Title of Invention

A NOVEL ORGANO SILICONE POLYMER ANTIFOAM AND A PROCESS FOR ITS MANUFACTURE

Abstract

A new organo-silicone polymer which would be effective as an antifoaming agent for dyeing of fabrics and the like. The organo-silicone polymer is obtained by equilibration of organo polysiloxane with amino silanes in the presence of catalyst. In particular, the process involves (i) reacting polydimethytsiloxane, alkyl / aryl siloxy ended silicone fluid and amino functional silane in the presence of a catalyst to obtain silicone polymer substantially free of contaminants, and (ii)adding the said silicone polymer obtained in (i) above, having OH groups maintaining a reaction temperature of 120°C to 180°C, preferably from 110°C to 120°C in the presence of a catalyst, thereby obtaining the organo polysiloxane compound of general formula (I). The organo silicone polymer would be cost-effective and would essentially avoid the problems of deposition of silicone oil in the walls of the dyeing machine to favour stainfree dyeing of fabrics in a cost-effective manner to meet the demands of mills. The polymer would be useful as an antifoaming agent in dyeing process which would favour stain free dyeing with favourable fabric characteristics to facilitate the subsequent stages of processing / treatments of fabrics and like to obtain finished products. The polymer would further provide for improved and cost-effective process of dyeing and processing of fabrics and the like.

Full Text

A NOVEL ORGANO SILICONS POLYMER ANTIFOAM AND A PROCESS FOR ITS MANUFACTURE 2. WACKER METROARK CHEMICALS LIMITED, D H Road. Mouja Chandi, PS Bishnupur. 24 Parganas (South), State of West Bengal. PIN - 743 503, India, an Indian company The following specification particularly describes the nature of the invention and the manner in which it is to be performed. A NOVEL ORGANO SILICONE POLYMER ANTIFOAM AND A PROCESS FOR ITS MANUFACTURE The present invention relates to a novel organo polysiloxane compound, its preparation and use. In the dyeing machine for the dyeing of polyester fabric or polyester-cotton or cotton, conventional activated silicone emulsion is in use as an antifoaming agent for controlling foam that affects uniform dyeing on the fabric. In the next step, the dyed fabric is finished where softening agents like cationic softener, amino silicone softener or other softener or mixture of these are used in the padding bath and subsequently drying and curing of the fabric is carried out followed by passing the fabric through stentor. The use of antifoaming agent is thus an essential ingredient in the dyeing process because during the dyeing process, foam causes inconsistent coloration. It is known to use dynamic silicone antifoam in the dyeing process because dynamic silicone antifoam is stable at high temperature, as well it doesn't impart any stain at high temperature. However, due to high price of dynamic silicone antifoam, mills generally prefer to use normal silicone antifoam in the dyeing process. Since the normal silicone antifoam is not stable at 60°C and above, it separates and gradually deposits inside the wall of the dyeing machine. After 10 to 15 no. of dyeing, silicone deposition is enough in the machine which start to impart stain in the fabric. Therefore, to avoid such disadvantages of staining, mills use dark coloured fabric to take on stain. Therefore, due to the non-availability of moderately priced silicone antifoam which could avoid the problem of staining of fabric during dyeing, mills usually prefer to use normal siltcone antifoam to keep down the cost and avoid the problems of staining to the extent possible using dark coloured fabrics. After dyeing, fabrics go to padding for finishing stage where softening of the dyed fabric using finishing chemicals is effected. For this purpose, systems like cationic softener or amino silicone emulsion or mixture of amino silicone emuision and 2 cationic softener is applied through padding mandrel and finally cured and dried in stentor at about 130°C to 150°C. Padding step is also a remarkable cost involving process-involving manpower, huge energy etc. The invention has for its object provide a new organo-silicone polymer which would be effective as an antifoaming agent for dyeing of fabrics and the like, would be cost-effective and also avoid the problems of staining of fabrics during dyeing. Yet another object of the present invention is to provide a novel organo silicone polymer which would be cost-effective and would essentially avoid the problems of deposition of silicone oil in the walls of the dyeing machine to favour stainfree dyeing of fabrics in a cost effective manner to meet the demands of mills. Yet another object of the present invention is to provide a novel organo silicone polymer useful as an antifoaming agent in dyeing process which would favour stain free dyeing with favourable fabric characteristics to facilitate the subsequent stages of processing / treatments of fabrics and like to obtain finished products. Yet another object of the present invention is to provide a process of manufacture of the novel organo silicone polymer for use as antifoaming agent and stain free dyeing of fabrics with improved fabric characteristics. Yet further object is to provide an improved process of dyeing and processing of fabrics and the like using the novel organo silicone which would make processing of fabrics in mills and the like, simple and cost-effective. Thus, according to one aspect of the present invention, an organo polysiloxane compound of general formula (I) F9ZhR3-(g+h)SiO(SiR2O)n(SiRYO)mSiR3-(g+h)ZhFg (I) where, R, which may differ, is a monovalent hydrocarbon radical preferably of 1 to 30 carbon atoms and F is a radical of general formula (A) 3 Re(OR5)SiO[4-(e+f)]J/2 (A) where, R5, which may differ, is a hydrogen atom, an alkyl radical preferably of 1 to 4 carbon atoms, an aryl radical or an alkoxyalkyl radical. and Y, which may differ, is a radical of general formula (B) (R2-NA-)Z R4-NR3A (B) where, R2 and R4, which may differ, are divalent hydrocarbon radicals preferably of 1 to 12 carbon atoms per radical, R3, which may differ, is a hydrogen atom or an alkyl radical or an aryl radical and A is an R3 radical or a different alkyl radical or a different aryl radical than R3, where Z, which may differ is a carbinol functional hydrocarbon radical of 1 to 100 carbon atoms per radical subject to the proviso that each molecule of general formula (I) contains at least one Y radical with at least one F radical and the n-units (SiR2O) and the m units (SiRYO) may have any distribution in the molecule. g is 0,1 or 2 ; n is 0 or an integer from 1 to 1000 ; m is 0 or an integer from 1 to 100 ; z is 0 or an integer from 1 to 10, preferably 0 or 1,2,3 ; e is 0,1,2 or 3 ; f is 0,1,2 or 3 ; h is 1,2 or 3 ; (e+f) is 0, 1, 2 or 3 ; (g+h) is1,2 or 3 The organosilicon compounds of the invention are preferably organo polysiloxanes. Preferably The compounds may be represented by the formula as under: The organosilicon compounds of the invention preferably have a viscosity of 50 mPa.s at 25°C to 100000 mPa.s at 60°C, more preferably of 50 mPa.s at 25°C to 10000 mPa.s at 60°C 4 The organosilicon compounds of the invention preferably have a molecular weight (Mn) of 500 g / mol to 1000000 g / mol, more preferably of 500 g / mol to 100000 g/mol. The organosilicon compounds of the invention preferably have an amine number of 0.01 mequiv / g to 4.0 mequiv / g, more preferably 0.1 mequiv / g to 2.0 mequiv /g. The organosilicon compounds of the invention can be present in liquid form. In accordance with another aspect of the present invention, there is provided a process for manufacturing the organo polysiloxane of general formula (I) comprising equilibration of organo polysiloxane with amino silanes in the presence of catalyst. In particular, according to a preferred aspect, the process of the invention comprises a process for manufacturing the organo polysiloxane compound of general formula (I) comprising i) reacting polydimethylsiloxane, alkyl / aryl siloxy ended silicone fluid and amino functional silane in the presence of a catalyst at 120°C to 200°C preferably 120°C to 150° C to obtain silicone polymer substantially free of contaminants, ii) adding the said silicone polymer obtained in (i) above, having OH groups maintaining a reaction temperature of 120°C to 180°C, preferably from 110°C to 120°C in the presence of a catalyst, thereby obtaining the organo pofysiloxane compound of general formula (I). iii) the reaction of the amino fluid and fume / precipitated silica in the above mentioned process is preferably carried out under high speed mixing. The process of the invention is preferably carried out using amino containing organosilicone compounds of general formula (II) 5 RaYcf(OR1)SiO[4-(a+c+d)] 2 (II) where R, which may differ, is a monovalent hydrocarbon radical, R1 which may differ, is a hydrogen atom, an alkyl radical, an aryl radical, an alkoxyalkyl radical or a radical F of the formula (A) Re(OR5)f SiO[4-(e+f)] 2 (A) where R is as defined above R5 which may differ, is a hydrogen atom, an alkyl radical, an aryl radical or an alkoxyalkyl radical Y, which may differ, is a radical of the formula (B) -(R2-NA-)2R4-NR3A (B) where R2 and R 4, which may differ, are divalent hydrocarbon radicals. R3, which may differ, is a hydrogen atom or an alkyl radical or an aryl radical, and A is a R3 radical or a different alkyl radical or an different aryl radical than R3. subject to the proviso that each molecule of formula (I) contains at least one Y radical with at least one F radical. z is 0 or an integer from 1 to 10, preferably 0 or 1,2,3 ; a is 0,1,2 or 3 , c is 0, 1 or 2 ; d is 0.1.2 or 3 ; e is 0, 1,2 or 3 ; f is 0,1,2 or 3 ; e+f is 0,1,2 or 3 and a+c+d is 0.1,2 or 3 R is preferably a monovalent hydrocarbon radical of 1 to 30 carbon atoms 6 Examples of R are alkyl radicals, such as methyl, ethyl, n-propyl, iso propyl, n-butyl, Isobutyl, tert-butyl, n-pentyl, Isopentyl, neopentyl, tert pentyl, hexyl such as n-hexyl, heptyl, such as n-heptyl, octyl, such as n-octyf and isooctyl, such as 2,2,4-trimethyl pentyl, nonyl, such as n nonyl, decyl such as n decyl, dodecyl such as n-dodecyl, octadecyl such as n-octadecy alkenyl, such as vinyl and allyl, cycloalkyl, such as cyclopentyl, cyclohexyl, cycloheptyl and methyl cyclohexyl, aryl such as phenyt, napthyl, anthryl and phenanthryl ; alkylaryl, such as o-, m-, p-totyl, xylyl and ethylphenyl; aralkyl, such as benzyl, ? and ?-phenylanthryl, of which methyl, ethyl, n-propyl, isopropyl are preferred and methyl is particularly preferred. R1 is preferably alkyl of 1 to 4 carbon atoms. Examples of alkyl R1 are methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl and tert butyl, of which methyl and ethyl are preferred. Examples of alkoxyalkyl are methoxyethyl, ethoxyethyl. Examples of aryl are phenyl, napthyl, anthryl and phenanthryl. R5 is same as R1. Examples of alkyl R are also fully applicable to alkyl R3 and R5. R2 and R4 are preferably a divalent hydrocarbon radical of 1 to 12 carbon atoms per radical; Examples of R4 are methylene, ethylene, propylene, butylene, cyclohexylene, octadecylene, phenyiene and butenylene, of which methylene, ethylene and n-propylene are preferred, in particular on account of their convenient obtainibility. Example of Y are H2N(CH2) - ; H2N(CH2)2 - ; NH2 (CH2)3- ; NH2 (CH2)4- ; NH2 (CH2)5- ; NH2 (CH2)2 NH (CH2) - ; NH2 (CH2)2 NH (CH2)3- ; NH2 (CH2)2 NH C(CH3)CH2- ; (CH3)2N(CH2)NH(CH2)3- ; CH3NH(CH2)3- ; H(NHCH2CH2)3- ; C4H9NH(CH2)2NH(CH2)2- and cyclo- C6H11NH (CH2)3-, of which NH2 (CH2)3- ; NH2 (CH2)2 NH (CH2)3- ; NH2 (CH2)2 NH C(CH3)CH2- are particularly preferred. 7 Example of Z are -(CH)3OH; -(CH)4OH; -(CH)2OH; -(CH2CH2O)6H; -(CH2CH2O)8H ; -(CH2CH2O)10H ; -(CH2CH2CH2O)6H ; -(CH2CH2CH2O)8H ; -(CH2CH2CH2O)10H of which -(CH)3OH ; -(CH2CH2O)6H are particularly preferred. The organo silicone compounds obtained following the above process comprise organo polysiloxane compounds of general formula (I) FgZhR3-(g+h)SiO(SiR2O)n(SiRYO)mSiR 3-(g+h) Zh Fg (I) where R, F, Z and Y are each defined above, subject to the proviso that each molecule contains at least one Y radical with at least one F radical and the n-units (SiR2O) and the m-units (SiRYO) may have any distribution in the molecule. The compounds used in the process of the invention have a viscosity preferably from 10mPa.s to 100000 mPa.s at 25°C, more preferably from 50 mPa.s to 10000 mPa.sat60°C. The organosilicone compounds are preferably prepared by equilibration of organopolysiloxanes selected from the group consisting of linear polysiloxanes having terminal triorganosiloxy groups, cyclic organosiloxanes and interpolymers of di-organosiloxane and mono-organosiloxane units with amino silanes, such as ? -aminopropylmethyldimethoxysilane or -aminoethylaminopropyl methyldimethoxysilane, in the presence of catalysts that promote equilibration, more preferably basic catalysts, such as alkali metal hydroxides, e.g {sodium hydroxide or potassium hydroxide) or trimethyl ammonium hydroxide. Depending on the molecular weight of the amino fluid synthesised above and number of hydroxyl groups or alkoxy group at the ends present, fume silica or 8 precipitated silica or alkyl resin or alkyl aryl resin used preferably fumed silica is used to obtain the organo silicon compounds of the invention in liquid form. The process of the invention utilises fume silica or precipitated silica or alkyl resin or alkyl aryl resin in such a amounts that the hydroxyl groups in fume silica or precipitated silica or alkyl resin or alkyl aryl resin is present in a molar ratio of preferably 0.1:1 to 1.2:1 more preferably 0.5:1 to 1:1 to OH attached at the end of the organo silicone compound of general formula (I). The process of the invention is carried out at a temperature of preferably 100°C to 180°C, more preferably 110°C to 150°C and preferably at the pressure of the ambient atmosphere, i.e. at 1020 hPa (absolute). However, the process of the invention can also be carried out at lower pressure, such as 3 hPa to 500 hPa or higher pressure. The process of the invention can be carried out in presence or absence of organic solvents Examples of organic solvents are toluene, xylene, n-heptane and cyclohexane. The organosilicon compounds of the invention can be emulsified and are then present in the form of emulsion. The emulsions are prepared by organo silicone compounds of the emulsion being mixed with emulsifiers, such as neutral or ionic emulsifiers, such as non-ionic or ionic emulsifiers, and water and subsequently emulsified. The preparation of emulsion is known to be one skill of art. The mixing and emulsifying can be carried out in customary mixing apparatus suitable for preparing emulsions such as high speed stator rotor stirrers after Professor P. Willems of the kind known under the registered trademark "Ultra-Turrax" The invention further provides a process for impregnating organic fibers with the organosilicon compounds of the invention. The organo silicon compounds of the invention can be used as softeners during dyeing for textiles, In which case the textiles are impregnated with the organosilicon compounds and simultaneously act as a antifoaming agent. This would achieve the advantages of imparting a 9 soft hand effect to the treated textile, an uniform dyeing, possessing good anchorage on the textiles and stability to yellowing on the textile fabrics. The inventive organosilicon compounds make a cost-effective process in which dyeing and softening can be done in a single step. Now, the dyeing and softening process are carried out in two steps. The inventive process for impregnating organic fibers in the form of filaments, yarns, webs, mats, strands, woven, loop-formingly knitted as have hitherto be impregnable with organosilicon compounds. Examples of impregnable fibers are fibers composed of keratin, especially wool, interpolymers of vinylacetate, cotton, rayon, hemp, natural silk, polypropylene, polyethylene, polyester, polyurethane, polyamide, cellulose, viscose, and mixture of at least two such fibers can be of natural or synthetic origin. The textiles can be present in the form of fabric webs or garments or parts of garments. Application to the fibers to be impregnated by inventive organosilicon compounds can be effected in any manner know to be suitable for Jet dyeing machine, soft flow machine, Jigger with any dyeing system like reactive dyes, vat dyes, dispersive dye. The inventive organosilicon compounds can work at an operating temperature from 20 °C to 150 °C in the machine, preferably temperature from 40°C to 130 °C. The inventive organosilicon compounds can work from ambient temperature to 10 Kg/ cm2 pressure in the machine, preferably from atmospheric pressure to 4 Kg/cm2 pressure. The inventive organosilicone compounds can also work at a pH from 3 to 10, preferably from 5 to 7 during the dyeing operation. The polymer of the invention of formula (I) can be obtained in the liquid form for use especially as an antifoaming agent with favourable fabric finishing softening characteristics during the dyeing process. According to another aspect of the present invention the same provides for a process of manufacture of the organo silicone polymer of formula (I) comprising : 10 i) reacting polydimethyl siloxane, alkyl / alkylsiloxy ended silicone fluid and amino functional silane in the presence of a catalyst at 120°C to 200°C preferably 120°C to 150°C to obtain silicone polymer substantially free of contaminants; ii) adding thereto the said silicone polymer obtained under (i) above, having OH groups maintaining a reaction temperature in the range of 120°C to 180°C, preferably 110°C to 120°C in presence of a catalyst to thereby obtain the amino silicon polymer of formula (II). In the above process, reaction of amino fluid and fume silica / precipitated silica is preferably carried out under high speed mixing. The catalyst suitable for use in the process of the invention can be any commercially available catalyst for silicone polymerisation Preferably, sodium hydroxide or potassium hydroxide or tetramethylammonium hydroxide or any siliconates of these compounds can be used. The objects / advantages of the present invention and its means for attaining are described hereunder in greater detail with reference to non-limiting exemplary embodiments hereunder. Examples Example-1 (without carbinol functional) 4000 gm silanol terminated polydimethylsiloxane having viscosity 80 cps, 50 gm 10 cps trimethylsiloxy terminated siloxane and 40 gm tetramethylammonium siliconate catalyst were reacted in the reactor under nitrogen purging 70 gm ?-Aminoethylaminopropyl methyl dimethoxy silane was added in the reactor under nitrogen purging and continue the reaction for about 6 hr at 120°C. Temperature was gradually increased to 150°C and kept at that temperature for 1 hr to deactivate the catalyst Distilled out the volatile at 150oC under 5 mm Hg pressure, 480 gm of volatile was found as a distillate. Removed the vacuum and started N2 purging 220 gm hydrophobic fumed silica was gradually added in the 11 reactor and continued the reaction for 6 hr. Liquid in the reactor was cooled and taken out from the reactor. Reacted material was passed twice through a More-House mill(grinder) for uniform particle distribution of powder. 3800 gm Light grey colour translucent polymer was obtained having viscosity 2500 Cps and volatile content 2.5%. Si29 NMR confirmed the desired structure of the polymer. Example- 2 (without carbinol functional) 4000 gm silanol terminated polydimethylsiloxane having viscosity 80 cps, 50 gm 10 cps trimethylsiloxy terminated siloxane and 40 gm tetramethylammonium siliconate catalyst were reacted in the reactor under nitrogen purging. 135 gm ?-Aminopropyl Methyl Dimethoxy Silane was added in the reactor under nitrogen purging and continue the reaction for about 6 hr at 120°C. Temperature was gradually increased to 150°C and kept at that temperature for 1 hr to deactivate the catalyst. Distilled out the volatile at 150°C under 5 mm Hg pressure. 480 gm of volatile was found as a distillate. Removed the vacuum and started N2 purging. 220 gm hydrophobic fumed silica was gradually added in the reactor and continued the reaction for 6 hr. Liquid in the reactor was cooled and taken out from the reactor. Reacted material was passed twice through a More-House mill (grinder) for uniform particle distribution of powder. 3850 gm Light grey colour translucent polymer was obtained having viscosity 2700 Cps and volatile content 2.2%. Example-3 (with carbinol functional) 3000 gm silanol terminated polydimethylsiloxane having viscosity 80 cps, 1000 gm ?,? hydroxypropyl polysiloxane (Wacker IM 11) and 40 gm tetramethylammonium siliconate catalyst were reacted in the reactor under nitrogen purging. 70 gm ?-Aminoethylaminopropyl Methyl Dimethoxy Silane was added in the reactor under nitrogen purging and continue the reaction for about 6 hr at 120°C. Temperature was gradually increased to 150°C and kept at that temperature for 1 hr to deactivate the catalyst. Distilled out the volatile at 150°C 12 under 5 mm Hg pressure. 530 of volatile was found as a distillate. Removed the vacuum and started N2 purging. 220 gm hydrophobic fumed silica was gradually added in the reactor and continued the reaction for 6 hr Liquid in the reactor was cooled and taken out from the reactor. Reacted material was passed twice through a More-House mill (grinder) for uniform particle distribution of powder. 3750 gm Light grey colour translucent polymer was obtained having viscosity 1800 Cps and volatile content 2.0%. Example-4 (with carbinol functional) 2000 gm silanol terminated polydimethylsiloxane having viscosity 80 cps, 2000 gm ??? EO ( ethylene oxide)modified polysifoxane ( Wacker IM 22) and 40 gm tetramethylammonium siliconate catalyst were reacted in the reactor under nitrogen purging. 70 gm ?-Aminoethylaminopropyl Methyl Dimethoxy Silane was added in the reactor under nitrogen purging and continue the reaction for about 6 hr at 120°C. Temperature was gradually increased to 150°C and kept at that temperature for 1 hr to deactivate the catalyst. Distilled out the volatile at 150°C under 5 mm Hg pressure. 580gm of volatile was found as a distillate. Removed the vacuum and started N2 purging. 220 gm hydrophobic fumed silica was gradually added in the reactor and continued the reaction for 6 hr. Liquid in the reactor was cooled and taken out from the reactor. Reacted material was passed twice through a More-House mill (grinder) for uniform particle Jtstribution of powder. 3700 gm Light grey colour translucent polymer was obtained having viscosity 2000 Cps and volatile content 3%. Example-5 (without catalyst) 2000 gm silanol terminated polydimethylsiloxane having viscosity 80 cps and 2000 gm ??? EO ( ethylene oxide) modified polysiloxane ( Wacker IM 22) were reacted in the reactor under nitrogen purging. 70 gm ?-Aminoethylaminopropyl Methyl Dimethoxy Silane was added in the reactor under nitrogen purging and continue the reaction for about 6 hr at 120°C. Temperature was gradually 13 increased to 150°C and kept at that temperature for 1 hr to deactivate the catalyst. Distilled out the volatile at 150°C under 5 mm Hg pressure. No volatile was found as a distillate. Cool down the reactor and fluid from the reactor was taken out. A white immiscible fluid was found. 50 gm fluid was centrifuse at 3000 rpm for 10 min. We found a clear separation in the centrifuge tube where top layer was PDM and bottom layer IM22. Therefore, no volatile was due to no reaction taken place in absence of catalyst. Here, all the inputs are non volatile and generally volatile is generated during equilibrium reaction in presence of catalyst and as reaction goes on, feed mixture become more and more clear. So, it is clear, catalyst presence in the reaction mixture is the must for the reaction. Emulsions were obtained using the polymer of Examples 1,2,3 and 4 above as detailed under TABLE I. The series of Emulsions in TABLE I were made using same emulsifiers with and without the polymer of the invention. TABLE I Example? E1 (gm) E2 (gm) E3 (gm) E4 (gm) E5 (gm) E6 (gm) Polymer of EX-1 230 Polymer of EX-2 230 Polymer of Ex-3 230 Polymer of Ex-4 230 Searyl Alcohol, 20 EO 82 82 82 82 82 82 Searyl alcohol 19 19 19 19 19 19 Acetic acid 7 7 7 7 7 7 Amino oil(Wacker AM-1) 230 230 Antifoam compound Water 810 810 810 810 810 810 Fungicide 5 5 5 5 5 5 14 The antifoaming and other related characteristics of the above emulsions of the invention having the novel polymer (Examples E4 and E5), other polymers without carbonyl group (Examples 1 and 2) and the emulsion E1 and E6 without incorporation of the novel polymer were tried each on 1200 M polyester fabric in jet-dyeing machine. Process : Protocol followed as hereunder : First, 500 Kg DM water introduced into the jet dyeing machine through a metering pump. After desizing and scouring, raw fabric loaded in the Jet-dye machine. Temperature inside liquid of the machine raised to 80°C and added dispersing dye, dispersing agent, EDTA into the machine from the feeding tank where all these chemicals pre-diluted with hot water. Machine was run for ten minutes with fabrics and allowed for thorough mixing of the dye with other ingredients. pH of the liquid was adjusted to 5 by acetic acid. 1 Kg E 2 emulsion of the invention was pre-diluted in feed in with 30 Kg water and feed to the machine. All flanges in the machine were then closely tied and temperature in the machine was raised to 120°C under high speed rotary movement of the fabric in the machine. Pressure inside the machine was maintained to 2.5-3 Kg/cm2. The total run was continued for 45 min and then the liquid inside the machine was cooled to 60°C. Drained the liquid inside the machine and took out fabric from the machine. Fabric was then cured at 100-110°C in a 20M stentor having temperature 100°C. Similarly, the same fabric treatment was done with E1, E3, E4, E5 and E6 emulsion of in the same machine. The antifoam characteristics of the emulsions of the E2, E3, E4, E5 and the conventional emulsions (E1 and E6) and fabric characteristics achieved in use of such emulsions in dying process were studied and the results are represented in accompanying Figures 1, 2, 3, 4, 5, 6, 7, 8 and 9. 15 From the above Figures (graphs), it is clear that silicone polymer emulsion of F2. E3. E4 and E5 using the polymer of the present invention showed comparable antifoam characteristics as that of conventional emulsion F6 but the emulsions E2, E3, E4 and E5 impart comparable softness to standard amino emulsion E1. We also observed emulsions of novel polymer E4 and E5 did not impart any unwanted stains on the fabric while the emulsions E1, E2, E3 and E6 caused substantial stains on the fabric. Notably, the fabric finish/quality achieved in use of emulsions having polymer of the novel invention (E 4 and E5) during dyeing was also found to be superior as would be evident from the data revealing gloss and softness characteristics of the treated fabrics Importantly, the above exemplary processes further reveal that use of the polymer emulsion of the invention as an antifoam agent during dyeing can apart from avoiding the staining of fabrics provide for favourable beneficial characteristics in the fabric for subsequent processing and/or finishing of fabrics. Thus the novel antifoam polymers of the invention which is about 30% less expensive than the dynamic silicon antifoam but favour stain free dyeing of fabrics simultaneously softening of the fabric is directed to make the processing of fabrics simple and cost-effective without affecting quality and character of the fabrics. WE CLAIM : 1. A process for manufacturing the organo polysiloxane compound of general formula (I) FgZhR3-(g+h)SiO(SiR2O)n(SiRYO)mSiR3-(g+h)ZhFg (I) where, R, which may differ, is a monovalent hydrocarbon radical preferably of 1 to 30 carbon atoms and F is a radical of general formula (A) Re(OR5)f SiO [ (4-(e+f)] /2 (A) where, R5, which may differ, is a hydrogen atom, an alkyl radical preferably of 1 to 4 carbon atoms, an aryl radical or an alkoxyalkyl radical and Y, which may differ, is a radical of general formula (B) (R2-NA-)z R4-NR3A (B) where, R2 and R4, which may differ, are divalent hydrocarbon radicals preferably of 1 to 12 carbon atoms per radical, R3, which may differ, is a hydrogen atom or an alkyl radical or an aryl radical and A is an R3 radical or a different alkyl radical or a different aryl radical than R3 where Z which may differ is a carbinol functional hydrocarbon radical of 1 to 100 carbon atoms per radical subject to the proviso that each molecule of general formula (I) contains at least one Y radical with at least one F radical and the n-units (SiR2O) and the m units (SiRYO) may have any distribution in the molecule. 16 g is 0,1 or 2 ; n is 0 or an integer from 1 to 1000, and m is 0 or an integer from 1 to 100 ; z is 0 or an integer from 1 to 10, preferably 0 or 1,2,3 ; e is 0,1,2 or 3 and ; f is 0,1,2 or 3 ; h is 1,2 or 3; (e+f) is 0, 1,2 or 3 ; (g+h) is1,2 or 3 comprising equilibration of organo polysiloxane with amino silanes in the presence of catalyst. 2. A process as claimed in claim 1 wherein R in the organo polysiloxane compound of general formula (I) thus formed are alkyl radicals comprising methyl, ethyl, n-propyl, iso-propyl, n-butyl, iso-butyl, tert-butyl, n-pentyl iso- pentyl, neo-pentyl, tert-pentyl, hexyl preferably n-hexyl, heptyl preferably n- heptyl, octyl n-octyl and iso-octyl 2,2,4-trimethyl pentyl, nonyl preferably n- nonyl, decyl preferably n-decyl, dodecyl n-dodecyl, octadecyl preferably n- octadecyl; alkenyl preferably vinyl and allyl; cycloalkyl preferably cyclopentyl, cyclohexyl, cycloheptyl and methyl cyclohexyl; aryl preferably phenyll, napthyl, anthiryl and phenanthryl; alkylaryl preferably o-, m-, p-tolyl, xylyl and ethylphenyl; aralkyl preferably benzyl, alpha- and beta-phenylethyl; preferably methyl, ethyl, n-propyl, isopropyl and more preferably methyl. 3. A process as claimed in claim anyone of claims 1 to 2 wherein R5 in the organo polysiloxane compound of general formula (I) thus formed comprises alkyl radicals preferably methyl, ethyl, n-propyl, iso-propyl, n-butyl and tertbutyl and more preferably methyl and ethyl, alkoxyalkyl radicals preferably methoxy ethyl and ethoxy ethyl, aryl radicals preferably phenyl, napthyl, anthryl and phenanthryl. 4. A process as claimed in anyone of claims 1 to 3 wherein R2 and R4 in the organo polysiloxane compound of general formula (I) thus formed are divalent hydrocarbon radicals comprising methylene, ethylene, propylene, butylene, cyclohexylene, octadecylene, phenylene and butenylene preferably methylene, ethylene and n-propylene. 17 5. A process as claimed in anyone of claims 1 to 4 wherein said the ? in the organo polysiloxane compound of general formula (I) thus formed is selected from NH2(CH2)-, NH2(CH2)2-, NH2(CH2)3-, NH2(CH2)4-, NH2(CH2)5-, NH2(CH2)2NH(CH2)3-, NH2(CH2)2NH(CH2)-, NH2(CH2)2NHC(CH3)CH2-, (CH3)2N(CH2)NH(CH2)3-, (CH3)NH(CH2)3-, H(NHCH2CH2)3-, (C4H9)NH(CH2)2NH (CH2)2- and cyclo-(C6Hn)NH(CH2)3 preferably NH2(CH2)3- , NH2(CH2)2NH(CH2)3-and NH2(CH2)2NHC(CH3)CH2- 6. A process as claimed in anyone of claims 1 to 5 where the said Z in the organo polysiloxane compound of general formula (I) thus formed is selected from -(CH)3OH, -(CH)4OH, -(CH)2OH, -(CH2CH2O)6H, -(CH2CH2O)8H, -(CH2CH2O)10H, -(CH2CH2CH2O)8H, -(CH2CH2CH2O)8H, (CH2CH2CH2O)10H, preferably -(CH)3OH, -(CH2CH2O)6H. 7. A process as claimed in anyone of claims 1 to 6 wherein the organo polysiloxane compound of general formula (I) thus formed preferably have a viscosity of 50 mPa.s at 25°C to 100000 mPa.s at 60°C and more preferably of 50 mPa.s at 25°C to 10000 mPa.s at 60°C. 8. A process as claimed in anyone of claims 1 to 7 wherein the organo polysiloxane compound of general formula (I) thus formed preferably have a molecular weight of 500 g / mol to 1000000 g / mol and more preferably of 500 g / mol to 100000 g / mol. 9. A process as claimed in anyone of claims 1 to 8 wherein the organo polysiloxane compound of general formula (I) thus formed preferably have an amine number of 0.01 mequiv / g to 4 mequiv / g and more preferably of 0.1 mequiv / g to 2.0 mequiv / g. 18 10. A process as claimed in anyone of claims 1 to 9 wherein the organo polysiloxane compound of general formula (I) thus formed can be present in the liquid form. 11. A process as claimed in anyone of claims 1 to 10 wherein the said amino silanes used comprise ? - aminopropylmethyld imethoxy silane or ?- -amino ethylaminopropylmethyldimethoxy silane. 12. A process as claimed in anyone of claims 1 to 11 wherein the said catalyst used comprises catalysts that promote equilibration preferably basic catalysts (including metal hydroxides) or trimethyl ammonium hydroxide or any siliconates of these compounds to thereby obtain the organo polysiloxane compound of general formula (I). 13. A process as claimed in claim 12 wherein the catalysts used are catalysts for silicone polymerisation preferably basic catalysts such as sodium hydroxide, potassium hydroxide, tetramethyl ammonium hydroxide or any siliconates thereof. 14.A process as claimed in anyone of claims 1 to 13 wherein depending upon the molecular weight of the amino fluid synthesised above and the number of hydroxyl groups or alkoxy groups at the ends present, fume silica or precipitated silica or alkyl resin of alkyl aryl resin is used, preferably fumed silica to obtain the organo silicon compound in the liquid form. 15. A process for manufacturing the organo polysiloxane compound as claimed in anyone of claims 1 to 14 comprising i) reacting polydimethyl siloxane, alkyl/aryl siloxy ended silicone fluid and amino functional silane in the presence of a catalyst at 120°C to 19 200°C preferably 120°C to 150° C to obtain silicone polymer substantially free of contaminants ; ii) adding the said silicone polymer obtained in (i) above, having OH groups maintaining a reaction temperature of 120°C to 180°C, preferably 110°C to 120°C in the presence of a catalyst, thereby obtaining the organo polysiloxane compound of general formula (I), the reaction of the amino fluid and fume / precipitated silica in the being preferably carried out under high speed mixing. 16. A process for manufacturing the organo polysiloxane compound as claimed in anyone of claims 1 to 15 comprising using fume silica, or precipitated silica in such amounts that the hydroxyl groups in fume silica or precipitated silica or alkyl resin or alkylaryl resin is present in a molar ratio of 0.1:1 to 1.2:1, more preferably 0.5:1 to 1:1 to OH attached at the end of the organo polysiloxane compound of general formula (I). 17.A process for manufacturing the organo polysiloxane compound as claimed in anyone of claims 1 to 16 wherein it is carried out at a temperature of preferably 100°C to 180°C, more preferably 110°C to 150°C, and at lower pressure, of 3 hPa to 500 hPa or higher pressure preferably at the pressure of the ambient atmosphere at 1020 hPa (absolute). 18. A process for manufacturing the organo polysiloxane compounds as claimed in anyone of claims 1 to 16 carried out in the presence or absence of organo solvents. 19. A process as claimed in claim 18 where the said organo solvents used are preferably toluene, xylene, n - heptane and cyclo hexane. 20 20. A process of treating fibers to produce softened and dyed fibers comprises impregnating the fibers in an emulsion of the organo polysiloxane compound of general formula (I). 21. A process as claimed in claim 20 wherein the organo fibers to be impregnated are in the form of webs, mats, filaments, yarns, strands, woven, loop formingly knitted have to be impregnable with organo silicon compounds. 22. A process as claimed in anyone claims 20 to 21 wherein the fibbers to be impregnated are fibers composed of keratin (especially wool), interpolymers of vinylacetate, cotton, rayon, hemp, natural silk, polypropylene, polyethylene, polyester, polyurethane, polyamide, cellulose, viscose and mixture of at least two such fibers of natural or synthetic origin. 23.A process as claimed in anyone of claims 20 to 21 wherein the fibbers comprise textile materials in the form of fabric webs or garments or parts of garments. 24. A process as claimed in anyone of claims 20 to 22 wherein the fibbers are impregnated in said compound of general formula (I) using any one or more of conventional dyeing machines preferably Jet dyeing machine, soft flow machine, Jigger machine with any dyeing system selected from reactive dyes, vat dyes, dispersive dyes. 25. A process as claimed in anyone of claims 20 to 23 wherein said steps of impregnated is carried out a temperature ranging from 20°C to 150°C preferably from 40°C to 130°C, at pressure ranging from ambient pressure to 10 kg / cm2 preferably from atmospheric pressure to 4kg / cm2 at pH from 3 to 10 preferably from 5 to 7 during the dyeing operation. 21 26. A process of manufacture of organo polysiloxane compound of general formula (I), and method of treating fibres with emulsion of said organo polysiloxane compound substantially as herein described and illustrated with reference to the accompanying examples/figures. A new organo-silicone polymer which would be effective as an antifoaming agent for dyeing of fabrics and the like. The organo-silicone polymer is obtained by equilibration of organo polysiloxane with amino silanes in the presence of catalyst. In particular, the process involves (i) reacting polydimethytsiloxane, alkyl / aryl siloxy ended silicone fluid and amino functional silane in the presence of a catalyst to obtain silicone polymer substantially free of contaminants, and (ii)adding the said silicone polymer obtained in (i) above, having OH groups maintaining a reaction temperature of 120°C to 180°C, preferably from 110°C to 120°C in the presence of a catalyst, thereby obtaining the organo polysiloxane compound of general formula (I). The organo silicone polymer would be cost-effective and would essentially avoid the problems of deposition of silicone oil in the walls of the dyeing machine to favour stainfree dyeing of fabrics in a cost-effective manner to meet the demands of mills. The polymer would be useful as an antifoaming agent in dyeing process which would favour stain free dyeing with favourable fabric characteristics to facilitate the subsequent stages of processing / treatments of fabrics and like to obtain finished products. The polymer would further provide for improved and cost-effective process of dyeing and processing of fabrics and the like.

Documents:

00531-cal-2000-abstract.pdf

00531-cal-2000-claims.pdf

00531-cal-2000-correspondence.pdf

00531-cal-2000-description(complete).pdf

00531-cal-2000-drawings.pdf

00531-cal-2000-form-1.pdf

00531-cal-2000-form-18.pdf

00531-cal-2000-form-2.pdf

00531-cal-2000-form-3.pdf

00531-cal-2000-form-5.pdf

00531-cal-2000-letters patent.pdf

531-CAL-2000-(09-03-2012)-FORM-27.pdf