Title of Invention

"A PROCESS FOR THE PREPARATION OF WATER REPELLENT CHEMICAL USEFUL FOR MAKING WATER PROOF CELLULOSE BASED TEXTILE MATERIALS"

Abstract The present invention relates to a process for the preparation of water repellent chemical useful for making water proof cellulose based textile materials. The fabrics generally used to make any clothing for general use do not have the property to repel water. The process steps are: reacting a transition metal oxide with concentrated hydrochloric acid, cooling the reaction mixture by known methods, adding branched chain alcohol to the said cooled reaction mixture to obtain a metal isopropoxide with a lower valency of the metal followed by adding a fatty acid under constant stirring to obtain water repellent chemical.
Full Text The present invention relates to a process for the preparation of water repellent chemical useful for making water proof cellulose based textile materials, a process for manufacture of water proof cellulose based textile materials and water proof textile materials made thereby.
The fabrics generally used to make any clothing for general use do not have the property to repel water. Many a times such water repellent property is necessary not only for protection of human beings but also for electronic and other gadgets which are to be used in any field experiments or surveys. Such clothing as on date are made water proof by using the technique of waxing. This technique renders the fabric heavy and normally becomes cumbersome to handle. In the present invention a process for the water repellent chemical has been developed, which does not alter the weight properties of the original fabric and is easy to apply.
The commonly used waxing technique to make the cloth water proof is not economical and gets costlier due to ever increasing price of the petroleum products. Further the waxing process leads to the increase in weight of the fabric and hence makes it difficult in handling, transportation and also in use. Also the waxing process is cumbersome. Reference may be made to an Indian patent (application no. 892/CAL/94). In this patent application use has been made of finely devided material consisting of cellulose material, mineral material, organic waste material and inorganic waste material and latex containing magnesium oxychloiride and /or magnesium oxysulphate. In this process also, the overall weight of the finished product increases significantly thus making it difficult to handle.
The main object of the present invention is to provide a process for the preparation of water repellent chemical useful for making cellulose based textile materials which obviates the drawbacks as mentioned above.
Another object of the present invention is to provide a chemical, which is easy to handle and is ecofriendly.
Yet another object of the present invention is to provide a chemical which maintains the weight characteristics of the cloth under treatment for water proofing.

Another object of the present invention is to provide a process for the manufacture of water proof cellulose based textile material using the water repellent chemical; which obviates the drawbacks as mentioned above.
Still another object of the present invention is to provide water proof textile materials.
Accordingly the present invention provides A process for the preparation of water repellent chemical useful for making water proof cellulose based textile materials which comprises: reacting a transition metal oxide with concentrated hydrochloric acid, cooling the reaction mixture by known methods, adding branched chain alcohol to the said cooled reaction mixture to obtain a metal isopropoxide with a lower valency of the metal, followed by adding a fatty acid under constant stirring to obtain water repellent chemical.
In an embodiment of the present invention the transition metal oxide used may be such as chromium oxide, iron oxide, titanium oxide, vanadium oxide.
In another embodiment of the present invention the amount of transition metal oxide used may be in the range of 20 wt% 30% of hydrochloric acid.
In yet another embodiment of the present invention the branched chain alcohol used may be such as isopropanol, butanol.
In another embodiment of the present invention the fatty acid used may be such as oleic acid, stearic acid.
In yet another embodiment of the present invention the amount of fatty acid used may be in the range of 10 wt% to 15 wt%
In another embodiment of the present invention the stirring of the mixture may be done by known methods such as magnetic stirring manual mechanical stirring.
Accordingly the present invention provides a process for the manufacture of water proof cellulose based textile materials which comprises: preparing a 2-5 wt.% aqueous solution of the water repellent chemical as described above, dipping a cellulose based

textile material in the said solution for full wetting, removing the cloth and drying by known methods.
In an embodiment of the present invention the cellulose based textile material used maybe of a composition having at least 70% cotton.
Accordingly the present invention provides water proof cellulose based textile material made by the process of the present invention.
hi an embodiment of the process of the present invention for preparing the water repellant chemical: 15-30 gms of transition metal oxide is taken and mixed with 30- 50ml of concentrated hydrochloric acid. This reaction mixture being exothermic heat generation occurs which necessitates cooling of the mixture. To the cooled reaction mixture is added of 150-300 ml.of branched chain alcohol. To this mixture is added a fatty acid in a quantity of 20 to 40 gms and the total mixture is stirred continuously. After this stirring the water repellant chemical is ready for use.
The treatment of the cloth is very simple. The water repellent chemical to be used is first made into a solution in ordinary water to make a 2-5wt. % solution. This solution is then ready for treating the fabric. The fabric is dipped for full wetting in the solution and taken out and hung dry. After the treated fabric is dried the same can be checked for water proofing by making a bag and pour water into it. This is then hung for a period of at least one day to see the presence of any water droplets on the outer surface. If it is observed that there are no water droplets on the outer surface it is established that the water proofing of the fabric treated with the water repellent chemical is effective.
The following examples are given by way of illustration only and should not be construed to limit the scope of the invention.
Example-1
15 gms of iron oxide of laboratory grade reagent purity was taken to which was added 30 ml of concentrated hydrochloric acid. This mixture was allowed to cool for some time and was further cooled by putting the beaker containing the mixture in ice cold water. To this was added 150 ml of isopropyl alcohol. Next, 20 gms. of Stearic acid was added to this mixture and was stirred continuously by means of magnetic stirrer to effect complete

dissolution of the fatty acid. The fully dissolved fatty acid thus completes the chemical which is ready for application to any cellulose based material.
20 ml of water repellent chemical was taken in a large bucket and to it was added water to make it to 1 litre. This give a 2 wt.% water repellent ready for use with the fabric. . The handkerchief was soaked in the solution for 10 minutes and then kept for complete dryness. After the handkerchief was fully dried it was made into a small bag and water was poured into it. The bag was hung from a thread and the same was kept untouched for 12 hours. The state of the handkerchief was examined after the said soaking time. No presence of any water droplets were found on the exterior of the handkerchief, thereby indicating the waterproofing of the cloth.
Example-2
30 gms of iron oxide of laboratory grade reagent purity was taken to which was added 30 ml of concentrated hydrochloric acid. This mixture was allowed to cool for some time and was further cooled by putting the beaker containing the mixture in ice cold water. To this was added 150 ml of isopropyl alcohol. Next, 20 gms. of Stearic acid was added to this mixture and was stirred continuously by means of magnetic stirrer to effect complete dissolution of the fatty acid. The fully dissolved fatty acid thus completes the chemical which is ready for application to any cellulose based material.
20 ml of water repellent chemical was taken in a large bucket and to it was added water to make it to 1 litre. This give a 2% water repellent ready for use with the fabric. The handkerchief was soaked in the solution for 10 minutes and then kept for complete dryness. After the handkerchief was fully dried it was made into a small bag and water was poured into it. The bag was hung from a thread and the same was kept untouched for 24 hours. The state of the handkerchief was examined after the said soaking time. No presence of any water droplets were found on the exterior of the handkerchief, thereby indicating the waterproofing of the cloth.
Example- 3
15 gms of iron oxide of laboratory grade reagent purity was taken to which was added 50 ml of concentrated hydrochloric acid. This mixture was allowed to cool for some time and was

further cooled by putting the beaker containing the mixture in ice cold water. To this was added 150 ml of isopropyl alcohol. Next, 20 gms. of Stearic acid was added to this mixture and was stirred continuously by means of magnetic stirrer to effect complete dissolution of the fatty acid. The fully dissolved fatty acid thus completes the chemical which is ready for application to any cellulose based material. 50 ml of water repellent chemical was taken in a large bucket and to it was added water to make it to 1 litre. This give a 5% water repellent ready for use with the fabric. . The handkerchief was soaked in the solution for 10 minutes and then kept for complete dryness. After the handkerchief was fully dried it was made into a small bag and water was poured into it. The bag was hung from a thread and the same was kept untouched for 24 hours. The state of the handkerchief was examined after the said soaking time. No presence of any water droplets were found on the exterior of the handkerchief, thereby indicating the waterproofing of the cloth.
Example- 4
15 gms of iron oxide of laboratory grade reagent purity was taken to which was added 30 ml of concentrated hydrochloric acid. This mixture was allowed to cool for some time and was further cooled by putting the beaker containing the mixture in ice cold water. To this was added 300 ml of isopropyl alcohol. Next, 30gms. of Stearic acid was added to this mixture and was stirred continuously by means of magnetic stirrer to effect complete dissolution of the fatty acid. The fully dissolved fatty acid thus completes the chemical which is ready for application to any cellulose based material.
50 ml of water repellent chemical was taken in a large bucket and to it was added water to make it to 1 litre. This give a 5% water repellent ready for use with the fabric. . The handkerchief was soaked in the solution for 10 minutes and then kept for complete dryness. After the handkerchief was fully dried it was made into a small bag and water was poured into it. The bag was hung from a thread and the same was kept untouched for 24 hours. The state of the handkerchief was examined after the said soaking time. No presence of any water droplets were found on the exterior of the handkerchief, thereby indicating the waterproofing of the cloth.

Example-5
30 gms of chromium oxide of laboratory grade reagent purity was taken to which was added 50 ml of concentrated hydrochloric acid. This mixture was allowed to cool for some time and was further cooled by putting the beaker containing the mixture in ice cold water. To this was added 150 ml of isopropyl alcohol. Next, 20 gms. of Stearic acid was added to this mixture and was stirred continuously by means of magnetic stirrer to effect complete dissolution of the fatty acid. The fully dissolved fatty acid thus completes the chemical which is ready for application to any cellulose based material.
20 ml of water repellent chemical was taken in a large bucket and to it was added water to make it to 1 litre. This give a 2% water repellent ready for use with the fabric. The handkerchief was soaked in the solution for 10 minutes and then kept for complete dryness. After the handkerchief was fully dried it was made into a small bag and water was poured into it. The bag was hung from a thread and the same was kept untouched for 24 hours. The state of the handkerchief was examined after the said soaking time. No presence of any water droplets were found on the exterior of the handkerchief, thereby indicating the waterproofing of the cloth.
Example-6
30 gms of iron oxide of laboratory grade reagent purity was taken to which was added 50 ml of concentrated hydrochloric acid. This mixture was allowed to cool for some time and was further cooled by putting the beaker containing the mixture in ice cold water. To this was added 150 ml of isobutanol . Next, 20 gms. of Oleic acid was added to this mixture and was stirred continuously by means of magnetic stirrer to effect complete dissolution of the fatty acid. The fully dissolved fatty acid thus completes the chemical which is ready for application to any cellulose based material.
20 ml of water repellent chemical was taken in a large bucket and to it was added water to make it to 1 litre. This give a 2% water repellent ready for use with the fabric. The handkerchief was soaked in the solution for 10 minutes and then kept for complete dryness. After the handkerchief was fully dried it was made into a small bag and water was poured

into it. The bag was hung from a thread and the same was kept untouched for 24 hours. The state of the handkerchief was examined after the said soaking time. No presence of any water droplets were found on the exterior of the handkerchief, thereby indicating the waterproofing of the cloth.
The novelty of the present invention lies in preparation of a water resistant chemical which when incorporated in cellulose based trextile material imparts water proof qualities and does not increase the weight of the cloth.. The other novelty of the invention is that the process involves simple process steps like mixing of the various ingredients and there is no heating required.
The inventive step lies in stabilisation of isopropoxide by adding the fatty acid resulting in a chemical which imparts water repellent property when a cellulose based textile material is treated with the resultant chemical obtained by the process of the present invention. The advantages of the invention are:
1. The process involves simple mixing .cooling and stirring and hence is economical.
2 The process is eco friendly.
3. The process uses commonly available chemicals .
4. The water proofing treatment of the cloth is simple and economical.
5. The water proof textile material is comparable or better than what is presently available.



We Claim:
1 . A process for the preparation of water repellent chemical useful for making water proof cellulose based textile materials which comprises: reacting a transition metal oxide with concentrated hydrochloric acid, cooling the reaction mixture by known methods, adding branched chain alcohol to the said cooled reaction mixture to obtain a metal isopropoxide with a lower valency of the metal, followed by adding a fatty acid under constant stirring to obtain water repellent chemical.
2. A process as claimed in claim 1 wherein the transition metal oxide used is selected from
chromium oxide, iron oxide, titanium oxide, vanadium oxide.
3. A process as claimed in claims 1 and 2 wherein the amount of transition metal oxide
used is in the range of 20 to 30 wt% of hydrochloric acid.
4. A process as claimed in claims 1-3 wherein the branched chain alcohol used is such as
isopropanol, butanol.
5. A process as claimed in claims 1-4 wherein the branched chain alcohol used is in the
range of 90 to 100wt%.
6. A process as claimed in claims 1-5 wherein the fatty acid used is such as oleic acid,
stearic acid.
7. A process as claimed in claims 1-6 wherein the amount of fatty acid used is in the range
of 10 to 15 wt%.
8. A process as claimed in claims 1-7 wherein the stirring of the mixture is done by known
methods such as magnetic stirring, manual mechanical stirring.
9. A process for the preparation of water repellent chemical useful for making water proof
cellulose based textile materials substantially as herein described with reference to the
examples.

Documents:

1288-del-1999-abstract.pdf

1288-del-1999-claims.pdf

1288-del-1999-correspondence-others.pdf

1288-del-1999-correspondence-po.pdf

1288-del-1999-description (complete).pdf

1288-del-1999-form-1.pdf

1288-del-1999-form-19.pdf

1288-del-1999-form-2.pdf

1288-del-1999-form-3.pdf


Patent Number 221665
Indian Patent Application Number 1288/DEL/1999
PG Journal Number 31/2008
Publication Date 01-Aug-2008
Grant Date 30-Jun-2008
Date of Filing 23-Sep-1999
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 DANESH CHANDRA PARASHAR NATIONAL PHYSICAL LABORATORY NEW DELHI INDIA.
2 AJIT KUMAR SARKAR NATIONAL PHYSICAL LABORATORY NEW DELHI INDIA.
PCT International Classification Number B32B 27/02
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA