Title of Invention	A LOW TFM DETERGENT BAR
Abstract	A low TFM detergent bar compring a)15 to 30% total fatty matter (TFM) b)25 to 70% inorganic particulars including talc and calcium carbonate. c)0.5 to 10% of alumino-silicate and d)3 to 20% water.

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COMPLETE AFTER PROVISIONAL LEFT ON J2100 FORM - 2 THE PATENTS ACT, 1970 (39 of 1970) & The Patents Rules, 2003 COMPLETE SPECIFICATION (See Section 10 and Rule 13) A LOW TFM DETERGENT BAR HINDUSTAN LEVER LIMITED, a company incorporated under the Indian Companies Act, 1913 and having its registered office at Hindustan Lever House, 165/166, Backbay Reclamation, Mumbai -400 020, Maharashtra, India The following specification particularly describes the invention and the manner in which it is to be performed. -1 MAR 2006 Technical field The invention relates to a detergent bar comprising low amount of total fatty matter. The invention in particular refers to a detergent bar comprising low amount of total fatty matter which provides for cleaning like a conventional bar while not compromising on desirable user properties like low grit, low mush, low rate of wear and high lather and is especially suitable for personal washing applications. Background and prior art Soaps have conventionally been used for cleaning purposes and toilet bars are generally prepared with total fatty matter (TFM) of 72-78 weight percent. Soaps have been traditionally prepared by saponification of oils of either plant or animal origin or by neutralization of a fatty acid mixture with an alkali. A soap with such a high amount of total fatty matter while providing sufficient cleaning and good bar integrity during storage and use, tends to be cost extensive to manufacture due to the high cost of the raw material viz. fatty acid mixture or the soaps. It has been determined in the past that this high level of total fatty matter is not required for the cleaning purposes. Sufficient cleaning can be obtained with much lower amount of total fatty matter, but such efforts often lead to bars where other user desirable properties like bar integrity, mush, rate of wear and smoothness are compromised. IN177828 (Hindustan Lever Ltd. 1997) relates to an improved process for preparing a low TFM content detergent bar with high water content comprising 25 to 70% by weight of colloidal aluminium hydroxide in the particle size range of 0.1 to 25 urn and 15 to 52% by weight water, and other minor ingredients which process comprises the steps of (i) reacting one or more fatty acids with aluminum containing alkaline material such as sodium aluminate to obtain a mixture of sodium aluminate and soap at a temperature of 60 to 95 °C, (ii) adding desired amount of water and (iii) adding other ingredients if desired and (iv) converting the product of step (iii) into bars in a known manner. The invention is more 2 particularly suited for producing bars having 30 to 55% TFM. It is desirable to prepare bars which has all of the desired properties during storage and use which has even lower amount of TFM in the range of 15 - 30% and other ingredients which ensure that the cost of producing the bars is even further lower. IN 187129 (Hindustan Lever Ltd. 1997) relates to a shaped detergent composition for laundry washing comprising soap, water and alumino-silicate formed in-situ wherein the fatty matter of the soap has an iodine value of at least 60 wherein the alumino-silicate is produced from selected precursor materials. It is desirable to provide for alternate detergent bars compositions and processes to prepare them which are flexible to a wider range of raw materials like total fatty matter of any iodine value. US 6207636 (Unilever, 2001) describes a low fatty matter content detergent bar composition comprising 25 - 70% total fatty matter, 9 - 16% by weight colloidal aluminum hydroxide and 12 - 57% water wherein one step in a process to make said bar comprises reacting one or more fatty acids or fats with sodium aluminate having a solids content of 20 - 55%; wherein the AI2O3 to Na20 is in the region 0.5 to 1.55:1. This publication particularly relates to composition having a higher TFM than 30%. Also, it is desirable to provide for alternative low TFM detergent bars and processes to prepare them which will ensure that availability of these low cost bars are not compromised due to the fluctuations in the availability and cost of the raw materials. The present inventors have now found that acceptable low TFM detergent bars can be prepared with an alumino-silicate structuring system which essentially has two types of inorganic particulates. Object of the invention It is thus an object of the invention to provide for low TFM detergent bars which can be prepared at lower cost. 3 It is another object of the invention to provide for low TFM detergent bars which can be prepared using readily available raw materials thereby having high flexibility in manufacture. It is yet another object of the invention to provide for low TFM detergent bars which give acceptable cleaning as compared to conventional bars while not compromising on user desired properties like high bar integrity, low mush, high lather and low grit while providing such bars to the consumers at low cost. Summary of the invention Thus, according to one aspect of the invention there is provided a low TFM detergent bar comprising (i) 15 to 30% total fatty matter (TFM) (ii) 25 to 70% inorganic particulates including talc and calcium carbonate (iii) 0.1 to 10% of alumino-silicate and (iv) 3 to 20% water It is particularly desirable that the detergent bar of the invention comprises calcium silicate. Detailed description of the invention The invention provides for a low total fatty matter (TFM) detergent bar that gives good cleaning while retaining all the user desired properties. The term total fatty matter, usually abbreviated to TFM is used to denote the percentage by weight of fatty acid and triglyceride residues present in soaps without taking into account the accompanying cations. For a soap having 18 carbon atoms, an accompanying sodium cation will generally amount to about 8% by weight. Other cations may be employed as desired for example zinc, potassium, magnesium, alkyl ammonium and aluminium. 4 The term soap denotes salts of carboxylic fatty acids. The soap may be derived from any of the triglycerides conventionally used in soap manufacture -consequently the carboxylate anions in the soap may contain from 8 to 22 carbon atoms. The soap may be obtained by saponifying a fat and/or a fatty acid. The fats or oils generally used in soap manufacture may be such as tallow, tallow stearines, palm oil, palm stearines, soya bean oil, fish oil, castor oil, rice bran oil, sunflower oil, coconut oil, babassu oil, palm kernel oil, and others. In the above process the fatty acids are derived from oils/fats selected from coconut, rice bran, groundnut, tallow, palm, palm kernel, cotton seed, soybean, castor etc. The fatty acid soaps can also be synthetically prepared (e.g. by the oxidation of petroleum or by the hydrogenation of carbon monoxide by the Fischer-Tropsch process). Resin acids, such as those present in tall oil, may be used. Naphthenic acids are also suitable. Tallow fatty acids can be derived from various animal sources and generally comprise about 1-8% myristic acid, about 21-32% palmitic acid, about 14-31% stearic acid, about 0-4% palmitoleic acid, about 36-50% oleic acid and about 0-5% linoleic acid. A typical distribution is 2.5% myristic acid, 29% palmitic acid, 23% stearic acid, 2% palmitoleic acid, 41.5% oleic acid, and 3% linoleic acid. Other similar mixtures, such as those from palm oil and those derived from various animal tallow and lard are also included. Coconut oil (CNO) refers to fatty acid mixtures having an approximate carbon chain length distribution of 8% C8, 7% C10, 48% C12, 17% C14, 8% C16, 2% C18, 7% oleic and 2% linoleic acids (the first six fatty acids listed being saturated). Other sources having similar carbon chain length distributions, such as palm kernel oil and babassu kernel oil, are included within the term coconut oil. 5 Fatty acid: A typical fatty acid blend consists of 5 to 30% coconut fatty acids and 70 to 95% fatty acids ex hardened rice bran oil. Fatty acids derived from other suitable oils/fats such as groundnut, soybean, tallow, palm, palm kernel, etc. may also be used in other desired proportions. The bar of the invention comprises TFM in an amount in the range of 15 to 30%, preferably 18 to 25 % by weight of the composition. It is desirable that the composition does not have any significant amount of free fatty acid. Synthetic surfactants: The detergent bar of the invention may optionally comprise synthetic surface active agents or surfactants which may be chosen from anionic, cationic, amphoteric, non-ionic or zwitterionic types. When present they are generally in amount not higher than 15 weight percent. Inorganic particulates: The bar of the invention includes inorganic particulates talc and calcium carbonate. Talc is a magnesium silicate mineral material, with a sheet silicate structure and a composition of Mg3Si4(OH)22 and may be available in the hydrated form. It has a plate like morphology and is essentially oleophilic / hydrophobic i.e they are wetted by oil rather than water. Calcium carbonate or chalk exists in three crystal forms viz. calcite, aragonite and vaterite. The natural morphology of calcite is rhombohedral or cuboidal, acicular or dendritic for aragonite and spheroidal for vaterite. Commercially, calcium carbonate or chalk known as precipitated calcium carbonate is produced by carbonation method in which carbon dioxide gas is bubbled through an aqueous suspension of calcium hydroxide. In this process the crystal type of calcium carbonate is calcite or a mixture of calcite and aragonite. The bar of the invention comprises the inorganic particulates in an amount in the range of 25 to 70%, more preferably 30 to 65% by weight of the composition. It is 6 preferred that talc and calcium carbonate are present in amounts in a weight ratio in the range of 1:4 to 8:1, more preferably in the range of 1:4 to 5:1. Optionally the inorganic particulate china clay may be present in the soap bar of the invention. Alumino-silcate structuring: The inorganic particulate structurant alumino silicate is present in the soap bar of the invention. It is preferably generated in situ using a source of monomeric aluminium to condense with silicate anion. The preferable components used for the generation of the structurant are aluminium sulphate and alkaline sodium silicate. It is also possible to incorporate readily available sodium alumino-silicate into the formulation. The alumino-silicate is preferably present in an amount in the range of 0.5 to 6% by weight of the composition. Calcium-silicate structuring: Optionally inorganic particulate structurant calcium silicate is present in the soap bar of the invention. It is preferably generated in situ from precursor material selected from a soluble calcium compound e.g. calcium hydroxide reacting with sodium silicate. Calcium silicate is preferably present in an amount in the range of 0.1 to 2%, more preferably 0.1 to 1 % by weight of the composition. Process: The process employed for preparing the low TFM detergent bar of the invention preferably comprises the steps of (i) neutralizing a fatty acid mixture to form soap, (ii) generating the alumino silicate insitu from the precursor materials, (iii) mixing the inorganic particulates and (iv) plodding and forming the resulting mixture into a bar. The invention is carried out in any mixer conventionally used in soap/detergent manufacture and is preferably a high shear kneading mixer. The preferred mixers include ploughshare mixer, mixers with kneading members of sigma type, multi wiping overlap, single curve or double arm. The double arm kneading mixers can be of overlapping or tangential in design. Alternatively the invention can be 7 carried out in a helical screw agitator vessel or multi head dosing pump/high shear mixer and spray drier combinations as in conventional processing. Other optional ingredients Benefit agents e.g. moisturisers, emollients, sunscreens, or anti ageing compounds may be incorporated in the composition of the invention. Examples of moisturisers and emollients include humectants like polyols, glycerol, cetyl alcohol, carbopol, ethoxylated castor oil, paraffin oils, lanolin and its derivatives. Silicone compounds such as silicone surfactants like DC3225C (Dow Corning) and/or silicone emollients, silicone oil (DC-200 Ex-Dow Corning) may also be included. Sun-screens such as 4-tertiary butyl-4'-methoxy dibenzoylmethane (available under the trade name PARSOL 1789 from Givaudan) and/or 2-ethyl hexyl methoxy cinnamate (available under the trade name PARSOL MCX from Givaudan) or other UV-A and UV-B sun-screens may also be incorporated. Water soluble glycols such as propylene glycol, ethylene glycol, glycerol, may be employed at levels upto 10%. Other additives such as one or more water insoluble particulate materials e.g. polysaccharides such as starch or modified starches and cellulose may be incorporated. Minor additives include colour, preservatives and perfumes, may optionally be incorporated. The invention will now be illustrated with reference to the following non-limiting examples. Comparative Examples A to F: Soap bars comprising low amounts of TFM and various amounts of other materials were prepared as shown in Table - 1, with the objective of preparing bars having all the desirable properties. The fatty acid was taken in a plough share mixer (PSM), heated to melt and neutralised with required amount of caustic alkali. This mass was brought to room temperature and mixed in a sigma mixer. The precursors of alumino-silicate or calcium silicate were added if any, 8 and inorganic particulates, if any. The uniform soap composition mix was then plodded and cut into bars in a conventional manner. The properties of the bars, thus prepared, are also summarized in Table-1. Table-1 Comp. Exp-A Comp. Exp-B Comp. Exp-C Comp. Exp-D Comp. Exp-E Comp Exp-F Type of soap 20CNOIV = 40 -42 20CNOIV = 40-42 20CNOIV = 40 -42 20CNOIV = 40 -42 IV = 90 20CNOIV = 40 -42 Soap, wt% 26.0 24.6 25.0 26.0 26.0 25.0 Talc 60.0 60.0 10.0 10.0 30.0 50.0 Calcite - - 50.0 20.0 - - Aluminium Sulphate - - - - - 1.0 Calcium Hydroxide - - - - - 0.2 Sodium silicate - 4.4 - - - 4.0 China Clay - - - 37.7 40.0 11.5 Water To 100 To 100 To 100 To 100 To 100 To 100 Bar property No bar integrity No bar integrity No bar integrity No bar integrity No bar integrity Bar is brittle The data in table-1 indicates that bars prepared in comparative examples A to F with only some but not all of the essential ingredients of the bar as per the invention produced bars with poor and unacceptable bar properties. Examples 1 to 3 Soap bars comprising low amounts of TFM and various amounts of other materials were prepared as shown in Table - 2, with the same process as used to prepare bars of comparative examples A to F. The properties of the bars, thus prepared, are also summarized in Table-2. 9 Table-2 Exp- 1 Exp-2 Exp-3 Type of soap 20CNO IV = 40 - 42 20CNO IV = 40 - 42 20 CNO IV = 40 - 42 Soap, wt% 24.0 25.0 23.3 Talc 12.5 12.3 40.0 Calcite 40.0 39.0 10.0 Aluminium Sulphate 1.5 1.5 1.0 Calcium Hydroxide - 0.2 0.2 Sodium silicate 5.0 5.0 4.0 China Clay 12.0 12.0 11.5 Water To 100 To 100 To 100 Bar property Bar integrityjustacceptable Good bar integrity Good bar integrity Mush Acceptable Good Good Lather Good Good Good The data in Table -2 indicates that bars prepared as per the invention provides for bars with low TFM while providing for the desired storage and user properties like good bar integrity, low mush, and high lather. Comparative Examples G and H Soap bars having substantial amount of free fatty acid were prepared as per the compositions as shown in Table-3, and as per process used for preparing bars of examples 1-3. The product characteristics are also summarized in table - 3. 10 Table-3 Comp Exp -G Comp Exp -H Type of soap 30CNO IV = 40 - 42 20CNO IV = 40 - 42 Soap, wt% 19.0 19.0 Hysteric Acid 5.0 2.0 Talc 12.7 12.7 Calcite 40.0 40.0 Aluminium Sulphate 1.3 1.3 Calcium Hydroxide 0.2 0.2 Sodium silicate 5.0 5.0 China Clay 11.8 11.8 Water To 100 To 100 Bar property Very high grit Very high grit The data in table - 3 indicate that bars having substantial amount of free fatty acid viz. hysteric acid, gave bars with unacceptable user properties viz. high grit. It is thus possible by way of the invention to prepare soap bars with very low amount of TFM and with readily available raw materials which enables production of low cost bars while not compromising on the user-desired properties like good bar integrity, high lather, smooth feel, low mush and low rate of wear. We Claim (1) A low TFM detergent bar comprising i. 15 to 30% total fatty matter (TFM) ii. 25 to 70% inorganic particulates including talc and calcium carbonate iii. 0.5 to 10% of alumino-silicate and iv. 3 to 20% water (2) A detergent bar as claimed in claim 1 wherein the bar comprises 0.1 to 2% calcium silicate. (3) A detergent bar as claimed in claim 2 wherein the calcium silicate is formed insitu from precursor material selected from a soluble calcium compound and sodium silicate. (4) A detergent bar as claimed in claim 3 wherein the soluble calcium compound is calcium hydroxide. (5) A detergent bar as claimed in anyone of claims 2 to 4 wherein calcium silicate is present in an amount in the range of 0.1 to 1%. (6) A detergent bar as claimed in any one of the preceding claims wherein alumino-silicate is present in an amount in the range of 0.5 to 4%. (7) A detergent bar as claimed in any one of the preceding claims wherein the inorganic particulates are present in an amount in the range of 30 to 65%. (8) A detergent bar as claimed in any one of the preceding claims wherein the inorganic particulates talc and calcium carbonate are present in a weight ratio of 1:4 to 8:1. 12 (9) A detergent bar as claimed in claim 8 wherein the ratio is in the range of 1:4 to 5:1. (10) A detergent bar as claimed in any one of the preceding claims wherein the inorganic particulates include china clay. (11) A detergent bar as claimed in any one of the preceding claims wherein the TFM is in the range of 18 to 25 wt%. (12) A detergent bar as claimed in any one of the preceding claims wherein the water content is in the range of 3 to 12%. (13) A detergent bar as claimed in any one of the preceding claims wherein the bar has substantially no free fatty acid. (14) A process for preparing a low TFM detergent bar as claimed in any one of the preceding claims comprising the steps of a. neutralizing a fatty acid mixture to form soap b. generating the alumino silicate insitu from the precursor materials c. mixing the inorganic particulates and d. plodding and forming the resulting mixture into a bar. Dated this 1st day of March 2006 HINDUSTAN LEVER LIMITED 13 ABSTRACT A low TFM detergent bar comprising (a) 15 to 30% total fatty matter (TFM) (b) 25 to 70% inorganic particulates including talc and calcium carbonate (c) 0.5 to 10% of alumino-silicate and (d) 3 to 20% water - 1 MAR 2006 14

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