Title of Invention

"A WATER PROOFING COMPOSITION AND TO A PROCESS FOR THE PREPARATION THEREOF"

Abstract

The Invention comprises a water proofing composition, which is capable of bing coated on natural packaging matrials such as craft paper, corrugated card board, cotton, jute, ply and wood etc. The compositon is prepared by mixing silicon rsins in an organic solvent along with a metal carboxylate catalyst and a cross-linking agnt to obtain cross linked silicone resin The silicon resin is synthesised by hydrolysis of a diorganodichlorosilane and an organotrichlorosilane at room temperature. The cross linked silicon rsin is dispersed in an : " non-aqueous and non-f lammab solution of a haloform.

Full Text

FIELD Of INVENTION; The Invention relates to a water proofing composition and to a process for the preparation thereof. Though not limited thereto, the water proofing composition of the present invention may advantageously be employed in making water repellent natural packaging material such as craft paper, pulp based paper board, jute based, ply based and wooden packaging material. PRIOR ART; Packaging materials made from craft paper, corrugated paper board, jute, ply and wood are used for packaging a variety of items including perishable food items, clothing, leather ind other variety of items. In order to safely transport these ijt^ns from one place to another place, it is essential that the packaging materials should be resistant to moisture, fflicrobi.al attack and thermal/radiation shocks. In general, packaging materials are provided with a coating of water proofing compositions to make these packaging materials resistant to degradation due to varying climatic conditions. Mostly, these water proofing compositons are based on organic polymeric materials, such as polystyrene, polybutadtejne, latex, wax, co-polymers of acrylic acid, alkyl methaacry laities, fluoro resins etc. The organic materials also utilise a variiety of cross-linking agents to form water repellent coating surface$. However, these organic materials, known in the prior art f Main disadvantage of these known water proofing compositions is that these compositions are used in aqueous solution and as such packaging materials coated with these compositibns require sufficient time for drying. These known water proofing compositions can not be coated on packaging materials containing such stored commodities which are susceptible to moisture. Another disadvantage of these known water proofing compositions is that these compositions can not be used over a wide range of temperature applications. Packaging materials coated with these water proofing compositions are not thermally stable and may show crack with the changing climatic conditions. Yet another disadvantge of the water proofing compositions^ known in the art, is that these compositions are susceptible to organic solvents. Still another disadvantge of the water proofing compositions, known in the art, is that coating of these compositions do not have better adhesive property. Yet another disadvantage of the water proofing compositions, known in the art is that these compositions such as fluoro-resins are generally costly . Still another disadvantage of the water proofing compositions, known in the art, is that coatings of these compositions are not very impact resistant. Yet another disadvantage of the water proofing compositions, known in the art, is that these compositions are not very eco-friendly. Another type of water proofing compositions, known in the art, are based on inorganic polymers such as perfluoroalkylethyl tris (alkoxy) silanes and polymeric fluorocarbon siloxane etc. These water proofing compositions utilise other additives apart from these inorganic compounds for making waterproofing coatings. However, these compositions, which are based on inorganic materials, also suffer from following disadvantages. Main disadvantage of these inorganic water proofing compositions, known in the art, is that these compositions are used in aqueous medium and as such coatings of these materials need adequate time for drying of the coating. As such, packaging containers, which are already packed with moisture sensitive items inside it, can not be coated with these type of water proofing compositions. Another disadvantage of the inorganic water proofing compositions, known in the art, is that these compositions need raw materials such as flouro-silicones, which are not easily available and very costly. Yet another disadvantage of the compositions, known in the art, is that these compositions require fluorine and fluorinating agents for synthesis, which are not very eco-friendly . OBJECTS OF THE INVENTIONS; Primary object of the invention is to propose a non-aqueous water proofihng composition which is based on an inorganic polymeric material and to a process for the preparation thereof* Another object of the invention is to propose a water proofing composition and to a process for the preparation thereof which is based on polyorgano siloxane resin. Still another object of the invention is to propose a water proofing composition, which is biologically inert and non-toxic. Yet another object of the invention is to propose a water proofing composition, which has improved capacity to withstand variation of temperature over a large range thereby rendering the coating of this composition crack proof in different climatic conditions. Still another object of the invention is to provide a process for preparation of a water proofing composition which has superior flow characteristics thereby leading to better impregnation of the cellulose texture of packaging material. Yet another object of the invention is to provide a process for preparation of a water proofing composition which results in a coating film of improved adhesion when coated on the packaging material. Still another object of the invention is to provide a process for preparation of a water proofing composition, which has an improved gloss. Yet another object of the invention is to provide a process for preparation of a water proofing composition which has an improved impact strength. Still another object of the invention is to provide a process for preparation of a water proofing composition which is non-flammable thereby making it safe while handling. Yet further object of the invention is to provide a process for preparation of a water proofing composition which is resistant to microbial attack Still further object of the invention is to provide a process for preparation of a water proofing composition which has a very fast drying time at room temperature thereby reducing the coating time. Yet further object of the invention is to provide a process for preparation of a water proofing composition which can be easily handled and coated safely without requiring sophisticated machinery. Still further object of the invention is to provide a process for preparation of a water proofing composition, which is simpler and cheaper to make. Yet further object of the invention is to provide a process for preparation of a water proofing composition which is eco-friendly. DESCRIPTION OF THE INVENTIONS: According to present invention, the water proofing composition is prepared by mixing silicone resins in an organic solvent along with a metal carboxylate catalyst and a cross linking agent to obtain 'cross linked siiicone resin. The silicone resin is synthesised by hydrolysis of a diorganodichlorosilane and an organotrichlorosilane at room temperature. The chemical reaction involved in the sysnthesis of the silicon resin is shown in the following. The chemical reaction involved in the cross linking of silicon resin with a cross linker has been shown in the following. The silicon resin and titanium of cross linker are cross linked through oxygen bonding. This cross linked silicone polymer is dispersed in a non-aqueous and non-flammable haloform solution. According to the present invention, the process of preparation of the water proofing composition comprises of following steps; (i) Synthesis of silicone resin bv hydrolysis of a diorganodichlorosilane and an organotrichlorosilane at room temperature in a three necked flask under continuous stirring Initially, silicon resin of desired quality is prepared by the hydrolysis of a diorganodichlorosilane and an organotrichlorosilane mixed together and taken in appropriate molar ratio. The molar ratio of the diorganodichlorosilane and organotrichlorosilane is taken in such a manner so that the total number of silicon atom and carbon atom from all the organochlorosilane moieties fall in the range of 1:3 to 1 ;6 preferably 1:4. The organic group attached with the silicon atom may be selected from hydrocarbon based alkyl or aryl groups having constituent carbon group from Gi TO C6. The diorganodichlorosilane used as one of the component is preferably methylphenyldichlorosilane or diphenyldichlorosilane or dimethyl dichlorosilane or a mixture of above. The organotrichlorosilane used as the other component is preferably phenyltrichlorositene or methyltrichlorosilane or a mixture of above. The mixture of both the above individual components i.e. diorganodichlorosilane and organotrichlorosilane are added in the water under continuous stirring at room temperature. The separated silicon, which is obtained at the end of the reaction, is washed repeatedly till the water becomes neutral. The silicon resin, thus obtained, is dried under vacuum at about 100 °C to obtain anhydrous silicon resin. (ii) Preparation of metal carboxvlate catalyst like Sn and Zn carboxvlate The silicon resin obtained from step (i) is cross linked with a cross linking agent. A metal carboxvlate of Sn or Zn is used as a catalyst in the cross linking reaction of silicon resin and cross linking agent. The Zinc metal carboxylaye catalyst should have two carboxylic groups having C4-C8, which may be linear or branched. The preferable zinc carboxylate is Zinc 2-ethylhexoate. Zinc octoate, carboxylate of zinc, is prepared freshly by standard method using zinc oxide and 2-ethylhexoic acid. The Sn carboxylate should contain two M-C aliphatic groups ranging from Ga to €4 and preferably it should be of type n-C4H9. The carboxylate group is from aliphatic Ca-Ci2 carbon containing acetates and preferably laurate carboxylate containing C12. Dispersion of silicone resin prepared in step (i) in an organic solvent at room temperature The silicon resin prepared in step (i) is taken into a three necked flask fitted with a pressure equalising dropping funnel and a mechanical stirrer. Toluene preferably carbon tetrachloride taken in ratio 1:1.2 (wt wise) to the silicon resin is added to the silicon resin under continuous stirring. The stirring of the solution is continued till the resin is completely dispersed in the toluene. Addition of catalyst to the dispersed solution of silicon resin prepared in step (HO The catalyst prepared in Step (ii) is added to the toluene solution prepared in step (iii). The quantity of catalyst is taken as about 0.1-0.4% preferably 0.2% wt wise to the silicon resin. (v) Addition of cross-linking agent to the solution of silicon resin and catalyst prepared in step (iv) The cross linking solution is prepared by adding about 0.5- 1.5 gm preferably 1 gm of metal tetraalkoxides preferably silicon or titanium tetraalkoxide to about 0.5-2 ml preferably 1 ml of toluene solution. The cross linking agent, prepared in above manner, is taken about 1.5-2.0% preferably 1.8% (wt wise) of the silicon resin and is added to the solution prepared in step (iv) using dropping funnel. At the end of this step, cross linked silicon resin is obtained. (vi) Addition of non-acaueous and non-flammable haloform solution to the solution of cross linked silicon resin obtained in step (v) A non-aqueous and non-flammable haloform, preferably carbon tetrachloride, is added to the solution prepared in step (v) under continuous stirring. The haloform is taken in about 4: 1 ratio (wt wise) to the solution prepared in step (v). The solution is further stirred for about 1-2 hours The resultant water proofing agent, thus prepared, is placed under nitrogen in air tight bottles. The invention will now be illustrated with the working examples, which are typical examples to illustrate the working of the invention and are not intended to be taken restrictively to imply any limitation on the scope of the present invention. WORKING EXAMPLE-1 Initially, 2 liter water is taken in a three necked flask fitted with pressure equalising dropping funnel at room temperature (25-30 °C). A solution of organochlorosalane comprising 129 gm (1 mole) of dimethyldichlorosilane and 352 gm (1 mole) of phenyltrichlorosilane are taken in pressure equalising dropping funnel. The entire mix of organochlorosilane, thus obtained, is gradually added to the water solution over a time period of 60-90 minutes under continuous stirring. The total solution is again stirred for one hour. The organic layer is washed several times till the water becomes neutral. The residual silicon is dried at 100 °C under vacuum of 0.1 mm of Hg. 500 gm of the dried silicon resin is again taken in a three necked flask and 500 ml of toluene is added to it. The solution is continuously stirred till the silicon resin is dispersed in the toluene. To this solution, 9 gm of titanium tetrabutoxide and 0.55 gm of zinc-2-ethylehexoate are added using the dropping funnel. The resultant solution is again vigorously stirred for one hour. Afterwards, 4040 gm of a non-aqueous and non-flammable haloform carbon tetrachloride is added to this solution and mixed properly. The final product, i.e. about 4.5 liter of water proofing composition, is kept under nitrogen in sealed bottles. WORKING EXAMPLE-2 Initially, 2 liter water is taken in a three necked flask fitted with pressure equalising dropping funnel at room temperature (25-30°C). Next, 191gm (1mole) of methylphenyldichlorosilane (a diorganodichlorosilane) and a solution of organotrichlorosilane comprising 211.5 gm (1 mole) of phenyltrichlorosilane and 149.5 gm (1 mole) of methyltrichlorosilane are taken in pressure equalising dropping funnel. This total mix of diorganodichlorosilane and organotrichlorosilane is gradually added to the water solution over a time period of 60-90 minutes under continuous stirring. The total solution is again stirred for about one hour. The organic layer of silicone is washed several times till the water becomes neutral. The residual silicon, thus obtained at the end of the reaction, is dried at 100 °C under vacuum of 0.1 mm of Hg. Next, 500 gm of the dried silicon resin is taken in a three necked flask and 500 ml of toluene is added to it. The resultant solution is continuously stirred till the silicon resin is totally dispersed in the toluene. To this solution, 9 gm of titanium tetrabutoxide and 0.55 gm of zinc-2-ethylehexoate are added using the dropping funnel. The resultant solution is again vigorously stirred for one hour. Afterwards, 4040 gm of a non-aqueous and non-flammable haloform carbon tetrachloride is added to this solution and mixed properly. The final product, i.e. about 4.5 liter of water proofing composition is kept under nitrogen in sealed bottles. WORKING EXAMFLE-3 Initially, 2 liter water is taken in a three necked flask fitted with pressure equalising dropping funnel at room temperature (25-30 °C). Next, a solution of diorganodichlorosilane comprising 243 gm (1 mole) diphenydichlorosilane and 258 gm (1 mole) of dimethyldichlorosilane are mixed with 149.5 gm (1 mole) of methyltrichlorosilane (an organotrichlorosilane) and are taken in a pressure equalising dropping funnel. The total mix of this organochlorosilane is gradually added to the water solution over a time period of 60-90 minutes under continuous stirring. The total solution is again stirred for one hour. The organic layer is washed several times till the water becomes neutral. The residual silicon , obtained at the end of this reaction, is dried at 100 °C under vacuum of 0.1 mm* of Hg. Next, 500 gm of the dried silicon resin is taken in a three necked flask and 500 ml of toluene is added to it. The resultant solution is continuously stirred till the silicon resin is dispersed in the toluene. To this solution, 9 gm of tetraethylsilicate and 0.55 gm of diisobutyttin are added using the dropping funnel. The resultant solution is again vigorously stirred for one hour. Afterwards, 4040 gm of a non-aqueous and non-flammable haloform carbon tetrachloride is added to this solution and mixed properly. The final end product i.e. about 4.5 liter of water proofing composition, is kept under nitrogen in sealed bottles. It is to be understood that the process of the invention is susceptible to adaptations, changes and modifications by those skilled in the art. Such adaptations, changes apd modifications are intended to be within the scope of the present invention, which is further set forth with the following claims. WE CLAIM; 1. A water proofing composition for making water repellant natural packing material comprising of wt wise 1:3 to 1:6 silicon polymer having alkyl and aryl pendant group, wt wise 1.5-2.0 cross linking agent having at least one variable valency metal alkoxide such as titanium butaoxide or tin butaoxide, wt wise 0.1-0.4 metal carboxylate catalyst such as zinc carboxylate, said carboxylate having a linear or branch carbon chain ranging from C2-Cio preferably €4 and non-aqueous and non-flammable haloform. 2. A composition as claimed in claim 1 wherein the said catalyst is taken wt wise preferably 0.2% of the silicon resin. 3. A composition as claimed in claim 1 wherein the said cross linker is taken wt wise preferably 1.8% of the silicon resin. 4. A composition as claimed in claim 1 wherein the said haloform solution is preferably carbon tetrachloride taken wt wise in 4:1 ratio to the said cross linked solution of silicon resin. 5. A process of the preparation of said water proofing composition comprising in the steps of: (i) Synthesis of silicon resin by hydrolysis of a diorganodichlorosilane and an organotrichlorosilane in range of 1:3 to 1:6 under continuous stirring; (ii) Dispersing silicon resin, prepared in step (i), in an organic solvent such as herein described; (iii) Adding a catalyst -such as Zinc Carboxylate to the dispersed solution of silicon resin prepared in step (ii) in the range of 0.1-0.4% to said Silicon resin; (iv) Adding a cross-linking agent to he solution of silicon resin wt. wise 1.5-2.0% to Silicon resin; (v) Adding an non-aqueous and non-flammable haloform to the solution of cross; linked silicon resin obtained in step (iv). 6. A process as claimed in claim 5 wherein said diorganodichlorosilane is preferably dichlorosilane and said orgnotrichlorosilane is preferably phenyltrichlorosilane and which are taken in such molar content so as to maintain the ration of Silicon and Carbon is preferably in the range of 1:4. 7. A process a claimed in claim 5 wherein said Zn carbosylate catalyst is prepared using Zinc oxide and 2-ethylhexoic acid, 8. A process as claimed in claim 5 wherein said organic solvent for dispersing the said silicon polymer is toluene preferably carbon tetrachloride taken in 1:2 ratio wt wise to said silicon resin. 9. A process as claimed in claim 5 wherein the said catalyst is taken wt wise preferably 0.2% of the silicon resin. 10. A process as claimed in claim 5 wherein the said cross linker is taken wt wise preferably 1.8% of the silicone resin. 11. A process as claimed in claim 5 wherein the said haloform solution is preferably carbon tetrachloride taken wt wise in 4:1 ratio to the said cross linked solution of silicon resin. 12. A process as claimed in claim 5 wherein said silicone polymer and titanium of said cross linker are cross linked to form cross linked silicone polymer through oxygen bonding. 13. A process as claimed in claim 5 wherein said cross linked silicone polymer is dispersed in a non-aqueous and non-flammable haloform solution preferably carbon tetrachloride.

Documents:

141-del-2002-abstract.pdf

141-del-2002-claims-02-05-2008.pdf

141-del-2002-claims.pdf

141-del-2002-correspondence-others-02-05-2008.pdf

141-del-2002-correspondence-others.pdf

141-del-2002-description (complete).pdf

141-del-2002-form-1.pdf

141-del-2002-form-18.pdf

141-del-2002-form-2.pdf

141-del-2002-form-3.pdf

141-del-2002-gpa.pdf