Classifications

• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D9/00—Compositions of detergents based essentially on soap
  • C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
  • C11D9/22—Organic compounds, e.g. vitamins
  • C11D9/26—Organic compounds, e.g. vitamins containing oxygen
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/0095—Solid transparent soaps or detergents
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D9/00—Compositions of detergents based essentially on soap
  • C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
  • C11D9/22—Organic compounds, e.g. vitamins
  • C11D9/26—Organic compounds, e.g. vitamins containing oxygen
  • C11D9/267—Organic compounds, e.g. vitamins containing oxygen containing free fatty acids
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D9/00—Compositions of detergents based essentially on soap
  • C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
  • C11D9/48—Superfatting agents

Definitions

• soaps ordinarily identified as milled soap have some small degree of translucency, they have no transparency and are not considered by those skilled in the soap art as transparent soaps. Soaps are known in the art as transparent soaps, however, and some have enjoyed for many years a limited commercial appeal. Such soaps, however, are expensive due to the method of making them, and those so-called transparent soaps which attempted to use cheaper methods of production are no longer found to be acceptable by present day commercial standards.
• One method used in the production of the more acceptable type of transparent soap is to prepare a soap base of reduced moisture content and then dissolve the soap in alcohol, removing the saline impurities by decantation. Alcohol is recovered from the soap by distillation. The soap mass is then cooled to solidify and mold. This method is expensive, time consuming, and involves the use of a high cost solvent. 7
• Tallow which is low in free acid, coconut oil and rosin are saponified with caustic soda in the presence of alcohol or alcohol and glycerine or in the presence of a sugar solution, and the soap mass recovered and molded.
• Another method involves the semi-boiled process and includes crutching the initial oils and fats at approximately 140 F., saponifying with caustic, then adding lye, and stirring until the soap has reached a desired consistency. This is followed by adding sugar dissolved in water, or alcohol and glycerine or combinations thereof. The mass is again crutched at about 160 F., and desired perfume and dyestuff added. The soap mass is molded by framing, then slabbed, cut and pressed. It is well known that neither the cold process nor the semi-boiled process produced soaps of high quality.
• the amount of free fatty acid that can be added is dependent on the amount of polyhydric alcohol used. When the free fatty acid content is increased, the polyhydric alcohol content must also be increased. For best results the quantities of each should be about equal, but the presence of more polyhydric alcohol than free fatty acid will not generally hurt the transparency. On the other hand, if much more free fatty acid than polyhydric alcohol is presentin the soap bar, it tends to become soft and loses transparency.
• the free fatty acid content should not be more than 1% greater than the polyhydric alcohol content, both amounts being by weight of the finishedbar. For example, if a bar contains 3% free fatty acid, it will not be transparent unless at least 2% polyhydric alcohol is present in the bar. In general the sup'erfatted transparent bars will contain from about 1% to about 5% by weight of free fatty acid, and polyhydric alcohol in an amount up to about 10% by weight.
• the salt and moisture limits to obtain transparency of the superfatted bars are not as critical as for non-superfatted bars.
• the moisture content of the finished bars will be in the range from about 17% to about 22.5% by Weight and the salt content thereof will be from amount up to about 10% by weight.
• the primary advantage of the method'of this invention is that it makes possible the economical production of a superfatted transparent soap having excellent lathering properties, firmness and a smooth appearance and waxy feel.
• the superfatted transparent soap can be produced without waste or time loss and with minimum cost. There is no solvent used which must be recovered. No unusual equipment not available in ordinary soap making is required. 5 I
• the superfatted transparent soap produced by the present invention has a pleasing firm yet velvety texture; During washing it does not form a'mushy' coating on its surface, and does not mar the appearance of the soap dish. It does not tend to form unsightly cracks, as is the case with many milled soaps. If the soap of the present invention is maintained for considerable lengths of time J in contact with water, as happens occasionally'when an incompletely dry soap dish is used, 'it may become' cloudy as to that contacted portion, but the soap, upon removal from such contact, will return to its original firmness" and transparency. Furthermore, and most surprisingly, bars of soap made by the process of this invention have the very desirable and unique advantage that they may he used even though worn to wafer thinness. Waste is therefore: avoided.
• i Soaps may range from opaqueness through a translucency into true' transparency, depending upon the method of manufacture.
• Various methods have been used to evaluate the translucency, and more specifically the transparency of soaps; A method for accurately measuring this property of a bar of soap is bythe use of the following apparatus developed for this purpose.
• the conels'ection has a diameter. of /2 inch at the top and 2 /2 inches at the base, which surrounds the face of thelight; thetop of .the'cone section is 9 /2 inches above the face of the lamp, and the lamp is a microscope lamp. with a, 120-volt,- 15-watt bulb having a blue iground-glass filter; The yolta'ge across the lamp J V bulb is adjusted until the light from the top of the cone section shines through a bar having a thickness of 2.75 cm. andiormsa barely perceptible.
• translucency which" is independent of color and is termed Thus, the lower the It is possible to measure readily the TV at other bar thicknesses and interpolate to the standard of 2.75 cm. used herein.
• This method of determining translucency is believed tobe superior to a reflectance test described in the art, be-' cause -it is relatively unalfected by soap color and gloss andavoidsthe difiiculty of cutting a soap bar to a required thickness of only of an inch.
• an ordinary milled toilet V soap of good quality even in the absence of pigments such as titanium dioxide which makes it opaque, has a, TV of greater: than 110, i'.e., it, is too opaque to be measured on the apparatus described. This is 'despite the factthat it has the sheen; and glossiness which are commonly referred toas the translucency of milled soap, to distinguish it from 'the dull nature of frame soaps. .
• the products of the present invention have a TV of 35' or'less, generally 30 or less, when freshly made.
• the mostjconvenient starting material for the present process is soap initially containing from about 28% to 'about 34%, usually approximately 30% to32%, moisture, e.g., a neat kettle soap.
• the precise composition of the initial stock used tov prepare the. soap is not critical 7 g as long as the composition does not differ materially from those ordinarily employed in the manufacture of'rnilled toilet soaps, 'Thus, for example, the relative proportions of fatty acids from .tallow and from coconut oil, and the relative eifeets of such ingredients on the physical characteristics of' milled toilet soap produced therefrom,
• the crutched kettle soap which has a moisture content of from about 28%. to 34%, usuallyiapproximately 30% to 32%, isnext subjected to a drying step.
• the drying is carried out to an extent which permits the desired moisture range to be obtained in the finished bar.
• Thedrying step can be carried out by any of the conventional drying methods, forexample, ordinary cabinet drying, It'is, however, preferred to. use themethod commonly known as flash dryingor, most preferably, the method of tubular drying as is described in US. Patent No. 2,710,067 of Bassett and Packard. When either flash drying or tubular drying I has been'use'd, the, soap at the end of the operation. will.
• the next operation is conveniently that of mixing the soap flakes.
• the polyhydric alcohol and salt may be added to the soap in the chip mixer. It is also a convenient time to adjust the water content and the salt'content.
• the condition of the soaprmass at the time of the mixing operation preferably should beone in which it will permit a, working andshearing of the mass tov be performed, For example, the soap mass should not be so hot that it is too soft or fluid to resist the operation of the mixer. For this reason, the temperature of'the soap at the beginning of the'mixing step should be below about 90 F., and preferably should be in the range of from 80 to 85F.
• the tem perature should not rise above about 110 F and preferably not above 104 51 I I I I
• the moisture content and the salt content must be adjusted so that in the finished product, they will be within the limits discussed above.
• small stock used. .It is, however, not necessary that this be the applicable in the formulation of the soap stock used in 1
• Otheroils which may be used in place ref-coconut oil are babassu,.cohune,.murumuru, ouri'cury, "palm kernel,
• crutching operation is not ;a critical feature of "the invention and may be conducted a by any conventional crutching method.
• the mixture during crutching is, as isconventional, in the liquid phase, at
• An alternative method of obtaining the soap amounts of various optional ingredients are added when desired. These includesuch substances as perfume, coloring material s, lanolin, resin, and preservatives. The presence or absence of any, some, or all of these optional ingredients is not controlling to the production of a superfatted transparent soap. bar having the desired characteristics of a high grade milled soap. 1
• Neat kettle, soap is, a convenient example of the soap starting material. What is required is simply a soap mass, howeverprepared, which is capableof having its moisture and. salt contents. adjusted to the levelsdisclosed herein and tolwhich can be. added. the free fatty acids and polyhydric alcohols.
• Thedrying ofneat kettle soap is only one of the possible ways of obtaining such a soap andwa mass, is, forexample, the reaction between free fatty acids and alkali,to which reaction mixture wateris added or removed asrequired in order to obtain a moisture content withinthe' required range.
• the amount of soap in the mixer and the typeof mixer bladesemployed must be such that the soapotfers a high degree of resistance to the motion of the. blades; because ofthis resistance, the mechanical energy of the mixer blades is converted into heat energy, and'the desired temperature of the mixture thereby obtained without addition of heat from an external source.
• the mixing is conducted for periods of time of about a half hour, the temperature thereby being raised to between 100 to 110 F preferably to between 100 F. and 104 F.
• it is not convenient to spend this amount of time in mixing since the desired transparency is more conveniently obtained during the subsequent milling, which need be no more than a nominal amount.
• the time of mixing generally employed is therefore about 15 minutes, although as little as about 4 minutes is enough to obtain satisfactory blending in of the polyhydric alcohol, salt, and other added materials, such as perfume or dye.
• the amount of working required will vary somewhat depending upon the particular soap stock and the particular working device used.
• the mixing times mentioned above are those for a Barbour-Stockwell mixer with thick counterrotating blades. It is, however, a matter of routine testing to find the preferred conditions when other types o working are used.
• 2,005,333 may be substituted for the usual mill rolls and mixer, assuming always that the same suitable conditions are maintained relative to the soap stock used. It is thus seen that what is required to make transparent soap by the process of the present invention is that a soap mass having the specified proportions of free fatty acid, polyhydric alcohol, salt and Water be subjected to working, its temperature raised to within the range of 100-110 F., preferably 100 F.-l04 F., and subsequently formed into bars. The working may take place during a mixing and/or a milling operation.
• the soap emerges from the mill in the form of very thin, flaky layers suitable for compacting by plodding into a bar form.
• the remaining steps in the conversion into bar form are not critical features, and are successfully accomplished by any conventional means.
• the soap leave the plodder at a temperature of from 98 to 110 F., preferably from 100 F. to 104 F. After the plodding, the soap is cut into individual cakes by usual means.
• the free fatty acid, polyhydric alcohol, water and salt contents be adjusted so that the finished soap has a content thereof within the range specified above.
• a certain portion of the water usually an amount sufiicient to reduce its percentage in the mixture by about 2 to 3, may be lost by evaporation, and this loss must be borne in mind when the water content is adjusted.
• salt When in the specification and the claims the term salt is employed, particular reference is made to sodium chloride, but it is also intended to include other Water-soluble, soap-compatible electrolytes such as potassium chloride and sodium sulfate.
• Kettle soap having a base stock of sodium tallow soap, 15% sodium coconut oil soap and containing about 32% water was charged to a crutcher. Sufficient stearic acid was added so that when the soap was dried and finished at 20% moisture it would contain 2% free stearic acid.
• the batch was heated to 210 F. and then dried to about 20% moisture by tubular drying, The soap was cooled and formed into chips on a chill roll and then placed in a chip mixer.
• Glycerine (2% of finished bar), dispersible pigments, perfume, salt to total 0.6% in the finished bar, lanolin (1% of finished bar) and about 2% water (dependent on the soap chip moisture) were added to the soap and the batch mixed for about /2 hour.
• the soap was milled by passing it over two 5 roll mills and then vacuum plodded. The temperature off the mills and out of the plodder was about F, The bar was highly transparent and possessed good milled soap properties.
• EXAMPLE 2 For this test the final product had the same composition as in Example #1 except no lanolin was added. Soap, glycerine, and stearic acid were mixed together and dried in the molten condition using a steam heated, open Paterson mixer. The dried chips were processed by passing the soap over a three roll mill, five times, and then vacuum plodding. The bar was highly transparent, tough and waxy.
• EXAMPLE 3 A bar was made as in Example #2 but no glycerine was added. This comparative bar was very soft and had poor translucency, thereby illustrating the importance of hav-. ing a polyhydric alcohol present in the bars of the invention.
• the moisture content. of the finished bat was 22.0%; its. salt content.was. 0.45%; its 'TVfwas 20.
• vbar was made "according to the. process of thisinvention froma soap havingabasefstock of 70% sodium tallow soap andf% coconut oil 50319:" Suflicient stearic aci'd'andglycerinewere added so that the finished bar. contained 2% ,stearic acid and 3% 'glycerine. The moisture content of'ithe finished :bar was 182%; its salt content was 0.37%; its TV was 23.
• soap having a Translucency Voltage of no greater than about 35 said process comprising working below about A bar was made according to the process of this invention from a soap having a base stock of 80% sodium ft'allow soap and 20% coconut oil soap.
• "Sufficient stearic acid and pentaerythritol' were. added so that the finished Bar Base Stock Free Polyhydric NaOl 1120 TV No. Fatty Acid ,Alcohol 7 V 1 85% sodiumtallow 2% stearic-..-. 2% sorbitol 21.0 14 soap; 15% sodi- I 7 um coconut soap do do '2%suga-r.----- .65 19.7 22 5%stear1c.
• EXAMPLE 9 effect of the fatty acid but does not deleteniously affect 1 the transparency and processing characteristics of' the bar 'in; an; amount 'up touabout 10.0%, the quantity of said free fatty acid being at most 1% greater thanthe polyhydric alcohol content based on the final bar composition, wherein the mechanical energy is converted' bar contained 2% stearic acid and 1% penta erythritol. into heat energy by working to an extent great enough tion than Ivorysoap, aproduct having a reputation of soap, tallow soap, 2% Emersol 132 and 2% glyeerine.
• the mechanical energy is converted' bar contained 2% stearic acid and 1% penta erythritol. into heat energy by working to an extent great enough tion than Ivorysoap, aproduct having a reputation of soap, tallow soap, 2% Emersol 132 and 2% glyeerine.
• I 1. 'A process for making, a superfatted transparent to cause the mixture to rise in temperature to within a range of from about 100 F. to about 110 F., the moisture and water-soluble soap-compatible, alkali metal neutral salt content having been adjusted prior to the end of the working step to lie within the range from about 17.0% to about 22.5% moisture and an amount of said salt from about 0.2% to about 1%, and plodding the soap mass into bar form.
• a process for making a superfatted transparent soap through which mass one-fourth inch thick, a 14 point boldface type is readable comprising working at a temperature above 90 F. and below 110 F., a toilet soap mass containing from about 1.0% to about 5.0% free soap-forming fatty acid and polyhydric alcohol which overcomes the adverse softening effect of the fatty acid but does not deleteriously affect the transparency and processing characteristics of the bar in an amount up to about the quantity of said free fatty acid being at most 1% greater than the polyhydric alcohol content based on the final bar composition, whereby heat is generated throughout said mass by such working, reducing said mass at a temperature between 100 F., and 1 10 F.
• said process comprising working :a toilet soap mass containing from about 1.0% to about 5.0% free soap-forming fatty acid and polyhydric alcohol which overcomes the adverse softening effect of the fatty acid but does not deleteriously affect the transparency and processing characteristics of the bar in an amount up to about 10%, the quantity of said free fatty acid being at most 1% greater than the polyhydric compound content based on the final bar composition, said soap mass having a moisture content of from 17.0% to about 22.5 and an amount of Water-soluble, soap-compatible, alkali metal neutral salt from about 0.2% to about 1%, whereby the temperature rises to not more than 110 F., reducing the mass to a ploddable form, and plodding into bars while maintaining the temperature substantially uniform, whereby a waxy textured, transparent, isotropic, microcrystalline soap is obtained.
• a superfatted transparent soap bar made from a toilet soap mixture, containing from about 1% to about 5% free soap-forming fatty acid and in which the final soap bar contains an amount of polyhydric alcohol which overcomes the adverse softening efiect of the fatty acid but does not deleteriously affect the transparency and processing characteristics of the bar up to about 10%, from about 17.0% to about 22.5 water and from about 0.2% to about 1% water-soluble, soapcompatible, alkali metal neutral salt, the quantity of free fatty acid being at most 1% greater than the polyhydric alcohol content, which is worked within a temperature range of about F. to about F.
• a superfatted transparent soap bar according to claim 4 which contains from about 1% to about 3% lanolin.
• a superfatted transparent soap bar made from a toilet soap mixture, containing about 2% free soapforming fatty acid and in which the final soap bar contains about 2% glycerine, about 0.6% water-soluble, soapcompatible, alkali metal neutral salt and about 20% moisture, the quantity of said free fatty acid being at most 1% greater than the polyhydric alcohol content, which has been formed by working at a temperature from about 100 F. to about-104 F.

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• Chemical & Material Sciences (AREA)
• Life Sciences & Earth Sciences (AREA)
• Engineering & Computer Science (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Oil, Petroleum & Natural Gas (AREA)
• Wood Science & Technology (AREA)
• Organic Chemistry (AREA)
• Health & Medical Sciences (AREA)
• Emergency Medicine (AREA)
• Detergent Compositions (AREA)
• Cosmetics (AREA)

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Cited By (17)

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Citations (7)

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• 0
  • NL NL264272D patent/NL264272A/xx unknown
• 1960
  • 1960-01-26 US US4626A patent/US3155624A/en not_active Expired - Lifetime
• 1961
  • 1961-01-16 GB GB1464/61A patent/GB972791A/en not_active Expired
  • 1961-01-25 DE DEU7747A patent/DE1167472B/de active Pending

Patent Citations (7)

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