Title of Invention	NOVEL CONCENTRATED AQUEOUS SURFACTANT COMPOSITIONS AND THEIR PREPARATION
Abstract	A process for the preparation of pourable surface composition having high solid content comprising the steps of (iii) Adding the amido amine into anionic surfactant, (iv) adding sodium monochoroacetate to the mixture of step (i) to from surfactant composition; wherein the said surfactant composition consists of amphoteric and anionic surfactant.

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FORM2 THE PATENTS ACT, 1970 (39 of 1970) & The Patents Rules, 2003 COMPLETE SPECIFICATION (See section 10; rule 13) 1. Title of the invention. - Novel concentrated aqueous surfactant compositions and their preparation. 2. Applicant(s) (a) NAME : GALAXY SURFACTANTS LTD. (b) NATIONALITY: INDIAN (c) ADDRESS : C-49/2, TTC Industrial Area, Pawne, Navi-Mumbai 400 703, Maharashtra, India. 3. PREAMBLE TO THE DESCRIPTION: The following specification particularly describes the invention and the manner in which it is to be performed: FIELD OF INVENTION The present invention relates to a process for the preparation of pourable surfactant composition having high concentration of solids. The present invention particularly relates to a process for the preparation of pourable surfactant composition in which amphoteric surfactant is synthesized in anionic surfactant thereby increasing the total solid content above 70 %. BACKGROUND OF THE INVENTION Surfactants are organic compounds that are amphipathic, meaning they contain both hydrophobic groups and hydrophilic groups. Therefore, they are typically sparingly soluble in both organic solvents and water. Surfactants reduce the surface tension of water by adsorbing at the air-water interface. They also reduce the interfacial tension between oil and water by adsorbing at the liquid-liquid interface. Many surfactants can also assemble in the bulk solution into aggregates that are known as micelles. Surfactants find application in many fields like personal care, oil recovery, r pharmaceutical, agrochemicals etc. Combination of different’ surfactants are used in personal care products like shampoo, liquid soap, bubble bath, etc and in home care products like dish wash, liquid detergent etc. to get required performance and aesthetic value. Characteristic behaviour of the surfactants in aqueous solution is due to micelle formation. The concentration at which surfactants begin to form micelles is known as the critical micelle concentration or CMC. When micelles form in water, their tails form a core that is like an oil droplet, and their heads form an outer shell, or corona, that maintains favourable contact with water. When surfactants 2 assemble in oil, the aggregate is referred to as a reverse micelle. In a reverse micelle, the heads are in the core and the tails maintain favourable contact with oil.. Surfactants behave differently at different concentration e.g. Fatty alcohol ether sulphate below 35% active matter are flowable, above 35% active matter up to 68% are non-flowable, at 68-72 % active matter again it is flowable. High active fatty alcohol sulphates and AOS are flowable above 60° C. Combination of many amphoteric surfactants like imidazoline mono and dicarboxylate and cocoamido propyl betain, with anionic surfactants like Sodium lauryl ether sulphate, Alfa olefin sulfonate, linear alkyl benzene sulfonate etc. is available in the market. Various attempts have been made in the prior art to prepare flowable high concentrate surfactants. Among these most common method is using lower alcohols like ethanol, methanol, IPA, propylene glycol, but this increases the cost of the product and risk of fire hazard. US Patent 4243549 describes a pourable aqueous surfactant composition comprising a combination of amphoteric and anionic surfactant. The process comprises heating and evaporating of water from low active surfactants. Heating and evaporation of water from low active surfactants is costly and cumbersome moreover it leads to foaming, gel formation, splitting of product resulting in high-level impurities like non- detergent organic matter, dioxane etc. US Patent 4440665 discloses an aqueous surfactant composition consisting substantially of at least 20 % and not more than 55 % (preferably not more than 45 %) by weight of water and active mixture consisting of at least 5 % by weight of said mixture of first amphoteric surfactant and at least 5 % by weight of said mixture of first amphoteric surfactant with at least 5 % by weight of said mixture of at least one non ionic surfactant and / or at least one amphoteric surfactant, non homologous with said first amphoteric surfactant said mixture in the 3 presence of water exhibiting a G phase and concentration of said mixture corresponding to that at which the composition can exist, at least predominantly in G phase. The aqueous surfactant composition of US 4440665 is mixtures of surfactants that form a fluid lamellar G phase within a narrow range of concentration. US 4440665 teach a combination of amphoteric and non-ionic surfactant, but the non-ionic surfactant becomes an unnecessary ingredient in some of the formulations where it is not required. For e.g. in some of the personal care product formulations like shampoo, non-ionic surfactants reduce foaming, which is a desired attribute. In some formulations, they may reduce the anti- microbial activity of preservatives like parabens. US Patent 4832871 discloses a method for the preparation of a flowable and pump able solution, which contains at least 70 weight percent of a betaine. The method comprises quaternization of a betaine in the presence of an alcohol. The use of alcohol not only increases the cost of the product but also increases the risk of fire hazard. US Patent 4861517 describes a method of preparation of flowable aqueous solutions of betaines with a solids content of 43 to 65% by weight and a betaine content of 37 to about 55% by weight. The method comprises addition of mineral acid into aqueous flowable betaine solutions But this process is very cumbersome and costly moreover the neutralization of the product obtained by the quaternization with mineral acid is necessary before use in personal care products. US Patent 5354906 describes an aqueous liquid solution of a betaine. The process comprises quaternizing a mixture of fatty acid amide with chloro acetic acid, using fatty acids and glycerol optionally. There is no additional benefit of addition of these ingredients. The fatty acid reduces foaming in the formulations 4 where it is actually desired; moreover the maximum solids, which can be reached, are 45% even after using these additives. US Patent 6207629 discloses concentrated aqueous betaine type surfactant compositions which include as fluidising additives dimers of fatty acids and/or phosphoric esters of fatty alcohols or polyethoxylated fatty alcohols. The process provides betaine type surfactant compositions having a high concentration, in a flowable liquid state by using such fluidizing additives, which does not have any particular function in the claimed formulation. US Patent 6335370 describes a composition containing an alkylamidopropylbetaine salt, water and ethanol inz` the form of fluid solutions. The process of preparing this surfactant composition comprises preparing intermediate coconut or palm oil dimethylamidopropylamides and in quaternizing them with monochloroacetic acid in the presence of sodium hydroxide or with sodium monochloroacetate in water/ethanol solvent medium. US Patent 6335370 discloses a concentrated aqueous alcoholic, low viscosity, clear, relatively colourless solutions, which are stable between the temperature ranges of 5 to ,50 degree. C and which contain at least 50 % by weight of alkylamidopropylbetaine. Here concentrated flowable alkylamidopropyl betain is also manufactured by carrying out quaternization in presence of alcohol, IPA etc. In the prior art processes surfactant composition having high solid content is prepared by evaporating the solvent. The quaternization reaction is carried out in presence of alcohol or with addition of some additives like glycerol, fatty acids, dimeric acids etc which increases the hazards on industrial scale as well as cost of the product. It also increases the impurities. 5 None of the prior art processes disclosed teaches the synthesis of amphoteric surfactant is synthesized in anionic surfactant in the quatemization reaction thereby increasing the total solid contents of the surfactant composition. OBJECT OF INVENTION It is thus an object of the present invention to provide a process for the preparation of pourable surfactant composition in which amphoteric surfactant is synthesized in anionic surfactant in the quarternization reaction giving a high concentration of surfactant with above 60 % of surfactant activity and which is free from undesirable impurities. It is further object of the present invention to provide a process for the preparation of pourable surfactant composition, which is cost effective. It is further object of the present invention to provide a process for the preparation of pourable surfactant composition, which does not require preservatives, as it is self-preservative. Yet another object of the present invention to provide a process for the preparation of pourable surfactant composition, which does not use alcohol thereby reducing the risk of fire hazard. SUMMARY OF INVENTION According to an aspect of the present invention there is provided a process for the preparation of pourable surfactant composition comprising steps of (i) Adding the amido amine into anionic surfactant, (ii) Adding sodium monochoroacetate to the mixture of Step (i) to form surfactant composition; 6 wherein the said surfactant composition consists of amphoteric and anionic surfactant. According to another aspect of the present invention there is provided a surfactant composition comprising an anionic and amphoteric surfactant; wherein the total solid contents of the surfactant composition is above 70 %. DETAILED DESCRIPTION Viscosity of surfactant compositions is a problem, which affects its pourability characteristics. Viscosity of an aqueous surfactant composition increases as the concentration increases. It has been found that as the total concentration of active ingredient in a dilute solution approaches a critical level, which is usually about 30% by weight, the viscosity of the solution begins to rise, causing difficulty in preparing and handling the solution. At the critical level the solution sets into an immobile gel or phase separation occurs. It is well known that solutions of betaines are liquid only below a particular concentration of total solids, which depends on the fatty acids or fatty acid mixture used for their preparation. For example a solution of a betaine derived form coconut fatty acids solidifies at a solids content of about 40% by weight. For this reason conventional commercial aqueous solutions of coconut amidopropyl betaine derived from coconut fat have total solids concentrations which are clearly below 40% by weight and in most cases about 35% by weight. The maximum achievable concentration of a still flowable solution of a betaine decreases as the number of carbon atoms is increased. A conventional commercial betaine solution has some definite percentage of impurity. Like if in a particular surfactant composition aminoamide has been used which has been obtained by the reaction of the fatty acids with 3-N, N-dimethyl aminopropylamine, and residual amounts of fatty acids will be present. If the 7 aminoamide has been synthesized from fats and 3-N, N-dimethyl aminopropylamine, portions of fatty acids and even glycerine will be present. A small amount of aminoamide is also normally there in the final composition because the reaction of the fatty amide with the tertiary amino groups like aminoamide and sodium chloro acetate is incomplete. Some of the methods involve mineral acids for the quaternization process which will also be present in traces in final composition and its use may be really hazardous in skin care products. Thus all the methods mentioned in the prior art employ such ingredients, which have their own drawbacks. The present inventors have invented the process for the preparation of surfactant composition having high percentage of solids in which amphoteric surfactant is synthesized in anionic surfactant during quaternization reaction thereby increasing the total solid contents of the surfactant composition. Thus according to present invention the process for the preparation of surfactant composition comprises following steps: (I) Fatty acid is reacted with amido propyl dimethyl amine to form fatty amido propyl dimethyl amine (II) fatty amido propyl dimethyl amine formed in step (I) is heated up to 65°C and then reacted with anionic surfactant, (Ill) In the mixture of step (li) sodium monochloroacetate is added slowly while stirring and the temperature is maintained at 80-85°C. Maintain the pH is maintained at 7.5 to 8.2 by adding caustic lye (47%). (IV) Temperature of mixture of step (III) is increased up to 95°C. The reaction is continued for about 8 hours. The pH of the mixture is maintained 10 -10.5 during the course of reaction. (V) Adjust the pH of the mixture of step (III) at 5.5 to 6.5 with sulphuric acid. 8 According to present invention amphoteric surfactant used has minimum 40 % of surfactant activity. Amphoteric surfactant used is selected from imidazoline mono and dicarboxylate and cocoamido propyl betain. The amphoteric surfactant used is preferably betaine of Formula (I). Preferably concentration of amphoteric surfactant is about 25% to about. 45%. 9 According to the present invention anionic surfactant used has minimum 5 % surfactant activity. The anionic surfactant is selected from fatty alcohol sulfates, and alkyl sulfonates. The anionic surfactant used is preferably sodium lauryl ether sulfate, sodium salt of alkyl benzene sulfonate, sodium salt of alpha olefin sulfonate. Preferably concentration of anionic surfactant used is about 5% to about 20% According to present invention amphoteric and anionic surfactant are selected such that the total surfactant activity of the composition is above 60 %. Advantages of the present invention: • Amphoteric surfactant is synthesized in anionic surfactant during quaternization reaction which increases the solid content of the product with required flowability. • Impurities formed e.g. MCA, NDOM and Dioxane is at very low level. • Cost of production is less. • It does not employ the use of hazardous solvents thereby making the overall process safe. The details of the invention, its objects and advantages are explained hereunder in greater details in relation to non-limiting exemplary illustrations. The examples are merely illustrative and do not limit the teaching of this invention and it would be obvious that various modifications or changes in the procedural steps by 10 those skilled in the art without departing from the scope of the invention and shall be consequently encompassed within the ambit and spirit of this approach and scope thereof. EXAMPLES: Example 1: To a stirred mixture of cocofatty acid amidoamine (340 g,87 %, 13% water), sodium salt of alpha olefin sulfonate (38 g, 94.0 %) at 65°C, sodium monochloroacetate (267 g, 43.91%, 1.03 moles) was added over the period of half an hour. The reaction mixture was stirred for 8 hours at 80 - 85°C by maintaining the pH between 7.5 to 8.2 with sodium hydroxide (47 % aqueous solution). ,cocofatty acid ( 35 g) was then added to reaction mixture and stirring was continued for 8 hours at 95°C while maintaining pH between 10 - 10.5. The pH adjusted to 5.5 to 6.5 with sulphuric acid. The flowable viscous product (700 g) so formed had the following composition. Solids 70.28 % Betaine 47.96 % AOS 5.10% NaCI 8.56 % Fatty acids 5.35 % Amidoamine 0.87% Other impurities 2.44 % Water 29.72 % Sodium monochloroacetate pH 6.2 Solidification Point 28°C 11 Example 2: To a stirred mixture of coco fatty acid amidoamine (100 g,), sodium salt of alkyl 2 mole ether sulfate (64 g, 70.09 % ) and water (96 ml) under nitrogen at 65°C, sodium mono chloro acetate (40 g, 98%, 1.03 moles) was added over the period of half an hour. The reaction mixture was stirred for 8 hours at 80 - 85°C by maintaining the pH between 7.5 to 8.2 with sodium hydroxide (47 % aqueous solution) and stirring was continued for 8 hours at 95°C while maintaining pH between 10 - 10.5. The pH adjusted to 5.5 to 6.5 with sulfuric acid. The flow able viscous product (300g) so formed had the following composition. Solids 61.20% Betaine 38.23 % SLES2 mole 12.00% NaCI 6.64 % Fatty acids 0.80 % Amidoamine 0.82 % Other impurities 3.63% Water 38.80 % Dioxane 14.2 ppm SMCA pH 6.2 Pour point > 24 °C Example 3: To a stirred mixture of coco fatty acid amido amine (100g,), sodium salt of alpha olefin sulfonate (120g, 37.3%) and water (40 ml) under nitrogen at 65°C, sodium monochloro acetate (40 g, 98%, 1.03 moles) was added over the period of half an hour. The reaction mixture was stirred for 8 hours at 80 - 85°C by 12 maintaining the pH between 7.5 to 8.2 with sodium hydroxide (47 % aqueous solution).Stirring was continued for 8 hours at 95°C while maintaining pH between 10 - 10.5. The pH was adjusted to 5.5 to 6.5 with sulfuric acid. The flow able viscous product (300 g) so formed had the following composition. Solids 62.74 % Betaine 38.13% AOS 15.20% NaCI 6.71 % Fatty acids 0.80 % Amidoamine 0.70 % Other impurities 2.0 % Water 37.26 % Sodium monochloroacetate pH 6.2 Pour point > 28 °C Example 4: To a stirred mixture of cocofatty acid amidoamine (100g,), sodium salt of alkyl benzene sulfonate (162g,.34.28 %) at 65°C, sodium monochloro acetate (40g, 98%, 1.03 moles) was added over the period of half an hour. The reaction mixture was stirred for 8 hours at 80 - 85°C by maintaining the pH between 7.5 to 8.2 with sodium hydroxide (47 % aqueous solution).Stirring was continued for 8 hours at 95°C while maintaining pH between 10 - 10.5. The pH was adjusted to 5.5 to 6.5 with sulfuric acid. The flow able viscous product (300 g) so formed had the following composition. Solids 66.54 % Betaine 38.73 % LABS 18.40% NaCI 6.80 % Fatty acids 0.80 % 13 Amidoamine 0.70% Other impurities 2.0 % Water 33.46 % Sodium monochloro acetate PH 6.2 Pour point > 28 ° C Example 5: To a stirred mixture of cocofatty acid amidoamine (1150 g, 87 % , 13% water), sodium salt of alpha olefin sulfonate (1255 g, 37.3 %) at 65°C, sodium monochloro acetate (402 g, 98%, 1.03 moles) was added over the period of half an hour. The reaction mixture was stirred for 8 hours at 80 - 85°C by maintaining the pH 7.5, to 8.2 with sodium hydroxide (47 % aqueous solution), cocofatty acid ( 85 g) was then added to reaction mixture and stirring was continued for 8 hours at 95°C while maintaining pH between 10 - 10.5. The pH was adjusted to 5.5 to 6.5 with surphuric acid. The flowable viscous product (2962 g) so formed had the following composition. Solids 66.54 % Betaine 38.78 % AOS 15.19% NaCI 6.94 % Fatty acids 3.25 % Amidoamine 0.47 % Other impurities 3.04 % Water 33.46 % Sodium monochloro acetate pH 6.2 Pour point >28°C 14 Example 6: To a stirred mixture of cocofatty acid amidoamine (340 g,87 %) and sodium salt of alpha olefin sulfonate (56 g, 94.0 %) at 65°C, sodium monochloroacetate (267 g, 43.91%, 1.03 moles) was added over the period of half an hour. The reaction mixture was stirred for 8 hours at 80 - 85°C by maintaining the pH between 7.5 to 8.2 with sodium hydroxide (47 % aqueous solution). Cocofatty acid (35 g) was then added to reaction mixture and stirring was continued for 8 hours at 95°C while maintaining pH between 10 - 10.5. Then pH was adjusted to 5.5 to 6.5 with sulfuric acid. The flow able viscous product (700 g) so formed had the following composition. Solids 72.70 % Betaine 47.96 % AOS 7.52 % NaCI 8.56 % Fatty acids 5.35 % Amidoamine 0.87 % Other impurities 2.44 % Water 27.30 % Sodium monochloro acetate pH 6.2 Pour point > 34 °C Example 7: To a stirred mixture of experiment no. 4 (72 gm) added sodium salt of alkyl 2 mole ether sulfate (43 g, 70.09 %). pH was adjusted to 6.5 to 7.5 with sulfuric acid. The flow able viscous product (115 g) so formed had the following composition 15 Solids 68.37 % Betaine 24.28 % SLES 26.51 % AOS 9.51 % NaCI 4.34 % Fatty acids 2.05 % Amidoamine 0.29% Other impurities 1.68% Water 31.63% Sodium monochloro acetate pH 7.2 Pour point >14°C Example 8: To a stirred mixture of cocofatty acid amidoamine (335 g ), sodium salt of alpha olefin sulfonate (192 g, 94.05 .%), cocofatty acid ( 30 g ), water (20 ml) at 65°C, sodium monochloroacetate (323 g 40%, 1.03 moles) was added over the period of half an hour. The reaction mixture was stirred for 8 hours at 80 - 85°C by maintaining. the pH 7.5 to 8.2 with sodium hydroxide (47 % aqueous solution). Stirring was continued for 8 hours at 95°C while maintaining pH between 10 -10.5. The pH was adjusted to 5.5 to 6.5 with sulphuric acid. The flowable viscous product (900 g) so formed had the following composition. Solids 72.17% Total Surfactant 60.00 % Betaine 42.00 % AOS 20.00 % NaCI 7.29 % Fatty acids 3.45 % Amidoamine 0.57 % 16 Other impurities 0.86 % Water 27.83% Sodium monochloroacetate 5 ppm pH 6.2 Pour point > 32 °C Solidification Point 24 °C 17 We Claim: 1. A process for the preparation of pourable surfactant composition having high solid content comprising the steps of (ii) Adding the amido amine into anionic surfactant, (iii) Adding sodium monochoroaeetate to the mixture of Step (i) to form surfactant composition; wherein the said surfactant composition consists of amphoteric and anionic surfactant. 2. The preparation of pourable surfactant composition as claimed in claim 1 wherein the amphoteric surfactant is synthesized in anionic surfactant. 3. The process as claimed in claim 1 wherein the said amidoamine is fatty amido propyl dimethyl amine. 4 The process as claimed in claim 1 wherein the said anionic surfactant is selected from fatty alcohol sulfates and alkyl sulfonates. 5. The process as claimed in claim 1 or 4 wherein the said anionic surfactant is selected from sodium lauryl ether sufate, sodium salt of alkyl benzene« sulfonate and sodium salt of alpha olefin sulfonate. 6. The process as claimed in claim 1 wherein the said anionic surfactant has a concentration of about 5% to about 20%. 7. The process as claimed in claim 1 wherein the said anionic surfactant has a concentration of about 10% to about 15%. 18 8. The process as claimed in claim 1 wherein' the said anionic surfactant wherein the said anionic surfactant has 8 to 22 carbon atoms. 9. The process as claimed in claim 1 or 2 wherein the synthesized amphoteric surfactant is imidazoline monocarboxylate or imidazoline dicarboxylate or cocoamido propyl betain. 10. The process as claimed in claim 1 or 2 wherein the said amphoteric surfactant has a concentration of about 25% to about 45%. 11. The process as claimed in claim 1 wherein the pH of the surfactant composition is adjusted at 5.5 to 6.5. 12. The process as claimed in claim 1 or 12 wherein of the pH surfactant composition is adjusted with sulfuric acid or hydrochloric acid. 13. The process as claimed in claim 1 wherein the said surfactant composition has a total solid content above 70 %. 14. The process for the preparation of pourable surfactant composition having high solid content substantially as hereinbefore described with reference to the preferred aspects, embodiments and features of the invention and illustrated with reference to the examples. Dated this 16th day of January 2006. 19

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