above, is effective in improving the exhaustibility of dye or chrome to the tune of 85-90%, the major limitation associated therewith is the lack of filling effect in the final leather, thereby exhibiting no improvement on grain tightness. Another limitation associated with the keratin hydrolysate is that it can be stored for a maximum period of 6 months only because of its proteinous nature, which results in its decaying tendency. No prior art is available on any protein-resin combination product. The main object of the present invention is to provide a process for the preparation of a novel proteinoid-acrylate composite having molecular weight in the range of 15000-20000 KD, which obviates the drawbacks stated above. Another object of the present invention is to provide a process for the preparation of a composite having thermo-tolerance more than 150°C. Yet another object of the present invention is to provide a process for the preparation of a composite, which can be stored for a period of minimum 1year. Still another object of the present invention is to provide a process for the economical use- of the abundantly available proteinous wastes to prepare proteinoid-acrylate composite. Yet another object of the present invention is to provide a process for preparing a composite, which on being used in leather processing, imparts grain tightness in leather and ensures better nap in suede leather, exhibiting at the same time an exhaustability of more than 98% in dye bath. Accordingly the present invention provides a process for the preparation of a proteinoid-acrylate composite having molecular weight in the range of 15000-20000 KD, which comprises i. aqueous washing of a proteinous material such as herein describeddby known method followed by conventional acid or alkali hydrolysis for a period of minimum 30 minutes and subsequent sterilisation of the resulting hydrolysate by known method, ii. separating the sterilised protein hydrolysate, as formed in step (i) by known method and adjusting the pH of the resulting solution in the range of 4.5 - 6 by conventional method, iii. treating the resulting solution with 10-30% v/v, of an acrylic polymer of molecular weight in the range of 12000-15000 KD for a period of minimum 30 minutes, followed by optional addition of 0.01-0.1% w/v antimicrobial agent,'such as herein described to get the proteinoid-acrylate composite. In an embodiment of the present invention, the source of proteinous material used may be hide, skin, fleshing, buffing dust, shaving dust, leather trimmings, animal hair. In another embodiment of the present invention, the known method of sterilisation used may be autoclaving, Ultraviolet radiation, refrigeration. In yet another embodiment of the present invention, the known method of separation used may be filtration, centrifuging, gravity separation. In still another embodiment of the present invention, the acrylate polymer used may be such as methyl acrylate, ethyl acrylate, propyl acrylate, butyl acrylate. In yet another embodiment of the present invention, the antimicrobial agent used may be such as parachloro meta cresol, ortho phenyl phenol, thio cyano thio methyl thio benzo thiozole, either individually or in combination. The process of the present invention is described below in detail. A proteinous source is washed well in aqueous medium to remove the adhering extraneous materials and the washed stock is subjected to either acid or alkali hydrolysis by conventional method for a period of minimum 30 minutes. While acid hydrolysis is carried out at a pH in the range of 1-2, alkali hydrolysis is carried out at a pH in the range of 10-12. The resulting protein hydrolysate is sterilised by known method and the sterilised solution is subjected to separation by known method to get the pure protein hydrolysate solution. pH of the pure protein hydrolysate solution, as obtained above, is adjusted in the range of 4.5-6 by conventional method and the resulting solution is treated with 10-30% v/v, of an acrylic polymer of molecular weight in the range of 12000-15000 KD, for a period of minimum 30 minutes under stirring condition to get the proteinoid-acrylate composite. 0.01-0.1% v/v, of antimicrobial agent is then added, as an optional step, to the resulting mass for storage. The novelty and non-obviousness of the present invention lies in copolymerising a protein hydrolysate with acrylic resin to prepare a substrate exhibiting the desirable characteristics, which are otherwise difficult to be achieved using either protein based syntan or acrylic syntan individually, thereby suggesting at the same time an economical option for utilizing the proteinous wastes of different industries including leather industry in useful way. 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 1 Kg of hide fleshing, collected from the lime yard of a tannery, was washed thoroughly with plain water to remove all the extraneous matters. The washed stock was then taken in a round bottomed flask and 3 litres of water was added to it. 44 gms of solid NaOH pellets were then added slowly to the flask with continuous stirring, which was continued for another 30 min. At this stage, pH of the solution inside the flask was noted to be 10 and the mouth of the flask was plugged with non-absorbent cotton. The flask was then autoclaved at a pressure of 1 Kg psi. After a period of three hours the flask was taken out of the autoclave and was allowed to cool down to a temperature of 25°C. The flask was then unplugged and the solution inside was filtered using filter paper. The solution was collected in a beaker and pH of the solution was found to be 11 which was brought down to 5.5 by adding 100 ml of dilute HCI. 200 ml of methyl acrylate having molecular weight of 12000 KD was added to the beaker with continuous stirring. After a period of 15 minutes, 0.5 gm of para chloro meta cresol with 0.5 gm of ortho-phenyl phenol were added to the beaker under stirring condition and the resulting solution of the proteinoid-acrylate composite was stored in a plastic container. The proteinoid-acrylate solution was used in retanning at a feed of 10% on shaved weight for cow upper leather and was found to exhibit good filling to the resulting leather. Example 2 1 Kg of buffing dust, collected from the buffing yard of a tannery, was washed thoroughly with ammoniacal water to remove all the extraneous matters. The washed stock was then taken in a round bottomed flask and 3 litres of water was added to it.'40 gms of solid NaOH pellets were then added slowly to the flask with continuous stirring, which was continued for another 45 min. At this stage, pH of the solution inside the flask was noted to be 10 and the mouth of the flask was plugged with non-absorbent cotton. The flask was then exposed to UV radiation in a wooden chamber. After a period of 3 hours the flask was taken out of the chamber and was unplugged. The solution inside the flask was then centrifuged and the supernatant was taken out in a beaker. pH of the suprnatant was found to be 11.2 which was brought down to 5.0 by adding 90 ml of dilute HCI. 200 ml of ethyl acrylate having molecular weight of 14000 KD was added to the beaker with continuous stirring. After a period of 15 minutes, 1 gm of ortho phenyl phenol was added to the beaker under stirring condition and the resulting solution of the proteinoid-acrylate composite was stored in a plastic container. The proteinoid-acrylate solution was used in retanning at a feed of 10% on shaved weight for cow upper leather and was found to exhibit improved glaze finish to the resulting leather. Example 3 1 Kg of shaving dust, collected from the shaving yard of a tannery, was washed thoroughly with ammoniacal water to remove all the extraneous matters. The washed stock was then taken in a round-bottomed flask and 3 litres of water was added to it. 100 ml of HCI was then added slowly to the flask with continuous stirring, which was continued for another 40 min. At this stage, pH of the solution inside the flask was noted to be 1 and the mouth of the flask was plugged with non-absorbent cotton. The flask was then sterilised by refrigeration method at temperature of 1°C for 5 hours. After a period of five hours the flask was taken out of the refrigeration . The flask was then unplugged and the solution inside was filtered using filter paper. The solution was collected in a beaker and pH of the solution was found to be 10.5 which was brought down to 5.5 by adding 150 gm of sodium acetate. 200 ml of butyl acrylate having molecular weight of 15000 KD was added to the beaker with continuous stirring. After a period of 15 minutes, 1 gm of thio cyano thio methyl thio benzo thiozole was added to the beaker under stirring condition and the resulting solution of the proteinoid-acrylate composite was stored in a plastic container. The proteinoid-acrylate solution was used in retanning at a feed of 10% on shaved weight for cow upper leather and was found to exhibit good filling to the resulting leather. Example 4 1 Kg of learther trimmings, collected from the tannery, was washed thoroughly with plain water to remove all the extraneous matters. The washed stock was then taken taken in a round bottomed flask and 3 litres of water was added to it. 44 gms of solid NaOH pellets were then added slowly to the flask with continuous stirring, which was continued for another 60 min. At this stage, pH of the solution inside the flask was noted to be 10 and the mouth of the flask was plugged with non-absorbent cotton. The flask was then autoclaved at a pressure of 1 Kg psi. After a period of four hours the flask was taken out of the autoclave and was allowed to cool down to a temperature of 29°C. The flask was then unplugged and the solution inside was subjected to gravity separation. The supernatant was collected in a beaker and pH of the solution was found to be 11 which was brought down to 5.5 by adding 95 ml of dilute HCI. 200 ml of propyl acrylate having molecular weight of 12000 KD was added to the beaker with continuous stirring. After a period of 15 minutes, 0.75 gm of para chloro meta cresol was added to the beaker under stirring condition and the resulting solution of the proteinoid-acrylate composite was stored in a plastic container. The proteinoid-acrylate solution was used in retanning at a feed of 10% on shaved weight for cow upper leather and was found to exhibit good filling to the resulting leather Example 5 1 Kg of animal hair, collected from the lime yard of tannery, was washed thoroughly with plain water to remove all the extraneous matters. The washed stock was then taken in a round bottomed flask and 3 litres of water was added to it. 44 gms of solid NaOH pellets were then added slowly to the flask with continuous stirring, which was continued for another 90 min. At this stage, pH of the solution inside the flask was noted to be 10 and the mouth of the flask was plugged with non-absorbent cotton. The flask was then autoclaved at a pressure of 1 Kg psi. After a period of three hours the flask was taken out of the autoclave and was allowed to cool down to a temperature of 24°C. The flask was then unplugged and the solution inside was filtered using filter paper. The solution was collected in a beaker and pH of the solution was found to be 11 which was brought down to 5.5 by adding 90 ml of dilute HCI. 200 ml of butyl acrylate having molecular weight of 15000 KD was added to the beaker with continuous stirring. After a period of 15 minutes, 5 gms of thio cyano thio methyl thio benzo thiozole was added to the beaker under stirring condition and the resulting solution of the proteinoid-acrylate composite was stored in a plastic container. The proteinoid-acrylate solution was used in retanning at a feed of 10% on shaved weight for cow upper leather and was found to exhibit good filling to the resulting leather The main advantages of the present invention are the following. 1. The process involves no difficult control parameters and hence it is easy to operate. 2. It provides a process to use the hydrolysable proteinous wastes, which otherwise create major disposal problem, for making auxiliaries for different industries including leather processing industry, thereby reducing the load of environmental pollution. 3. The composite prepared by the process of the present invention can withstand a temperature upto 200°C and hence it can be used for the processing of glazed finished leathers. 4. The composite prepared by the process of the present invention results in grain tightening and ensures that the resulting leather is more amenable to buffing not only for making corrected grain leathers, but also for getting good nap while making suede leathers. 5. The composite ensures exhaustion of dye bath to the tune of 98%. 6. The product exhibits a shelf life of one year. We claim : 1. A process for the preparation of proteinoid-acrylate composite having molecular weight in the range of 15000-20000 KD, which comprises : i. aqueous washing of a proteinous material such as herein described by known method followed by conventional acid or alkali hydrolysis for a period of minimum 30 minutes and subsequent sterilization of the resulting hydrolysate by known method, ii. separating the sterilized solution, as formed in step (i) by known method and adjusting the pH of the resulting solution in the range of 4.5-6 by conventional method, iii. charaterized in that treating the resulting solution with 10-30% v/v, of an acrylic polymer of molecular weight in the range of 12000-15000 KD for a period of minimum 30 minutes, followed by optional addition of antimicrobial agent such as herein described in the range of 0.01-0.1% w/v, to get the proteinoid-acrylate composite. 2. A process as claimed in claim 1 wherein the source of proteinous material used is hide, skin, fleshing, buffing dust, shaving dust, leather trimmings, animal hair. 3. A process as claimed in claim 1 wherein the known method of sterilization used is autoclaving, ultraviolet radiation, refrigeration. 4. A process as claimed in claim 1 wherein the known method of separation used is filtration, centrifuging, gravity separation. 5. A process as claimed in claim 1 wherein the acrylate polymer used is methyl acrylate, ethyl acrylate, propyl acrylate, butyl acrylate. 6. A process as claimed in laim 1 wherein the antimicrobial agent used is parachloro meta cresol, ortho phenyl phenol, thio cyano thio methyl thio benzo thiozole, either individually or in combination. 7. A process for the preparation of proteinoid-acrylate composite having molecular weight in -the range of 15000-20000 KD substantially as herein described with examples.

Full Text

The present invention relates to a process for the preparation of a proteinoid-acrylate composite having molecular weight in the range of 15000-20000 KD. More particularly, the present invention relates to a process for the preparation of a proteinoid-acrylate composite for application as filler-cum-syntan in leather processing industry. The syntan of the present invention has
potential application in post tanning wet processing section of leather
processing industry to get filling effect, grain tightness and softness in the
processed leather. The composite may also be used as filler in cardboard
industry.
One of the important operations, leathers are subjected to during the post
tanning wet operations is retanning, which has a major role to play in
connection with tightness, fullness and softness of the final leather. Different
syntans are conventionally used for this purpose depending on the
requirement of properties and end uses of the final leather.
Retanning syntans have usually been of non-proteinous nature. They may in
general be classified into two broad categories - phenolic syntan and resin
syntan.
Phenolic syntans are essentially phenol/ cresol/napthol/formaldehyde
containing acid derivatives, which can partially or completely replace vegetable
tanning materials for imparting tanning effect. Hence, they are also known as
replacement syntans. The phenolic syntans exhibit better filling effect in leather
and also result in better nap in suede leather. The main limitation of these

syntans lies in poor degradability as well as poor exhaustion in the range of 50-60% during dyeing, thereby adding to the effluent problem by way of increasing total dissolved solids of the waste water.
Resin syntans are essentially the sodium or ammonium salts of different resins, other than those, of phenol formaldehyde types. Resins of urea, dicyanamide, melamine etc., with formaldehyde or resins of acrylic and methacrylic acids, di-isocyanates, dialdehyde have generally been of much use. These syntans not only posses tanning properties, but also exhibit selective filling effect to ensure that the looseness of the leathers is removed. Thus these syntans provide uniformity, softness and grain tightness to the leather. As reported by Ludvik, (United Nations Industrial Development Organization, Report, 1,24,1996), the limitation associated with these syntans of poor exhaustion to the tune of maximum 60% during dyeing of leather, thereby adding to the effluent problem. Another major limitation associated with the resin syntans is that they are not stable at a temperature of more than 80°C, thereby rendering them unsuitable for producing leathers to be glaze finished.
The above limitations of the conventional resin syntans have prompted the researchers to look for better option in the realm of leather syntan. Ramamurthy et al (Journal of Society of Leather Technologists and Chemists, 73,168,1989) provided a process for preparing keratin hydrolysate for using as protein based syntan in leather processing, whereby the keratinous protein is hydrolysed by using acid or alkali. Conventionally, the acid hydrolysis of protein is carried out

at a pH in the range of 1-2, while alkali hydrolysis is done at a pH in the range
of 10-12. While the keratin hydrolysate, as prepared above, is effective in
improving the exhaustibility of dye or chrome to the tune of 85-90%, the major
limitation associated therewith is the lack of filling effect in the final leather,
thereby exhibiting no improvement on grain tightness.
Another limitation associated with the keratin hydrolysate is that it can be stored
for a maximum period of 6 months only because of its proteinous nature, which
results in its decaying tendency.
No prior art is available on any protein-resin combination product.
The main object of the present invention is to provide a process for the
preparation of a novel proteinoid-acrylate composite having molecular weight
in the range of 15000-20000 KD, which obviates the drawbacks stated above.
Another object of the present invention is to provide a process for the
preparation of a composite having thermo-tolerance more than 150°C.
Yet another object of the present invention is to provide a process for the
preparation of a composite, which can be stored for a period of minimum 1year.
Still another object of the present invention is to provide a process for the
economical use- of the abundantly available proteinous wastes to prepare
proteinoid-acrylate composite.
Yet another object of the present invention is to provide a process for preparing
a composite, which on being used in leather processing, imparts grain tightness

in leather and ensures better nap in suede leather, exhibiting at the same time
an exhaustability of more than 98% in dye bath.
Accordingly the present invention provides a process for the preparation of a
proteinoid-acrylate composite having molecular weight in the range of
15000-20000 KD, which comprises
i. aqueous washing of a proteinous material such as herein describeddby known method followed by

conventional acid or alkali hydrolysis for a period of minimum 30 minutes
and subsequent sterilisation of the resulting hydrolysate by known method, ii. separating the sterilised protein hydrolysate, as formed in step (i) by known
method and adjusting the pH of the resulting solution in the range of 4.5 - 6
by conventional method, iii. treating the resulting solution with 10-30% v/v, of an acrylic polymer of
molecular weight in the range of 12000-15000 KD for a period of minimum
30 minutes, followed by optional addition of 0.01-0.1% w/v antimicrobial
agent,'such as herein described to get the proteinoid-acrylate composite.
In an embodiment of the present invention, the source of proteinous material
used may be hide, skin, fleshing, buffing dust, shaving dust, leather
trimmings, animal hair.
In another embodiment of the present invention, the known method of
sterilisation used may be autoclaving, Ultraviolet radiation,
refrigeration.
In yet another embodiment of the present invention, the known method of
separation used may be filtration, centrifuging, gravity separation.
In still another embodiment of the present invention, the acrylate polymer used
may be such as methyl acrylate, ethyl acrylate, propyl acrylate, butyl acrylate.
In yet another embodiment of the present invention, the antimicrobial agent
used may be such as parachloro meta cresol, ortho phenyl phenol, thio cyano
thio methyl thio benzo thiozole, either individually or in combination.
The process of the present invention is described below in detail.
A proteinous source is washed well in aqueous medium to remove the adhering
extraneous materials and the washed stock is subjected to either acid or alkali
hydrolysis by conventional method for a period of minimum 30 minutes. While
acid hydrolysis is carried out at a pH in the range of 1-2, alkali hydrolysis is
carried out at a pH in the range of 10-12.
The resulting protein hydrolysate is sterilised by known method and the
sterilised solution is subjected to separation by known method to get the pure
protein hydrolysate solution.
pH of the pure protein hydrolysate solution, as obtained above, is adjusted in
the range of 4.5-6 by conventional method and the resulting solution is treated
with 10-30% v/v, of an acrylic polymer of molecular weight in the range of
12000-15000 KD, for a period of minimum 30 minutes under stirring condition
to get the proteinoid-acrylate composite. 0.01-0.1% v/v, of antimicrobial agent is
then added, as an optional step, to the resulting mass for storage.

The novelty and non-obviousness of the present invention lies in copolymerising a protein hydrolysate with acrylic resin to prepare a substrate exhibiting the desirable characteristics, which are otherwise difficult to be achieved using either protein based syntan or acrylic syntan individually, thereby suggesting at the same time an economical option for utilizing the proteinous wastes of different industries including leather industry in useful way. 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
1 Kg of hide fleshing, collected from the lime yard of a tannery, was washed thoroughly with plain water to remove all the extraneous matters. The washed stock was then taken in a round bottomed flask and 3 litres of water was added to it. 44 gms of solid NaOH pellets were then added slowly to the flask with continuous stirring, which was continued for another 30 min. At this stage, pH of the solution inside the flask was noted to be 10 and the mouth of the flask was plugged with non-absorbent cotton.
The flask was then autoclaved at a pressure of 1 Kg psi. After a period of three hours the flask was taken out of the autoclave and was allowed to cool down to a temperature of 25°C. The flask was then unplugged and the solution inside was filtered using filter paper. The solution was collected in a beaker and pH of the solution was found to be 11 which was brought down to 5.5 by adding 100 ml of dilute HCI.

200 ml of methyl acrylate having molecular weight of 12000 KD was added to the beaker with continuous stirring. After a period of 15 minutes, 0.5 gm of para chloro meta cresol with 0.5 gm of ortho-phenyl phenol were added to the beaker under stirring condition and the resulting solution of the proteinoid-acrylate composite was stored in a plastic container.
The proteinoid-acrylate solution was used in retanning at a feed of 10% on shaved weight for cow upper leather and was found to exhibit good filling to the resulting leather.
Example 2
1 Kg of buffing dust, collected from the buffing yard of a tannery, was washed thoroughly with ammoniacal water to remove all the extraneous matters. The washed stock was then taken in a round bottomed flask and 3 litres of water was added to it.'40 gms of solid NaOH pellets were then added slowly to the flask with continuous stirring, which was continued for another 45 min. At this stage, pH of the solution inside the flask was noted to be 10 and the mouth of the flask was plugged with non-absorbent cotton.
The flask was then exposed to UV radiation in a wooden chamber. After a period of 3 hours the flask was taken out of the chamber and was unplugged. The solution inside the flask was then centrifuged and the supernatant was taken out in a beaker. pH of the suprnatant was found to be 11.2 which was brought down to 5.0 by adding 90 ml of dilute HCI.

200 ml of ethyl acrylate having molecular weight of 14000 KD was added to the beaker with continuous stirring. After a period of 15 minutes, 1 gm of ortho phenyl phenol was added to the beaker under stirring condition and the resulting solution of the proteinoid-acrylate composite was stored in a plastic container.
The proteinoid-acrylate solution was used in retanning at a feed of 10% on shaved weight for cow upper leather and was found to exhibit improved glaze finish to the resulting leather.
Example 3
1 Kg of shaving dust, collected from the shaving yard of a tannery, was washed thoroughly with ammoniacal water to remove all the extraneous matters. The washed stock was then taken in a round-bottomed flask and 3 litres of water was added to it. 100 ml of HCI was then added slowly to the flask with continuous stirring, which was continued for another 40 min. At this stage, pH of the solution inside the flask was noted to be 1 and the mouth of the flask was plugged with non-absorbent cotton.
The flask was then sterilised by refrigeration method at temperature of 1°C for 5 hours. After a period of five hours the flask was taken out of the refrigeration . The flask was then unplugged and the solution inside was filtered using filter paper. The solution was collected in a beaker and pH of the solution was found to be 10.5 which was brought down to 5.5 by adding 150 gm of sodium acetate.

200 ml of butyl acrylate having molecular weight of 15000 KD was added to the beaker with continuous stirring. After a period of 15 minutes, 1 gm of thio cyano thio methyl thio benzo thiozole was added to the beaker under stirring condition and the resulting solution of the proteinoid-acrylate composite was stored in a plastic container.
The proteinoid-acrylate solution was used in retanning at a feed of 10% on shaved weight for cow upper leather and was found to exhibit good filling to the resulting leather.
Example 4
1 Kg of learther trimmings, collected from the tannery, was washed thoroughly with plain water to remove all the extraneous matters. The washed stock was then taken taken in a round bottomed flask and 3 litres of water was added to it. 44 gms of solid NaOH pellets were then added slowly to the flask with continuous stirring, which was continued for another 60 min. At this stage, pH of the solution inside the flask was noted to be 10 and the mouth of the flask was plugged with non-absorbent cotton.
The flask was then autoclaved at a pressure of 1 Kg psi. After a period of four hours the flask was taken out of the autoclave and was allowed to cool down to a temperature of 29°C. The flask was then unplugged and the solution inside was subjected to gravity separation. The supernatant was collected in a beaker and pH of the solution was found to be 11 which was brought down to 5.5 by adding 95 ml of dilute HCI.

200 ml of propyl acrylate having molecular weight of 12000 KD was added to the beaker with continuous stirring. After a period of 15 minutes, 0.75 gm of para chloro meta cresol was added to the beaker under stirring condition and the resulting solution of the proteinoid-acrylate composite was stored in a plastic container.
The proteinoid-acrylate solution was used in retanning at a feed of 10% on shaved weight for cow upper leather and was found to exhibit good filling to the resulting leather
Example 5
1 Kg of animal hair, collected from the lime yard of tannery, was washed thoroughly with plain water to remove all the extraneous matters. The washed stock was then taken in a round bottomed flask and 3 litres of water was added to it. 44 gms of solid NaOH pellets were then added slowly to the flask with continuous stirring, which was continued for another 90 min. At this stage, pH of the solution inside the flask was noted to be 10 and the mouth of the flask was plugged with non-absorbent cotton.
The flask was then autoclaved at a pressure of 1 Kg psi. After a period of three hours the flask was taken out of the autoclave and was allowed to cool down to a temperature of 24°C. The flask was then unplugged and the solution inside was filtered using filter paper. The solution was collected in a beaker and pH of the solution was found to be 11 which was brought down to 5.5 by adding 90 ml of dilute HCI.

200 ml of butyl acrylate having molecular weight of 15000 KD was added to the
beaker with continuous stirring. After a period of 15 minutes, 5 gms of thio
cyano thio methyl thio benzo thiozole was added to the beaker under stirring
condition and the resulting solution of the proteinoid-acrylate composite was
stored in a plastic container.
The proteinoid-acrylate solution was used in retanning at a feed of 10% on
shaved weight for cow upper leather and was found to exhibit good filling to the
resulting leather
The main advantages of the present invention are the following.
1. The process involves no difficult control parameters and hence it is easy to
operate.
2. It provides a process to use the hydrolysable proteinous wastes, which
otherwise create major disposal problem, for making auxiliaries for different
industries including leather processing industry, thereby reducing the load of
environmental pollution.
3. The composite prepared by the process of the present invention can
withstand a temperature upto 200°C and hence it can be used for the
processing of glazed finished leathers.
4. The composite prepared by the process of the present invention results in
grain tightening and ensures that the resulting leather is more amenable to
buffing not only for making corrected grain leathers, but also for getting
good nap while making suede leathers.

5. The composite ensures exhaustion of dye bath to the tune of 98%.
6. The product exhibits a shelf life of one year.

We claim :
1. A process for the preparation of proteinoid-acrylate composite having
molecular weight in the range of 15000-20000 KD, which comprises :
i. aqueous washing of a proteinous material such as herein described by known method followed by conventional acid or alkali hydrolysis for a period of minimum 30 minutes and subsequent sterilization of the resulting hydrolysate by known method,
ii. separating the sterilized solution, as formed in step (i) by known method and adjusting the pH of the resulting solution in the range of 4.5-6 by conventional method,
iii. charaterized in that treating the resulting solution with 10-30% v/v, of an acrylic
polymer of molecular weight in the range of 12000-15000 KD for
a period of minimum 30 minutes, followed by optional addition of antimicrobial agent such as herein described in the range of 0.01-0.1% w/v, to get the proteinoid-acrylate composite.
2. A process as claimed in claim 1 wherein the source of proteinous material
used is hide, skin, fleshing, buffing dust, shaving dust, leather trimmings,
animal hair.
3. A process as claimed in claim 1 wherein the known method of sterilization
used is autoclaving, ultraviolet radiation, refrigeration.

4. A process as claimed in claim 1 wherein the known method of separation
used is filtration, centrifuging, gravity separation.
5. A process as claimed in claim 1 wherein the acrylate polymer used is
methyl acrylate, ethyl acrylate, propyl acrylate, butyl acrylate.
6. A process as claimed in laim 1 wherein the antimicrobial agent used is
parachloro meta cresol, ortho phenyl phenol, thio cyano thio methyl thio
benzo thiozole, either individually or in combination.
7. A process for the preparation of proteinoid-acrylate composite having
molecular weight in -the range of 15000-20000 KD substantially as herein
described with examples.

Documents:

210-del-2001-abstract.pdf

210-del-2001-claims.pdf

210-del-2001-correspondence-others.pdf

210-del-2001-correspondence-po.pdf

210-del-2001-description (complete).pdf

210-del-2001-form-1.pdf

210-del-2001-form-19.pdf

210-del-2001-form-2.pdf

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Patent Number

231049

Indian Patent Application Number

210/DEL/2001

PG Journal Number

13/2009

Publication Date

27-Mar-2009

Grant Date

28-Feb-2009

Date of Filing

27-Feb-2001

Name of Patentee

COUNCIL OF SCIENTIFIC AND INDUSTRIAL RESEARCH

Applicant Address

RAFI MARG, NEW DELHI-110 001, INDIA.

Inventors:

#	Inventor's Name	Inventor's Address
1	JAMES KANAGARAJ	CENTRAL LEATHER RESEARCH INSTITUTE, ADYAR, CHENNAI-600020, INDIA.
2	MOHAMED RAFIUDDIN AHMED	CENTRAL LEATHER RESEARCH INSTITUTE, ADYAR, CHENNAI-600020, INDIA.
3	RAJADAS JAYAKUMAR	CENTRAL LEATHER RESEARCH INSTITUTE, ADYAR, CHENNAI-600020, INDIA.
4	NATESAN SAMIVELU	CENTRAL LEATHER RESEARCH INSTITUTE, ADYAR, CHENNAI-600020, INDIA.
5	BUDDIPUDI RAMANAIAH	CENTRAL LEATHER RESEARCH INSTITUTE, ADYAR, CHENNAI-600020, INDIA.

PCT International Classification Number

C04B 28/04

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1			NA