HK1112016B - Soap bars comprising alpha sulfonated alkyl ester or sulfonated fatty acid - Google Patents

Description

Soap bars containing alpha sulfonated alkyl esters or sulfonated fatty acids

This application is a continuation-in-part application of U.S. application serial No. 10/502915 filed on 8/5/2003, and 10/502915 is a national phase application of PCT/US03/02861 filed on 31/1/2003, claiming priority of U.S. provisional application serial No. 60/353693 filed on 31/1/2002, all of which are incorporated herein by reference.

Technical Field

The present invention describes techniques relating to compositions containing a primary surfactant of a soap, a fatty acid, a sulfonated fatty acid or an alpha sulfonated alkyl ester, a secondary synthetic surfactant, an electrolyte and a polyol, wherein the composition is suitable for use in forming a precursor cleansing/laundry bar premix (i.e., "soap noodles" (soap noodles)), a personal cleansing bar or a laundry detergent bar. In particular, the present invention relates to compositions suitable for processing into solid or semi-solid personal cleansing and/or laundry detergent bars comprising alpha-sulfonated fatty acid alkyl esters and/or sulfonated fatty acids and at least one synthetic anionic, amphoteric, zwitterionic, nonionic, or semi-polar surfactant. The technology described herein also relates to improved processes for producing the precursor cleaning/laundry bar surfactant premix or personal cleaning/laundry detergent bars. Embodiments of the present compositions and methods exhibit improved processing characteristics and are capable of forming cleaning or detergent bars having high hardness, high damage resistance, low abrasion, and low soft cake formation (mush formation) during consumer use.

Description of the related Art

Personal cleansing and laundry detergent bars and their precursor formulations have become the focus of great profit. People typically wash their skin and remove it several times daily with various surface active detergent bar formulations. An ideal skin cleansing bar would be one that gently cleanses the skin, causes little or no irritation, does not degrease and excessively dry the skin, or stretches the skin after frequent daily use. Most high lathering soap bars fail in this regard.

The processability, substantivity, spreadability and marring properties of personal cleansing and laundry cleansing bars and the processability of their precursor detergent compositions have been the focus of great interest to the personal care and laundry industries. Precursor cleansing/laundry bar surfactant premixes that have low tack and are easy to extrude and mold are highly desirable. Also very desirable are finished bars (final bars) which are easy to process from such precursor compositions which are very mild, strong but not hard, have low spreadability and are not easily damaged.

Synthetic detergent bars, often referred to as "combo bars" (i.e., bars with a high amount of soap) and/or "syndet bars" (i.e., bars with little or no soap) are well known in the art, as are natural "soap" bars for personal care. Synthetic detergent bars generally have poor physical properties, such as deodorization, poor processability, stickiness, brittleness, softness of the bar (gumminess), poor lather quality, lack of mildness, or combinations thereof. Moreover, the problem of formulating synthetic detergent bars is not limited to the performance characteristics of the finished bars. Most synthetic bars made with some mild surfactants are difficult to manufacture. The processing conditions of such bars present high technical challenges for industrial scale producers, mainly due to the need for expensive specialized processing equipment.

Conversely, the manufacture of relatively pure "soap" bars is well defined as a process sequence involving milling, plodding and shaping. For example, coconut/tallow soaps become relatively plastic when heated and are easily molded and formed at relatively low pressures. However, most synthetic detergent and detergent filler ingredients used for cleaning or laundry detergent bars become excessively plastic and pasty, and the machinery used for manufacture and processing is often complex and must be specially designed. See, for example, U.S. patent No.2678921 issued 5-18/1954. Ideally, the processing of synthetic detergent bars or synthetic detergent bars should be fast and without problems in milling, extrusion, stamping, shaping and stamping into bars. Most mild synthetic detergent bars do not meet some or all of these requirements.

Synthetic detergent bar formulations for personal care are well known in the art. See, for example, U.S. patent No.5328632, granted 12/7/1994, U.S. patent No.5510050, granted 23/4/1996, U.S. patent No.5393449, granted 28/2/1995, WO95/27036, filed 30/3/1995, and WO 95/27038, filed 30/3/1995. Major disadvantages of most synthetic surfactant toilet bar (toilet bar) formulations include poor lathering, poor spreadability and poor processability due to stickiness. The use of high foaming anionic surfactants can produce acceptable levels of foaming, but unfortunately, the use of high foaming anionic surfactants actually results in poor processability. However some known mild mixtures of sodium coconut/tallow alkyl glyceryl ether sulfonate (AGS) have a good foaming potential but are difficult to process due to their stickiness or water absorption. It is understood that processability, substantivity, spreadability, low damage, mildness, lathering and rinsability (rinsability) make the selection of surfactants and the stoichiometry of mild personal cleansing bar ingredients a critical and difficult task. Thus, it should also be understood that the rather stringent requirements of formulating mild personal cleansing bars limit surfactant selection, and that the final formulation exhibits a certain degree of compromise. Mildness is generally obtained at the expense of processability, effective cleaning, lathering or rinsability, and vice versa. Processability is generally obtained at the expense of spreadability or damage to the finished bar.

Synthetic detergent bar formulations for laundry cleaning are also well known. See, for example, U.S. patent No.5965508 issued on 12.10.1999, WO95/27036 filed on 30.3.1995, and WO 95/27038 filed on 30.3.1995. The laundry detergent bars have been used widely in areas of the world where automatic washing machines are not commonly available. The ideal laundry detergent bar can effectively clean clothes, has acceptable foaming characteristics, low smearing, and pleasant odor and appearance. Mildness is also highly desirable because these laundry detergent bars come into contact with the skin during laundering.

Methods of making laundry detergent bars are also known. See, for example, Philippine patent No.23689, granted on 27 th.9/1989 and Philippine patent No. 245151, granted on 3 th.8/1990. Very similar to synthetic detergent bars for personal care, laundry detergent bars often have many of the same physicochemical problems, e.g. roughness, poor lathering, poor spreadability, poor marring and poor processability due to stickiness.

Conventional milled soap (milled toiletries soap) is prepared by a process generally comprising the steps of: (1) drying soap having a moisture content of about 28% to about 30% to a moisture content of about 7% to about 14%, (2) forming a precursor "soap noodles" from the dried soap by passing it through a screw extruder, (3) mixing various desired additives such as colorants, fragrances, etc. into the soap noodles, (4) passing the mixture formed in (3) through a mill or series of mills ("milling" soap) and thereby forming a soap ribbon, (5) passing the milled soap mixture from (5) through additional screw extruders to form soap segments (log) (i.e., "plodding" the soap to form "billets"), and (6) cutting the segments into segments (i.e., billets) and stamping the segments or billets into the desired bar form.

The soaps dried in step (1) may generally be obtained by saponification of the fats or neutralization of the free fatty acids. Because drying cannot be completely uniform, the dried soap inevitably contains some particles that are too dry and harder than the rest of the mass of dried soap. If the soap also contains free fatty acids, the heterogeneity of the free acids in the soap may also contribute to the presence of harder soap particles that dry the rest of the soap mass. The hard particles generally have a diameter of about 0.5 to about 10 mm. These particles are retained in the soap by the first molding step (2) and the mixing step (3). In the milling step (4), the soap is "worked up" and the over-dried particles are broken up into very small particles (typically less than about 0.25mm in diameter) and uniformly dispersed in the soap mass. When not milled, the finished bar may have a harsh or gritty feel during use due to the relatively large, excessively dry soap particles (also known as "hard spots") which dissolve at a slower rate. When the soap has been properly ground, overly dry soap is not noticeable in use because it has been reduced to a very small particle size and uniformly dispersed throughout the soap mass. See uk patent No.512551, granted on 9/19/1939, which is incorporated herein by reference.

U.S. Pat. No.2894912 ('912 patent) and U.S. Pat. No.3376229 (' 229 patent) disclose compositions containing C₆-C₁₈Acyl isethionates as the primary detergent and mild detergent soaps and soap bars containing low levels of fatty acids and soaps. In the' 912 patent, chips that are processed into strands are made from an aqueous slurry of 40-50% of the ingredients mixed at a temperature of 38 deg.C-93 deg.C, or from a mixture of dry ingredients mixed for an extended period of time at 100 deg.C. In the' 229 patent, the noodles are prepared by mixing an acyl isethionate, a fatty acid, and an anion at a temperature of about 110 ℃ to 113 ℃ for about 15 minutesIonic syndet and soap. The latter bars contain at least about 4% by weight sodium isethionate as a processing aid.

In us patent No.4707288, a mixture of acyl isethionate, fatty acid, soap and sodium isethionate of greater than 2 wt% are mixed in granular form at a temperature of 60 ℃ to 86 ℃ using a special cavity transfer mixer (cavity transfer mixer) under high shear to give a toilet bar with low grit.

U.S. patent No.4696767 discloses a process for making mild toilet bars in which a slurry of acyl isethionate, water and a polyol (such as sorbitol) is heated at a temperature of 100 ℃ to 120 ℃ at 4-10 p.s.i.g. to form a stable solution. The slurry was then mixed with neat soap (neat soap) and heated to about 150 c at a pressure of 4 atmospheres to yield a chip-like mass of soap bars without grit prior to the vacuum drying and plodding steps. However, the presence of the polyol results in more water penetration into the soap dish (soap dish) and increased cost of the bar. The patent also teaches that the use of particulate acyl isethionate results in problems such as lacrimation (i.e., dripping of material from the soap bar). Also, larger acyl isethionate particles produce bars with grit.

In us patent No.4663070, a toilet bar composition is described in which soap is the primary surfactant. A liquid mixture containing most of the soaps and acyl isethionate, fatty acid, water and sodium isethionate is formed at a temperature of 96 ℃ to 103 ℃. In U.S. patent No.5030376, a similar mixture containing a greater proportion of soap is processed under high shear conditions in a specialized cavity transfer mixer while the temperature is maintained below 40 ℃, thereby forming a mixture with some soap in the delta phase. U.S. patent No.5041233 also relates to similar mixtures in which a mixture of acyl isethionate, fatty acid and soap is made at a temperature of 82 ℃ to 94 ℃ with soap formed in situ. The patent states that hydrolysis of the high viscosity mixture and acyl isethionate leads to problems in the finished product.

The above description of the related art shows that various processes have been used to produce personal cleansing and laundry detergent bar premixes and the resulting mild detergent soaps, toilet bars. Additionally, soap bars are commercially manufactured in a variety of structures that are aesthetically pleasing. These products are often damaged by damage, defined as the formation of undesirable, white, chalk-like cracks (shatter marks) in and around the indented areas in conventional soaps. Damage typically occurs during handling, shipping, and distribution of the finished product to the consumer.

About 1 to 2 weeks after soap bar preparation, ordinary gifts and decorative soaps are bruised or chipped, especially in the corners of complex or unique structures. When soap products are packaged side-by-side, damage often occurs because the individual strips strike each other or the carton walls or side walls. Such damage is readily apparent, especially for colored soaps, where chalk-like cracks form around scratches or chips.

Currently, labor intensive packaging methods are used to protect conventional soap bases from damage. New products that rely heavily on aesthetically pleasing qualities require expensive cardboard boxes and/or protective packaging in the early days to prevent surface defects. Even with these special precautions, conventional formulations cannot be guaranteed to avoid surface defects.

Thus, based on the foregoing, there is a need for excellent personal cleansing and/or laundry detergent bar formulations that exhibit increased mildness, improved processability, reduced spreadability, improved lather potential, and sheeting properties, and low damage characteristics.

Brief description of the invention

Thus, the present technology overcomes one or more of the above-mentioned disadvantages of conventional soap bar compositions and processes by exhibiting surprising performance and processing synergies. In particular, based on the surprising and unique synergy found between the component compounds of the present technology, the compositions of the present technology can be used as precursor cleansing/laundry bar surfactant premixes or "soap noodles", personal cleansing bars, or laundry detergent bars. Such bars produced according to embodiments of the present technology generally exhibit improved processability, increased lather, reduced spreadability, reduced marring, improved color stability, and/or impart good feel and after-feel (after-feel) properties to the skin. Furthermore, the composition may be translucent and/or may be processed into translucent personal cleansing and/or laundry detergent bars with appropriate selection of additive ingredients. The compositions are preferably generally suitable for processing using standard extrusion and/or screw extruder equipment.

Preferably, the composition according to the present technique comprises: soaps, preferably tallow and/or coconut fatty acid soaps; an alpha sulfonated alkyl ester, a sulfonated fatty acid, and/or mixtures thereof; c₆-C₂₂Fatty acids, salts, polyols, and small amounts of water. Furthermore, embodiments of the present invention may also contain one or more auxiliary synthetic anionic, amphoteric, zwitterionic, nonionic, or semi-polar surfactants.

It has been surprisingly found that the use of polyols greatly facilitates and improves the production of precursor cleansing/laundry bars, "soap noodles", and the production of personal cleansing/laundry detergent bars made from the noodles. The bars typically contain a very low moisture content, thereby increasing the hardness of the bar and reducing the wear rate during use. The compositions of the present invention have low processing viscosity, improved drying characteristics, and substantially no gritty feel due to the presence of hard soap particles ("hard spots") as compared to conventional soap bar compositions that are substantially free of polyols.

Furthermore, the compositions are useful for making stamped personal cleansing and/or laundry detergent bars, which generally have improved processability, are mild to the skin, have improved smear and bar firmness, have good lathering properties and/or reduced spoilage. The compositions of the present technology may also be used to produce dishwashing pastes (dish washes), gels and body washes (body washes), among other uses. In addition, the present invention provides improved methods of making precursor cleansing/laundry bars, "soap noodles", personal cleansing bars and laundry detergent bars.

Particularly preferred embodiments of the present disclosure include: from about 40% to about 93% by weight of soap slurry, preferably containing soap from tallow and/or coconut oil fatty acids; about 1% to about 15% C₆-C₂₂A fatty acid; from about 1% to about 30% of a mixture consisting of (i) an alpha sulfonated alkyl ester, sulfonated fatty acid, or mixtures thereof, and (ii) a synthetic anionic, amphoteric, zwitterionic, nonionic, or semi-polar surfactant; from about 0.5% to about 2% of sodium sulfate, sodium chloride, sodium carbonate, potassium sulfate, potassium chloride, potassium carbonate, calcium sulfate, calcium chloride, calcium carbonate, magnesium sulfate, magnesium chloride, or magnesium carbonate salt; from about 0.01% to about 5.0% of a polyol; and optionally from about 0% to about 10% alkanolamide.

Other embodiments of the present invention relate to improved methods of producing precursor cleansing/laundry bars, "soap noodles", personal cleansing bars and laundry detergent bars derived from the compositions of the technology described herein. The method preferably comprises: forming an initial mixture comprising the above-described soap slurry, fatty acid, surfactant mixture, salt, polyol, and optionally alkanolamide at a temperature in the range of from about 65 ℃ to about 105 ℃; removing from the initial mixture water in a total amount of about 5 wt% to about 90 wt% to form a thick mixture; and extruding the thick mixture. The method can further comprise molding the extruded mixture, re-extruding the molded material to form a billet, cutting the billet, and stamping the cut billet to form the personal cleansing or laundry detergent bar.

Detailed Description

One embodiment of the present technology is a composition comprising: soaps, preferably tallow and/or coconut fatty acid soaps; an alpha sulfonated alkyl ester, a sulfonated fatty acid, and/or mixtures thereof; c₆-C₂₂Fatty acids, salts, polyols, and small amounts of water. Furthermore, the above embodiment is preferableContaining one or more auxiliary synthetic anionic, amphoteric, zwitterionic, nonionic, or semi-polar surfactants, waxes, and/or other additives or surfactants. Optionally, the composition may also contain an alkanolamide.

Soaps:

according to this particular embodiment, the soap preferably has the following general chemical formula:

wherein R is₁Is C₆-C₂₂Hydrocarbyl, alkyl, or combinations thereof, n is 1 or 2, and L is sodium, potassium, calcium, magnesium, ammonium, monoethanolammonium, diethanolammonium, triethanolammonium, or mixtures thereof. Preferably, the soap is present as an aqueous slurry, which preferably contains about 53% to about 90% of the initial mixture and/or thick mixture, before or after drying or dewatering of the soap mixture. More preferably, the soap is present in about 68% to about 78% by weight of the finished soap bar. The initial aqueous slurry may contain any percentage of water, however, the slurry preferably contains from about 30% to about 50% water in the initial mixture. As described below, most of the water is preferably removed prior to forming the finished soap bar.

Also preferably, the soap is a tallow or coconut fatty acid soap or mixtures thereof. More preferably, the soap comprises from about 60% to about 90% tallow soap and from about 10% to about 40% coconut fatty acid soap.

Fatty acid:

the fatty acid is preferably C containing a hydrocarbon group, an alkyl group, or a combination thereof₆-C₂₂A fatty acid. More preferably, the fatty acid is C₁₂-C₂₀A fatty acid. The fatty acid is preferably present in about 1 wt% to about 15 wt%, more preferably about 2 wt% to about 4 wt%.

The (free) fatty acids used according to the present technique generally correspond to the fatty acids used to prepare conventional soaps. Fatty acid materials desirably incorporated into the present invention include, for example, hydrocarbon materials, especially saturated, having a chain length of from about 6 to about 22. These fatty acids may be of single chain length of high purity and/or crude mixtures such as those derived from fats and oils. The industry term "triple pressed stearic acid" includes about 45 parts stearic acid and 55 parts palmitic acid. Furthermore, the term stearic acid as used in the context of the soap industry means a mixture of fatty acids that is primarily stearic acid, as is also used herein.

Compositions according to the present technology, and methods of producing such compositions, may include soaps, in some embodiments saturated, derived from hydrocarbons having a chain length of from about 6 to about 22 (including carboxyl carbons). In some manifestations described in this particular embodiment, the soap is a sodium salt, but other soluble soaps may be used. Potassium, calcium, magnesium, monoethanolammonium, diethanolammonium, triethanolammonium, and mixtures thereof are considered acceptable.

The soaps may be prepared by in situ saponification or ion exchange with the halide salts of the corresponding fatty acids, but they may also be introduced as preformed soaps.

Alpha sulfonated alkyl esters or alpha sulfonated fatty acids:

the compositions and methods of the present invention preferably use alpha sulfonated alkyl esters, alpha sulfonated fatty acids, or mixtures thereof. The alpha sulfonated alkyl esters preferably have the following general formula:

wherein R is₃Is C₆-C₂₂Hydrocarbyl, alkyl or combinations thereof, R₄Is straight chain orBranched chain C₁-C₆Hydrocarbyl, alkyl, or combinations thereof, n is 1 or 2, M is hydrogen, sodium, potassium, calcium, magnesium, ammonium, monoethanolammonium, diethanolammonium, triethanolammonium, or mixtures thereof.

The sulfonated fatty acids preferably have the general formula:

wherein R is₅Is C₆-C₂₂Hydrocarbyl, alkyl, or combinations thereof, N is 1 or 2, wherein N is hydrogen, sodium, potassium, calcium, magnesium, ammonium, monoethanolammonium, diethanolammonium, triethanolammonium, or mixtures thereof.

Embodiments of the present technology may disclose one or other such anionic surfactants or a mixture of both. A single such anionic surfactant or a mixture of two types of anionic surfactants may also be used in combination with an auxiliary synthetic anionic, amphoteric, zwitterionic, nonionic or semi-polar surfactant, as described below. Some embodiments using a mixture of alpha sulfonated alkyl esters and sulfonated fatty acids preferably use a ratio of about 10: 1 to about 1: 10.

The compositions of the present technology and methods of producing such compositions preferably contain (or use) from about 1 wt% to about 30 wt% of an anionic surfactant containing an alpha sulfonated alkyl ester and/or sulfonated fatty acid. The alpha sulfonated alkyl esters used are generally prepared as follows: by means of e.g. SO₃The sulfonating agent of (a) sulfonates the fatty acid alkyl ester and then neutralizes with a base such as sodium hydroxide, potassium hydroxide, calcium hydroxide, magnesium hydroxide, monoethanolamine, diethanolamine or triethanolamine, or a mixture thereof. When prepared in this manner, the alpha sulfonated alkyl esters typically contain small amounts, typically no more than 33 wt%, of alpha sulfonated fatty acids, i.e., di-salts resulting from ester hydrolysis. In general, large quantities of disalts are obtained by hydrolysis of a known quantity of a mono-salt; hydrolysis can be carried outIs completed in situ during the preparation of the composition. Thus, the alpha sulfonated alkyl ester and alpha sulfonated fatty acid may be provided to the composition as a mixture of ingredients naturally derived from sulfonation of fatty acid alkyl esters or as individual ingredients or used in the process of the present technology. Furthermore, it is known to those skilled in the art that minor amounts of impurities, such as sodium sulfate, unsulfonated Methyl Esters (ME) and unsulfonated Fatty Acids (FA), may also be present in the mixtures of the present technology.

The alpha sulfonated alkyl ester, i.e., alkyl ester sulfonate surfactant, may include, for example, C₆-C₂₂Linear esters of carboxylic acids (i.e. fatty acids) with gaseous SO₃Sulfonation was carried out according to "The Journal of American oil chemists Society," 52(1975), pages 323-329. In addition, suitable starting materials include derived natural fatty materials such as tallow, palm oil, and the like. In some embodiments of the technology described herein, the alpha sulfonated alkyl ester is desirably a sulfonated methyl ester, as further described herein.

However, preferred embodiments may comprise alpha sulfonated alkyl esters alone, sulfonated fatty acids alone, or a mixture of the two. The ingredient or mixture of ingredients may be provided in any form, but is preferably provided as an aqueous mixture.

Electrolyte (salt):

the compositions of the technology described herein and the methods of producing the compositions generally comprise (or use) from about 0.5% to about 2% by weight of salt. Without being bound by any particular theory, it is believed that the salt may be any salt that is capable of achieving a bar formulation as an embrittling agent (crisping agent) or as a builder (builder). Preferably, the salt is selected from sodium sulphate, sodium chloride, sodium carbonate, potassium sulphate, potassium chloride, potassium carbonate, calcium sulphate, calcium chloride, calcium carbonate, magnesium sulphate, magnesium chloride or magnesium carbonate, or mixtures thereof. In a more preferred embodiment of the present technology, the salt is magnesium chloride, sodium chloride or a mixture thereof. In a most preferred embodiment, the salt is sodium chloride.

Polyol:

the polyol may be a polyol, a sugar or a polyethylene glycol, generally defined as a nonvolatile, di-or higher polyol. Specific examples may include, without limitation, glycerol (glycerin), propylene glycol, glycerol (glycerin), sorbitol, sucrose and polyethylene glycol having a molecular weight of 200-]Homopolymer (100000-5000000), polyglycol and its derivatives, hexanediol (2-methyl-2, 4-pentanediol), 1, 3-butanediol, 1, 2, 6-hexanetriol, ethylhexanediol (ethoxydiol), USP (2-ethyl-1, 3-hexanediol), C₁₅-C₁₈Vicinal diols, and polyoxypropylene derivatives of trimethylolpropane.

Useful polyols of the present technology are typically liquid water-soluble aliphatic polyols or polyethylene or polypropylene glycols. The polyols may be saturated or contain olefinic bonds; it must have at least two alcohol groups attached to separate carbon atoms in the chain, and must be water soluble and liquid at room temperature. If desired, the compounds may have an alcohol group attached to each carbon atom in the chain. Among the useful compounds are, for example, ethylene glycol, propylene glycol, glycerol and mixtures thereof. In some embodiments, the polyol is glycerol. Water-soluble polyethylene glycols, water-soluble polypropylene glycols which may be used in accordance with the present techniques are those prepared by the polycondensation of ethylene glycol molecules or propylene glycol molecules to form high molecular weight ethers having terminal hydroxyl groups. The polyethylene glycol compounds may be diethylene glycol up to those having a molecular weight of about 800, in some embodiments having a molecular weight of about 100-. Typically, polyethylene glycols having a molecular weight of up to 800 are liquid and completely soluble in water. When the molecular weight of polyethylene glycols increases beyond 800, they become solid and less soluble in water. The solids may be used herein as plasticizers, particularly ductile at 35 ℃ to about 46 ℃. The polypropylene glycol compound may range from dipropylene glycol to polypropylene glycol having a molecular weight of about 2000, in some embodiments less than 1500, and in other embodiments less than 1000. They are usually liquid at room temperature and readily soluble in water.

Auxiliary synthetic surfactants:

the present technology also preferably contains a combination of an auxiliary synthetic anionic, amphoteric, zwitterionic, nonionic or semi-polar surfactant with an alpha sulfonated alkyl ester, sulfonated fatty acid or mixtures thereof. Preferably, the auxiliary synthetic surfactant is present in an amount such that the mixture of total surfactants comprises from about 1% to about 30% by weight of the total composition. More preferably, the supplemental synthetic surfactant is present in an amount of from about 5% to about 15% of the total composition.

Contemplated auxiliary synthetic surfactants include, but are not limited to, the following: cocamidopropyl betaine, laurylamidopropyl betaine, cocamidopropyl hydroxysultaine, sodium cocoamphoacetate, sodium lauryl sulfoacetate, sodium lauryl ether sulfoacetate (sodium laurethsultaine), disodium lauryl ether sulfosuccinate, disodium lauryl sulfosuccinate, cocamide monoethanolamine, cocamidopropyl amine oxide, laurylamidopropyl amine oxide, lauryl/myristyl amidopropyl amine oxide, sodium alpha olefin sulfonate, sodium lauryl sulfate, sodium cocoyl isethionate, sodium lauryl ether sulfate, potassium lauryl sulfate, magnesium lauryl sulfate, sodium laurimidodipropionate, sodium lauryl sarcosinate, sodium lauryl ether sarcosinate, alkylpolyglycosides, sodium lauryl lactate, sodium lauryl amphoacetate, sodium cocoate, mixtures thereof, and derivatives thereof.

More preferably, the auxiliary synthetic surfactant is cocamidopropyl betaine, sodium lauryl sulfoacetate, disodium lauryl ether sulfosuccinate, acyl lactylate, sodium alpha olefin sulfonate, potassium lauryl sulfate, sodium cocosulfate, or sodium lauryl ether sulfate. Most preferably, the auxiliary synthetic surfactant is cocamidopropyl betaine.

The additive comprises the following components:

the compositions disclosed herein may also optionally contain alkanolamides having the general formula:

wherein n is 6-16. Preferably, the alkanolamide is present in an amount of from about 0% to about 10%, most preferably from about 2% to about 5%.

The compositions and methods of producing such compositions may also optionally contain (or use) additional ingredients, surfactants, pH adjusters, lubricants, wetting agents, viscosity agents (viscocity agents), buffers, and the like, as disclosed in PCT application WO 03/063819, which is incorporated herein by reference and which claims priority.

For example, some additives may include from about 0.5 wt% to about 10 wt% of a sucrose glyceride, a functional metal soap, a succinamic acid ester, a sulfosuccinamic acid ester, a mono-or di-or triglyceride, chitosan, or mixtures thereof. Similarly, the compositions and methods of making the compositions may also contain (or use) from about 0.1 wt% to about 10 wt% of flavorants, lubricants, moisturizers, viscosity control formulations, and other agents suitable for incorporation into the compositions of the present invention and known to those skilled in the art.

Other optional additives may include additional detergent surfactants, for example acyl isethionates, such as sodium acyl (cocoyl) isethionate (SCI). Examples of suitable anionic surfactants include, among others, sodium, potassium, magnesium, calcium, ammonium, Monoethanolammonium (MEA), Diethanolammonium (DEA), Triethanolammonium (TEA), or alkylamine salts of the following acids, or mixtures thereof: sulfonic acids, polysulfonic acids, sulfonic acids of oils, paraffinsulfonic acids, lignosulfonic acids, petroleum sulfonic acids, tall oil acids, olefin sulfonic acids, hydroxyolefin sulfonic acids, polyene sulfonic acids, polyhydroxy polyene sulfonic acids, perfluorocarboxylic acids, alkoxylated carboxylic sulfonic acids, polycarboxylic acid polysulfones, alkoxylated polycarboxylic acid polysulfones, phosphoric acids, alkoxylated phosphoric acids, polyphosphoric acids, and alkoxylated polyphosphoric acids, fluorinated phosphoric acids, phosphate esters of oils, phosphinic acids, alkylphosphinic acids, aminophosphinic acids, polyphosphonic acids, vinylphosphinic acids, phosphonic acids, polyphosphonic acids, alkyl phosphonates, alpha-phosphonofatty acids, organo-amin-polymethylphosphonic acids, organo-aminodialkylene-phosphonic acids, alkanolamine phosphonic acids, trialkylphosphonic acids (triallyl phosphonic acid), acylamidomethane phosphonic acids, alkyliminodimethylene phosphonic acids, polymethylene-bis (nitrilo-dimethylene) tetrakis (aminodimethylene) tetrakis (methyleneene) phosphonic acids, Alkyl di (phosphonoalkylene) oxyaminoacids, substituted aminomethylphosphonates, phosphoramidites (phosphonoamic acids), acylated amino acids (e.g., amino acids that react with alkyl acid chlorides, alkyl esters, or carboxylic acids to yield N-acyl amino acids), N-alkylacyl amino acids, hydrolysates of acylated proteins, branched alkylbenzene sulfonic acids, alkyl glyceryl ether sulfates, alkyl sulfates, alkoxylated alkyl sulfates, alpha-sulfonated ester diacids, alkoxylated alpha-sulfonated alkyl ester acids, alpha-sulfonated dialkyl diester acids, di-alpha-sulfonated dialkyl diester acids, alpha-sulfonated alkyl acetic acids, primary and secondary alkyl sulfonic acids, perfluorinated alkyl sulfonic acids, sulfosuccinic mono-and diester acids, polysulfosuccinic acids, sulfosuccinic diester acids, sulfosuccinamic acids, itaconic acid, and mixtures thereof, Sulfosuccinamic acid, sulfosuccinimidyl acid, phthalic acid, sulfophthalic acid, sulfoisophthalic acid, anthranilic acid, sulfoanthranilic acid, alkyl ketosulfonic acids, hydroxyalkane-1-sulfonic acid, lactonesulfonic acid, sulfonic acid amides, sulfonic acid diamides, alkylphenol sulfates, alkoxylated alkylphenol sulfates, alkylated cycloalkyl sulfates, alkoxylated alkylated cycloalkyl sulfates, dendritic polysulfonic acids, dendritic polycarboxylic acids, dendritic polyphosphoric acids, sarcosine, isethionic acid, tauric acid, fluorinated carboxylic acids, fluorinated sulfonic acids, fluorinated sulfuric acids, fluorinated phosphonic acids and phosphinic acids, and mixtures thereof.

Suitable nonionic surfactants generally include those disclosed in U.S. patent No.3929678 to Laughlin et al, column 13, line 14 to column 16, line 6, issued 12/30 1975, which is incorporated herein by reference. Other suitable nonionic surfactants may include, for example, those selected from the group consisting of: polyoxyethylated alkylphenols, polyoxyethylated linear alcohols, polyoxyethylated branched alcohols, polyoxyethylated polyoxypropylene glycols, polyoxyethylated mercaptans, fatty acid esters, glyceryl fatty acid esters, polyglyceryl fatty acid esters, propylene glycol esters, sorbitol esters, polyoxyethylated sorbitol esters, polyoxyethylene glycol esters, polyoxyethylated fatty acid esters, primary alkanolamides, ethoxylated primary alkanolamides, secondary alkanolamides, ethoxylated secondary alkanolamides, tertiary acetylenic diols, polyoxyethylated polysiloxanes, N-alkylpyrrolidones, alkylpolyglycosides, alkylpolysaccharides, EO-PO block polymers, polyhydroxy fatty acid amides, amine oxides, and mixtures thereof.

The compositions and methods of making the compositions may be formulated and carried out such that the pH is from about 4.0 to about 10.0, and in some embodiments, from about 5 to about 9.5. Techniques for controlling pH at the recommended usage level include the use of buffers, bases, acids, and the like, which are well known to those skilled in the art. Optional pH adjusters can include, but are not limited to, citric acid, succinic acid, phosphoric acid, sodium hydroxide, sodium carbonate, and the like.

Other optional ingredients may include chelating agents such as disodium ethylenediaminetetraacetate, selected from the group consisting of amides, amine oxides, betaines, sulfobetaines and C₈-C₁₈Co-surfactants of fatty alcohols, hydrated cationic polymers, suitable plasticizers, non-volatile, non-ionic silicone conditioning agents, polyalkyl or polyaryl siloxanes, and pearlizing agents (pearlescing agents)/suspending agents,detergent builders, antibacterial agents, optical brighteners, dyes or pigments, polymers, fragrances, cellulases, softening clays, smectite-type softening clays, polymeric clays, flocculants, dye transfer inhibiting formulations, optical brighteners, skin feel enhancers (skin feeleneshancers) including aluminosilicate and non-aluminosilicate odor control materials, polyethers (chitans), triglycerides, glycerol, succinamates, sucroglycerides, functional metal soaps and mixtures thereof.

The compositions of the present technology may be transparent and/or made into transparent personal cleansing or laundry detergent bars upon suitable processing and/or selection of optional ingredients and components as detailed herein. Furthermore, the compositions may be used to produce clear dishwashing gels, pastes or solutions, or other applications or forms apparent to those skilled in the art. Whether transparent or opaque, the composition may be present as a solid tablet or as a gel.

Moreover, the compositions of the present technology and methods of producing the compositions may optionally contain (or use) from about 1.0 wt% to about 15.0 wt% of a wax, in some embodiments, for example, a paraffin wax having a melting point of about 54 ℃ to about 180 ℃. The wax may include, without limitation, beeswax, spermaceti wax, carnauba wax, bayberry wax, candelilla wax, montan wax, ozokerite, ceresin, paraffin wax, synthetic waxes such as Fisher-Tropsch wax, microcrystalline waxes, derivatives thereof, or mixtures thereof. Wax ingredients are used in the compositions of the present technology to impart mildness, plasticity, firmness and processability to the skin. Waxes also provide the final product with a glossy appearance and a smooth feel.

Thus, one component of the present technology compositions may be a wax, in some embodiments a paraffin wax having a melting point of about 54 ℃ to about 82 ℃, in other embodiments a paraffin wax of about 60 ℃ to about 74 ℃, and in other embodiments a paraffin wax of about 61 ℃ to about 71 ℃. A "high melting" paraffin wax is a paraffin wax having a melting point of about 66 ℃ to about 71 ℃. A "low melting" paraffin wax is a paraffin wax having a melting point of about 54 c to about 60 c. In some embodiments, the paraffin wax is a fully refined petroleum wax that is odorless, tasteless, and meets FDA requirements for use as a coating for food and food packaging. Such paraffins are readily available commercially. A suitable paraffin Wax is available, for example, from National Wax co under the trade name 6975.

Processing:

other embodiments of the present technology relate to an improved process for making precursor cleansing/laundry bars, "soap noodles", personal cleansing bars and laundry detergent bars, obtained from the compositions of the present invention.

The method preferably comprises: an initial mixture containing the above-described soap slurry, fatty acid, surfactant mixture, salt, polyol, secondary synthetic surfactant, and optionally alkanolamide is first formed at a temperature of about 65 c to about 105 c. Preferably, the surfactant mixture is a mixture of sulfonated fatty acids or alpha sulfonated alkyl esters plus auxiliary synthetic surfactants. Most preferably, both sulfonated fatty acids and alpha sulfonated alkyl esters are used.

Next, the method preferably includes: water is removed from the initial liquid mixture in a total amount of about 5 wt% to about 90 wt% of the water, thereby forming a thick mixture. According to the present process embodiment, the removal of water from the initial liquid mixture is preferably achieved by scraped wall vacuum evaporation drying at low pressure or hot drum drying at ambient pressure. More preferably, from about 55% to about 85% by weight of the water is removed from the initial liquid mixture, and most preferably from about 60% to about 80% by weight of the water is removed from the initial liquid mixture.

Alternatively, the same values noted above can also be expressed by the requirement that a sufficient amount of water be removed such that the residual water content is from about 1.74% of the final thick mixture (e.g., about 70% aqueous slurry with 58% of the initial mixture, 90% water removed) to about 26.5% of the final mixture (e.g., about 70% aqueous slurry with 93% of the initial mixture, 5% water removed). More preferably, 3.48% of the final thick mixture (e.g., about 70% aqueous slurry containing 58% of the initial mixture, with 80% water removed) is to about 11.16% of the final mixture (e.g., about 70% aqueous slurry containing 93% of the initial mixture, with 60% water removed). Thus, water preferably comprises from about 3% to about 20% of the thick mixture. More preferably, water comprises from about 8% to about 15% of the thick mixture.

Finally, the thick (concentrated) mixture is preferably extruded to form a sheet, solid, or semi-solid particle. The process can also include molding the tablet, solid, or semi-solid particles to form molded particles, extruding the molded particles to form billets, cutting the billets, and stamping the cut billets to obtain personal cleansing or laundry detergent bars.

The process of the present invention generally overcomes many of the above-mentioned disadvantages of previously known processes. For example, the process of the present invention results in substantially uniform soap noodles that produce soap bars with minimal grittiness. Furthermore, the process is carried out at a temperature of 105 ℃ or less in order to conserve energy and minimize hydrolysis of the alpha sulfonated alkyl ester. In addition, the method uses standard bar processing equipment. In addition, the bars produced by the improved process have desirable hardness, water permeability, low grit, high slip, and no damage (even if dried to particularly low moisture levels, and aged on the shelf for several months).

While the compositions of the present technology are very useful in soap bar and laundry bar applications, other applications of these compositions are possible. The compositions of the technology described herein may be used in the form of liquid, paste or gel dishwashing compositions or as liquid, slurry or gel dishwashing compositions, hand soaps including anhydrous hand cleaners, all-purpose cleaners, body washes, other laundry detergent compositions such as laundry powders, pre-stain (prespotter) or stain bars (stain sticks), fabric treatment compositions including Triethanolamine (TEA) soaps for dry cleaning, shampoos including human, pet and carpet use, car washes, soaps for scrubbing and brushing pads, sink drops (toil sink drops) and/or cleaners, personal care creams and lotions and the like.

Definitions, abbreviations, and CTFA nomenclature

Definitions, abbreviations and CTFA nomenclature used in the present invention are listed below:

BHT butylated hydroxytoluene (di-tert-butyl-p-cresol)

BHA butylated hydroxyanisole (3-tert-butyl-4-hydroxyanisole)

Coconut oil fatty acid Emery 627 (available from Henkel division Emery Corporation, trade name,) and coconut oil fatty acids that can replace Emery 627

EDTA ethylene diamine tetraacetic acid

Hyamine di-isobutyl-phenoxy-ethoxy-ethyl-dimethyl-benzyl ammonium chloride

MC-48A 6: 1 average mixture of sulfonated banded coconut oil methyl ester and coconut oil fatty acid (i.e., in the range of 5: 1 to 7: 1)

Pristerene 4981 stearic acid (from Unichema); an iodine value of about 1.0 at maximum; about 65% of C₁₈Fatty acid, about 28% C₁₆Mixture of fatty acids and about 2% myristic fatty acid

SFA disalt; alpha-sulfonated fatty acids (e.g., produced by SME hydrolysis)

SME monosalt; alpha-sulfonated alkyl esters (e.g., alpha-sulfonated methyl esters)

Unreacted methyl ester of UA

AlphaBSS-45 alpha sulfonated methyl ester from Stepan Company has the following properties: average chain length 13.6; sodium SME/SFA activity 43-45%; SME/SFA ratio is 1.3-1.8: 1; solid 53-55%; 5-7% of inorganic salt; water ═ 45 to 48 percent; 1-3% of free oil; working pH 4-9.

The invention is illustrated by the following non-limiting examples. All proportions appearing in the examples, as well as elsewhere in the specification, are by weight unless otherwise specified.

In the following examples, all amounts are in weight percent of active material, unless otherwise specified. It will be understood by those skilled in the art that modifications may be made without departing from the spirit or scope of the invention. The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention or the particular methods or compositions described herein. All amounts and ranges, temperatures, results, etc. used herein are approximate unless otherwise indicated.

Examples

Example 1: process for making cleansing bars

One procedure for preparing the soap/SME combination bar is as follows:

(1) neat soap was dissolved in a steam jacketed screw blender (18-200 ℃ F.).

(2) Alpha Thiomethyl ester, as a dry slurry or aqueous solution, was added to a stirring screw mixer and stirred for 5 minutes.

(3) Additives that reduce adhesion, such as glycerin or sodium chloride (0.1-2.0%) may be added to the screw mixer at this point and mixing continued for an additional 2 minutes.

(4) The wet soap is air dried or vacuum dried to reduce its moisture content to below 5%.

(5) The flavor, titanium dioxide and other minor additives were added to the ground soap chips and ground again (this time in situ using a crimper-plate).

(6) Soap mixing was performed by a Beck screw extruder (commercially available from Stephan Beck Plodder co.). The temperature of the screw extruder was maintained at 90-100F using a water circulation system.

(7) Strips were pressed from the extruded ribbons using a Midget multi press (available from denison.

Example 2: preparation of Mono-salt Sulfonated Methyl Ester (SME) MC-48

MC-48 as defined above is commercially available from a variety of sources. The preparation thereof is well known to the person skilled in the art.

Example 3: preparation of di-salt Sulfonated Fatty Acids (SFA)

Approximately 3500g of MC-48 acid were placed in a 4L beaker and stirred rapidly with slow addition of approximately 330g of sodium hydroxide. When the sodium hydroxide is completely added, the resulting SFA material has a thick, slurry-like consistency. The crude SFA was recrystallized by washing with methanol, water and salting out the pure SFA product. Crude SFA was analyzed by titrating the material with 0.02N quaternary ammonium salt (hyamine) and indicated the presence of about 46.6% of the disodium salt of MC-48. The recrystallized SFA product was about 99.8% of the disodium salt of MC-48.

EXAMPLE 4 preparation of SME: SFA samples in a ratio of 1: 1

About 138.5g of MC-48 acid was added to I L of a resin kettle equipped with heating means, stirring means, pH measuring means and nitrogen purge means. The acid was heated to 55 ℃ and about 18.7g of sodium hydroxide powder was added in small portions. With the addition of sodium hydroxide, heating occurred, from 55 ℃ to about 71 ℃, during which time cooling was performed to maintain the mixture below about 80 ℃. Towards the end of the addition of sodium hydroxide, the mixture became very thick and about 15.6g of methanol were added to keep the mixture semi-fluid. The final product was a slurry at room temperature, i.e., 25 ℃. The final SFA/SME product was titrated with 0.02N quaternary ammonium salt, which indicated that the material was about 41.65% SME (monosalt) and about 40.34% SFA (disalt). .

Example 5: preparation of samples with a 2: 1 ratio of SME to SFA

Approximately 53.4g of undigested alpha-thioformic acid were placed in a 500mL 4-neck flask equipped with heating, condenser and stirring. The acid was heated to 130 ℃ for 1 minute to digest the acid. After digestion the acid was cooled to 75 ℃ and about 5.3g of anhydrous methanol was added, which resulted in an exotherm to about 85 ℃. Next, about 6.4g of hydrogen peroxide (35% solution) was added and the resulting mixture was heated to about 120 ℃ for about 5 minutes. After this period of time, the mixture was cooled to about 60 ℃ and 8.82g of water was added to give a gelatinous mixture. The mixture was then cooled further to 40 ℃ and sodium hydroxide (50% solution) was added dropwise until the pH reached 6. The final product was a soft flowable yellow gel. The actives (active) were determined by titration with 0.02N quaternary ammonium salt to be 46.3% SME (monosalt) and 22.5 SFA (disalt).

Example 6: preparation of SME: SFA samples in a 25: 1 ratio

Approximately 50g of undigested α -thiomethyl acid was placed in a 500mL round bottom flask and heated to 130 ℃ using a hot oil bath for 1 minute. A mechanical stirrer with a glass shaft and teflon paddle was used to ensure thorough mixing. The apparatus includes a condenser (allihn type) to prevent any loss of solvent vapour. After digestion the acid was cooled to 70 ℃, approximately 5.3g of anhydrous methanol was added and mixed thoroughly. About 1.825g of hydrogen peroxide (50% solution) was then added and the resulting mixture was heated to about 89 ℃ for about 64 minutes. After this period of time, the mixture was cooled to about 40 ℃, 64.7g of water was added and mixed thoroughly. The acid was neutralized by the addition of sodium hydroxide (50% solution) until a pH of about 6.5 was reached, maintaining a temperature below 45 ℃ throughout the process using a water/ice bath. The final product was analyzed by titration with 0.02N quaternary ammonium salt and was found to contain 35.82% SME (monosalt) and 1.36 SFA (disalt) with a SME to SFA ratio of 26.3: 1.

Example 7: preparation of samples containing various amounts of SME and SFA

In general, samples containing different amounts of SFA and SME (e.g., the total amount of each or either of the two present in the initial liquid mixture, and optionally varying amounts of total SFA and SME actives) can be obtained, for example, by changing the hydrolysis of SME to that of SFA (e.g., by changing the hydrolysis conditions, and/or the amount of methanol used for hydrolysis). Similarly, mixtures may be combined, and/or different amounts of pure (or relatively pure) SME or SFA may be added to adjust the concentration of a particular mixture. Those skilled in the art will recognize how to achieve the specific ratios indicated herein (if not otherwise disclosed), as well as other ratios and formulations encompassed by the technology described herein and the scope of the appended claims.

Example 8: cleansing bar formulations

Table 1 provides two bar formulations without alpha sulfonated alkyl esters or sulfonated fatty acids, or without polyols, used here as control formulations.

TABLE 1

Tables 2-5 provide examples of formulations for skin cleansing bars containing no auxiliary synthetic surfactant, showing the weight percent of the ingredients in the finished cleansing bar.

TABLE 2

TABLE 3

TABLE 4

TABLE 5

Example 9: cleansing bar formulations containing additional synthetic co-surfactants

Examples of skin cleansing bar formulations containing added supplemental synthetic surfactant are given in tables 6-15, showing the weight percent of each ingredient in the finished cleansing bars.

TABLE 6

TABLE 7

TABLE 8

TABLE 9

Watch 10

TABLE 11

TABLE 12

Watch 13

TABLE 14

Watch 15

TABLE 16

Example 9: manufacturing process

The formulations disclosed in tables 1-16 may be prepared according to the following procedure. The following is an exemplary formulation manufacturing process:

and (4) a spiral stirring step. About 127.3 parts of a mixture containing: 31.67% water, 46.7% 85/15 tallow/coconut oil (T/CN) soap, 0.43% sodium chloride, 2.75% glycerin, 4.69% coconut oil free fatty acid (CNFA), 9.46% sodium coconut alpha sulfomethyl ester 1: 1 mono/di ratio slurry, and 3.93% Ninol CMP or LMP, added to the screw mixer in the order specified. The product was mixed at about 85-90 ℃.

And (5) vacuum drying. The screw mixer mixture was then vacuum dried at an absolute pressure of about 50mm Hg to reduce the moisture content of the mixture to 10% and the soap was molded into noodles.

And (5) combining. The soap noodles were weighed and placed in a batch mixer. Adding TiO 0.50 part to noodle 97.0 part₂2.0 parts of perfume, 0.1% BHT, 0.1% citric acid, 0.15 parts of colorant solution, and 0.15 parts of a solution containing about 40% EDTA. The combined ingredients were mixed thoroughly.

And (5) grinding. All of the rolls of the three roll soap mill were set at approximately 85 deg.f to 105 deg.f (29 deg.c to 41 deg.c). The mixture from the mixer was passed through a grinder several times to obtain a homogeneous mixture. This is a direct mixing step.

And (4) a molding and stamping step. The barrel temperature of the conventional screw extruder was set to about 35 ℃ and the nose temperature (nosetemperature) was set to about 42 ℃. The screw extruder used was a two-stage twin-screw extruder between which a vacuum of about 40-65mm Hg was allowed. The soap segments extruded from the screw extruder are generally round and cut into individual plugs (plugs). These plugs are then stamped on conventional soap stamping equipment to give finished soap bars.

It has been found that soap bars made from the above composition have surprising performance and processing advantages. These advantages are illustrated below by damage data, phase behavior and rheology/microstructure distribution.

Example 10: soap bar damage

Damage is damage caused by impact to the soap bars during handling and shipping. This is a well known feature for consumers to rate strips. Bar soap producers prefer that soap formulations with low damage characteristics to reduce consumer rejection should not suffer any damage or rough handling (roughhandling) during shipping. The bars of the invention have low breakage when dropped compared to conventional soap bars. For the purpose of illustration, the soap bars made according to the present invention were tested and the tests quantitatively compared different bars by their damage characteristics.

Each sample was weighed and then dropped from a specified height to damage the strip. As a result, exactly 7 feet provided sufficient impact to clear the failure characteristics of the strip. The strip will fall in such a way that the small end of the strip hits the ground, with the most visible possible damage (vertical impact against the extruded end of the strip). The failure level of the bars was then analyzed in terms of the crack rating of the dry impact bars. Using this rating, the damage value of the strip is determined by grading the visible strip damage.

TABLE 16 Dry impact crack rating

Damage value	Visual characteristics
		0	Without cracking or chipping, smooth dents
1	Very fine spider-web cracks

2	Hairline shaped crack
		3	Visible deep cracks, possibly crumbling
4	Slight chipping along the edge of failure
		5	Significant fragmentation along the impact zone
6	The strips are significantly deformed/crushed and split from the strip in bulk

The analytical strip damage test method is repeatable. Samples were tested in triplicate to ensure reproducibility and to determine standard deviation. The evaluation standard deviation of the sample damage value was 0.39, indicating a high reproducibility in the range of dry impact crack rating 1.

This test method was used to determine the failure characteristics of several experimental bars made according to the technique described herein versus several conventional commercial bars. Each strip was dropped from a height of 7 feet and failure was measured to calculate the total damage value for each sample.

The results are summarized in table 17, indicating that the failure value of the experimental bars according to the present technique is 0, which is lower than the value of any commercial bar evaluated in the test. It is apparent that the compositions of the present invention provide a bar that is less damaging than conventional, conventional or combination bars.

TABLE 17 Damage test results

Sample (I)	Mean value of damage
		Commercially available US combination Bar A	4.66
Commercially available US combination Bar B	3.33
		Commercially available Mexican combination strip A	1.66
The present preparation 3	0.33
		The present preparation 5	0.0
The present preparation 6	0.0

Example 11: viscosity of the oil&Rheology of

It has also been surprisingly found that the soap bar compositions disclosed herein containing sulfonated alkyl esters and polyols are easier to process than conventional soap compositions. Without being bound by any particular theory, it is believed that the enhanced processability of the bar composition of the present invention is due in part to its rheological and viscosity characteristics; in particular, the initial soap slurry compositions according to the present techniques generally have low viscosity at low temperatures. Moreover, formulations according to the present technology generally exhibit a constant viscosity more quickly in shear testing. Table 18 illustrates that certain exemplary formulations of the present technology are less viscous than control samples without sulfonated fatty acids or sulfonated alkyl esters, or without polyols. The viscosity data were obtained in a constant shear measurement at 70 ℃.

Table 18 viscosity of SME soap slurry from constant flow test

Without being bound by any theory, it is believed that the low viscosity is due at least in part to the lower phase transition temperature of the inventive composition from the undesirable hexagonal microstructure to the desirable lamellar microstructure. It is believed that compositions having a lamellar microstructure generally have a lower shear viscosity than compositions having a hexagonal microstructure. Embodiments tested by the technique described herein have a layered microstructure at about 60 ℃ compared to a control sample with a phase transition temperature of about 80 ℃ without SME or polyol. Table 19 illustrates the phase morphology of two embodiments of the present technology compared to a control sample without SME or polyol. In particular, at 60 ℃, the composition without sulfonated fatty acid/alpha sulfonated alkyl ester and polyol shows mainly a hexagonal microstructure, which has high viscosity and yield stress and which is known to be more difficult to process. These tests also show that there is a synergistic relationship in the compositions using or containing the sulfonated fatty acid or alpha sulfonated alkyl ester and the polyol, i.e., the compositions containing both the surfactant and the polyol have a more desirable viscosity and microstructure than the compositions containing only one.

TABLE 19 microstructure of SME soap slurries

It is also believed that the improved rheological and microstructural properties of the compositions of the present invention may also result in improved physical characteristics of the bars produced. For example, in a layered structure, water bonds with polar groups of a surfactant and forms an aqueous phase of a sheet-type highly ordered structure. The water distribution is more uniform and can be homogenized due to the rapid recovery of its structure under shear. This makes the drying properties of the layered soap melt much better. Since the moisture is uniformly distributed in the soap melt/slurry, there are few dry and moist spots in the extruded strands. During storage or use of the strips, different amounts of water are not lost or absorbed causing the strips to crack at the point of differential moisture gradient. Thus, the evaporation of water from the strands made from the layered soap melt/slurry is more uniform over time and can exhibit much better elastic characteristics.

Without being bound by any particular theory, it is believed that the preferred compositions evenly distribute the bound water such that the water does not readily evaporate at storage temperatures. As a result, there is little crystallization in the finished bar, making it less susceptible to damage. This is another positive and desirable quality of SME bar technology.

The present invention, and the manner and method of making and using it, have now been described in such full, clear, concise and exact terms as to enable any person skilled in the art to which it pertains to make and use the same. It will be understood that certain embodiments of the present invention have been described above and that modifications may be made thereto without departing from the spirit and scope of the invention as set forth in the appended claims.

The invention comprises the following technical scheme:

bar composition according to claim 1, comprising:

(a) 40-93% by weight of C₆-C₂₂Soaps;

(b) 1-15% by weight of C₆-C₂₂A fatty acid;

(c) 1% to 30% by weight of a mixture consisting of (i) an alpha sulfonated alkyl ester, a sulfonated fatty acid, or mixtures thereof, and (ii) an auxiliary synthetic surfactant selected from the group consisting of sodium lauryl sulfate, sodium lauryl ether sulfate, potassium lauryl sulfate, magnesium lauryl sulfate, sodium coco sulfate, and mixtures thereof;

(d)0.5 wt% to 2 wt% of an electrolyte selected from the group consisting of sodium sulfate, sodium chloride, sodium carbonate, potassium sulfate, potassium chloride, potassium carbonate, calcium sulfate, calcium chloride, calcium carbonate, magnesium sulfate, magnesium chloride, and magnesium carbonate;

(e)0.01 wt% to 5.0 wt% of a polyol; and

(f) 3-20% by weight of water.

2. The soap bar composition of claim 1 wherein the soap has the formula:

wherein R is₁Is C₆-C₂₂A hydrocarbyl group, an alkyl group, or a combination thereof, n is 1 or 2, and L is a cation.

3. The composition of claim 2, wherein the soap is a mixture of tallow soap and coconut oil fatty acid.

4. The composition of claim 3, wherein the soap comprises 60% to 90% by weight tallow soap and 10% to 40% by weight coconut oil fatty acid soap.

5. The composition of claim 1 comprising an alpha sulfonated alkyl ester having the formula:

wherein R is₃Is C₆-C₂₂Hydrocarbyl, alkyl or combinations thereof, R₄Is straight or branched C₁-C₆Hydrocarbyl, alkyl, or combinations thereof, n is 1 or 2, and M is hydrogen, sodium, potassium, calcium, magnesium, ammonium, monoethanolammonium, diethanolammonium, or triethanolammonium.

6. The composition of claim 1, comprising a sulfonated fatty acid having the formula:

wherein R is₅Is C₆-C₂₂A hydrocarbyl group, an alkyl group, or a combination thereof, N is 1 or 2, wherein N is hydrogen, sodium, potassium, calcium, magnesium, ammonium, monoethanolammonium, diethanolammonium, orAnd (3) triethanolammonium.

7. The composition of claim 1 further comprising up to 10% by weight of an alkanolamide.

8. The composition of claim 1, comprising a mixture of alpha sulfonated alkyl esters and sulfonated fatty acids, the ratio of alpha sulfonated alkyl esters to sulfonated fatty acids being 1: 10 to 10: 1 by weight.

9. The composition of claim 1 wherein the ratio of the alpha sulfonated alkyl ester, sulfonated fatty acid, or mixtures thereof to the auxiliary synthetic surfactant selected from the group consisting of sodium lauryl sulfate, sodium lauryl ether sulfate, potassium lauryl sulfate, magnesium lauryl sulfate, sodium coco sulfate, and mixtures thereof is from 10: 1 to 1: 10 by weight.

10. The composition of claim 1, wherein the electrolyte is sodium chloride, sodium sulfate, potassium chloride, and potassium sulfate.

11. The composition of claim 1 wherein the polyol is selected from the group consisting of glycerin, polyglyceryl esters, sorbitol, propylene glycol and mixtures thereof.

12. The composition of claim 1, comprising 8 wt% to 15 wt% water.

13. The composition of claim 1, wherein the composition has a layered microstructure at 65 ℃.

14. The composition of claim 1, wherein the composition has a phase transition temperature of less than 80 ℃.

Technical solution 15. a method of preparing a personal cleansing or laundry detergent bar premix comprising:

(a) forming an initial mixture at a temperature of 65 ℃ to 105 ℃ comprising:

(i) 40-93% by weight of C₆-C₂₂An aqueous slurry of soap;

(ii) 1-15% by weight of C₆-C₂₂A fatty acid;

(iii) 1-30% by weight of a mixture of an alpha sulfonated alkyl ester, sulfonated fatty acid, or combination thereof and a synthetic surfactant selected from the group consisting of sodium lauryl sulfate, sodium lauryl ether sulfate, potassium lauryl sulfate, magnesium lauryl sulfate, sodium coco sulfate, and mixtures thereof;

(iv)0.5 wt% to 2 wt% of an electrolyte selected from the group consisting of sodium sulfate, sodium chloride, sodium carbonate, potassium sulfate, potassium chloride, potassium carbonate, calcium sulfate, calcium chloride, calcium carbonate, magnesium sulfate, magnesium chloride, and magnesium carbonate;

(v) 0.5-5.0% by weight of a polyol

(b) Removing a sufficient amount of water from the initial mixture to form a thick mixture containing from 3 wt% to 20 wt% residual water; and

(c) the thick mixture is extruded to form an extruded material.

16. The process of claim 15, wherein the residual water comprises 8 wt% to 15 wt% of the thick mixture.

17. The method of claim 15, further comprising molding the extruded material to form a molded material.

18. The method of claim 15, further comprising extruding the moldable material to form a billet, cutting the billet, and stamping the cut billet to obtain the finished product.

19. The process of claim 15 further comprising up to 15 wt.% of an alkanolamide.

20. The method of claim 15, wherein the electrolyte is sodium chloride, sodium sulfate, potassium chloride, and potassium sulfate.

21. The method of claim 15, wherein the polyol is selected from the group consisting of glycerol, polyglycerol esters, sorbitol, propylene glycol and mixtures thereof.

Claims (21)

1. A soap bar composition comprising:

(a) 40-93% by weight of C₆-C₂₂Soaps;

(b) 1-15% by weight of C₆-C₂₂A fatty acid;

(c) 1% to 30% by weight of a mixture consisting of (i) an alpha sulfonated alkyl ester, a sulfonated fatty acid, or mixtures thereof, and (ii) an auxiliary synthetic surfactant selected from the group consisting of sodium lauryl sulfate, sodium lauryl ether sulfate, potassium lauryl sulfate, magnesium lauryl sulfate, sodium coco sulfate, and mixtures thereof;

(d)0.5 wt% to 2 wt% of an electrolyte selected from the group consisting of sodium sulfate, sodium chloride, sodium carbonate, potassium sulfate, potassium chloride, potassium carbonate, calcium sulfate, calcium chloride, calcium carbonate, magnesium sulfate, magnesium chloride, and magnesium carbonate;

(e)0.01 wt% to 5.0 wt% of a polyol; and

(f) 3-20% by weight of water.

2. A bar composition according to claim 1, wherein the soap has the formula:

wherein R is₁Is C₆-C₂₂A hydrocarbyl group, an alkyl group, or a combination thereof, n is 1 or 2, and L is a cation.

3. The composition of claim 2 wherein the soap is a mixture of tallow soap and coconut fatty acid.

4. The composition of claim 3 wherein the soap comprises 60% to 90% by weight tallow soap and 10% to 40% by weight coconut oil fatty acid soap.

5. The composition of claim 1 comprising an alpha sulfonated alkyl ester having the formula:

wherein R is₃Is C₆-C₂₂Hydrocarbyl, alkyl or combinations thereof, R₄Is straight or branched C₁-C₆Hydrocarbyl, alkyl, or combinations thereof, n is 1 or 2, and M is hydrogen, sodium, potassium, calcium, magnesium, ammonium, monoethanolammonium, diethanolammonium, or triethanolammonium.

6. The composition of claim 1, comprising a sulfonated fatty acid having the formula:

wherein R is₅Is C₆-C₂₂Hydrocarbyl, alkyl, or combinations thereof, N is 1 or 2, wherein N is hydrogen, sodium, potassium, calcium, magnesium, ammonium, monoethanolammonium, diethanolammonium, or triethanolammonium.

7. The composition of claim 1 further comprising up to 10% by weight of an alkanolamide.

8. The composition of claim 1 comprising a mixture of alpha sulfonated alkyl esters and sulfonated fatty acids, the ratio of alpha sulfonated alkyl esters to sulfonated fatty acids being from 1: 10 to 10: 1 by weight.

9. The composition of claim 1, wherein the ratio of the alpha sulfonated alkyl ester, sulfonated fatty acid, or mixtures thereof to the auxiliary synthetic surfactant selected from the group consisting of sodium lauryl sulfate, sodium lauryl ether sulfate, potassium lauryl sulfate, magnesium lauryl sulfate, sodium coco sulfate, and mixtures thereof is from 10: 1 to 1: 10 by weight.

10. The composition of claim 1, wherein the electrolyte is sodium chloride, sodium sulfate, potassium chloride, and potassium sulfate.

11. The composition of claim 1 wherein the polyol is selected from the group consisting of glycerin, polyglycerol esters, sorbitol, propylene glycol and mixtures thereof.

12. The composition of claim 1, comprising 8% to 15% by weight water.

13. The composition of claim 1, wherein the composition has a layered microstructure at 65 ℃.

14. The composition of claim 1, wherein the composition has a phase transition temperature of less than 80 ℃.

15. A method of preparing a personal cleansing or laundry detergent bar premix comprising:

(a) forming an initial mixture at a temperature of 65 ℃ to 105 ℃ comprising:

(i) 40-93% by weight of C₆-C₂₂An aqueous slurry of soap;

(ii) 1-15% by weight of C₆-C₂₂A fatty acid;

(iii) 1-30% by weight of a mixture of an alpha sulfonated alkyl ester, sulfonated fatty acid, or combination thereof and a synthetic surfactant selected from the group consisting of sodium lauryl sulfate, sodium lauryl ether sulfate, potassium lauryl sulfate, magnesium lauryl sulfate, sodium coco sulfate, and mixtures thereof;

(iv)0.5 wt% to 2 wt% of an electrolyte selected from the group consisting of sodium sulfate, sodium chloride, sodium carbonate, potassium sulfate, potassium chloride, potassium carbonate, calcium sulfate, calcium chloride, calcium carbonate, magnesium sulfate, magnesium chloride, and magnesium carbonate;

(v) 0.5-5.0% by weight of a polyol

(b) Removing a sufficient amount of water from the initial mixture to form a thick mixture containing from 3 wt% to 20 wt% residual water; and

(c) the thick mixture is extruded to form an extruded material.

16. The process of claim 15 wherein the residual water comprises 8% to 15% by weight of the thick mixture.

17. The method of claim 15, further comprising molding the extruded material to form a molded material.

18. The method of claim 15, further comprising extruding the moldable material to form a billet, cutting the billet, and stamping the cut billet to obtain a finished product.

19. The process of claim 15 further comprising up to 15 wt.% of an alkanolamide.

20. The method of claim 15, wherein the electrolyte is sodium chloride, sodium sulfate, potassium chloride, and potassium sulfate.

21. The method of claim 15 wherein the polyol is selected from the group consisting of glycerol, polyglycerol esters, sorbitol, propylene glycol and mixtures thereof.