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US2970964A - Opaque liquid detergent composition - Google Patents

Opaque liquid detergent composition Download PDF

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Publication number
US2970964A
US2970964A US653052A US65305257A US2970964A US 2970964 A US2970964 A US 2970964A US 653052 A US653052 A US 653052A US 65305257 A US65305257 A US 65305257A US 2970964 A US2970964 A US 2970964A
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sodium
alkyl
parts
detergent
weight
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US653052A
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William C Krumrei
Blinka Joseph
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Procter and Gamble Co
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Procter and Gamble Co
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Priority to NL226933D priority Critical patent/NL226933A/xx
Priority to BE566727D priority patent/BE566727A/xx
Application filed by Procter and Gamble Co filed Critical Procter and Gamble Co
Priority to US653052A priority patent/US2970964A/en
Priority to DEP20489A priority patent/DE1081172B/en
Priority to FR1200847D priority patent/FR1200847A/en
Priority to GB12160/58A priority patent/GB847712A/en
Priority to CH5843058A priority patent/CH379672A/en
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Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/46Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur
    • A61K8/466Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur containing sulfonic acid derivatives; Salts
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/46Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur
    • A61K8/463Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing sulfur containing sulfuric acid derivatives, e.g. sodium lauryl sulfate
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/12Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/16Sulfonic acids or sulfuric acid esters; Salts thereof derived from divalent or polyvalent alcohols
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/12Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/29Sulfates of polyoxyalkylene ethers
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/0005Other compounding ingredients characterised by their effect
    • C11D3/0089Pearlescent compositions; Opacifying agents
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/02Preparations for cleaning the hair

Definitions

  • This invention relates to a liquid anionic organic synthetic detergent composition which gives good performance and which has a desirable nacreous appearance without the use of opacifiers that afiect stability or act as performance loads.
  • the opacifying agent of this inven tion consists essentially of suspended crystals of an undissolved portion of an anionic organic synthetic detergent constituent and thus contributes to, rather than detracts from, the active detergent of the composition.
  • Translucent and transparent liquid synthetic detergents are common in the industry, but, from a consumer point of view, it has become desirable to develop an efiicient opaque product which has the appearance of liquefied white or colored bar soap. Opacity in a liquid product increases its sight appeal to the purchaser who associates the opacity with his favorite bar soap, powdered soap, or-hand lotion which he has been accustomed to over the years; a transparent or translucent product does not have this particular appeal.
  • opacifiers finely divided organic solids such as wax or stearic acid, and organic liquids such as emulsified fats or oils, adversely affect the sudsing performance of the detergent. dirt particles which the detergent is designed to remove from the fabric and thus create a slightly greater detergency requirement for the product. While some substances such as wax may help produce bubbles, the bubbles are short lived and are unsuitable for dishwashing or laundry sudsing.
  • Opaque liquids are difiicult to prepare from the above mentioned opacifiers because the solids must often be very finelyground or finely ground and introduced into the liquid as a paste. Fine grinding is difiicult in the Inactive opacifying particles are similar to r case of some solids, but often is essential to reduce the tendency toward gravitational separation. Many of the opacifiers comomnly used such as titanium oxide and bentonite have a specific gravity greater than that of the vehicle in which the opacifier is suspended. This factor increases the tendency to settle. An opaque product, to be successful, must have a high degree of stability on standing.
  • An object of this invention is to provide a quality opaque liquid detergent in which the opacifier is also an active component.
  • a further object is to develop an opacifier in a liquid detergent composition which will act compatibly with the rest of the components to form a stable product.
  • a further object is to produce a liquid detergent with a desirable opalescent sheen.
  • the present invention is based on the. discovery that suspended crystals of a.kyl glyceryl ether sulfonates impart to concentrated liquid synthetic detergent solutions a desirable opaque appearance.
  • the aqueous solution of synthetic detergent contains in suspension an alkali metal salt, such as a sodium or potassium salt, of an alkyl glyceryl ether sulfonate having from about 16 to about 18 carbon atoms in the alkyl radical.
  • Electrolyte salts which usually accompany anionic organic sulfuric reaction products together with common water soluble organic solvents, can also be present in the detergent solution as more fully hereinafter defined.
  • the opacifier is normally suspended in the detergent solution by first dissolving a suitable alkyl glyceryl ether sulfonate salt in the detergent solution at a temperature at which the said salt is substantially completely soluble and then cooling the solution to a temperature, preferably room temperature, at which the alkyl glyceryl ether sulfonate salt is substantially insoluble.
  • a suitable composition can also be made by reducing the alkyl glyceryl ether sulionate salt to very small particle form in a colloidal mill and then appropriately suspending such particles in the detergent solution at room temperature, for example.
  • the specific gravity of the alkyl glyceryl ether sulfonate salts used as opacifiers in accordance with this invention is about 1.25, which is only slightly higher than the specific gravity of the detergent solutions (about 1.02 to 1.20). Thus, there is but little tendency toward the gravitational separation that is normally encountered in the use of conventional opacifying agents which present a greater specific gravity differential.
  • the opacifier is substantially insoluble in the concentrated detergent solution at room temperatures, it becomes dissolved when the detergent solution is diluted to the concentrations normally used in forming a washing solution.
  • the opacifiers employed in the instant invention havethe additional advantage of ultimately becoming available as cleansing agents to contribute to the overall detergeney characteristics of the product.
  • liquid detergent compositions of this invention contain from about 25% to about 85% water, they are diluted 200 or more fold when added to water to form the conventional washing solution. This dilution is sufficient to effect substantially complete solution of the suspended opacifier of the detergent composition when the temperature of the wash water is within the temperature range normally employed, i.e., from about 90 F. to about 130 F.
  • the opacifier dissolves to become a part of the active detergent ingredient.
  • plete solution of the alkyl glyceryl ether sulfonate opacifier is desirable for achieving maximum detergency benefit, it has been observed that any undissolved opacifier does not remain completely inert but rather enhances sudsing performance during the washing operation.
  • the substantially insoluble alkyl glyceryl ether sulfonates are those with alkyl chain lengths of about C to about C Alkyl glyceryl ether sulfonates with alkyl chain lengths of C or less are too soluble to be used as opacifiers but are, of course, used extensively as the substantially complete dissolved primary detergent in the present compositions.
  • Single alkyl glyceryl ether sulfonates with an alkyl radical of 16 or 18 carbon atoms can be employed in this invention; but it is ordinarily more Although comsodium sulfite and bisulfite to produce the sodium alkyl glyceryl ether sulfonate.
  • comsodium sulfite and bisulfite to produce the sodium alkyl glyceryl ether sulfonate.
  • To produce the potassium alkyl glyceryl ether sulfonate the corresponding potassium salts are used in the processes.
  • the basic anionic synthetic detergents referred to in this invention are the substantially completely watersoluble (at room temperature) alkali metal (to be interpreted as including ammonium) salts of organic sulfuric recation products having in their molecular structure alkyl radicalshaving from'about 8 to about 18 carbon atoms and radicals selected from the group consisting of sulfonic acid and sulfurici acid ester radicals.
  • the alkali metal salts of the sulfuric reaction products which find greatest utility are those which have from 10 to 14 carbon atoms and predominantly 12 carbon atoms in the alkyl radical, but since other constituents of the detergent molecule can be varied to increase the degree of solubility, the number of carbon atoms in the alkyl radical can also be adjusted upwardly in such instances to as high as 18, for example.
  • Important examples of the synthetics which may be used in the composition of the present invention are the sodium or potassium lauryl glyceryl ether sulfonates made by the processes described above; sodium or potassium alkyl convenient and less expensive to use a mixture of such compounds in which the alkyl radicals are derived from readily available fatty alcohol mixtures.
  • the higher alcohols derived from the reduction of tallow is a preferred source for the production of the opacifier used in the composition of this invention because they contain predominantly 16 and 18 carbon atoms.
  • Another source is the higher molecular weight fraction from a fatty alcohol mixture derived from coconut oil or palm kernel oil. Such mixtures are commonly fractionated in the industry to produce a fraction consisting predominantly of C and C alcohols which have outstanding utility in the preparation of the more soluble synthetic detergents.
  • a by-product of such fractionation is a mixture of alcohols commonly referred to as Stenol, a fatty alcohol mixture consisting predominantly of C and C
  • Stenol a fatty alcohol mixture consisting predominantly of C and C
  • the alkyl glyceryl ether sulfonates which are suitable for the opacifier of the composition of this invention and the more soluble alkyl glyceryl ether sulfonates which can be used as an active synthetic detergent of the composition are produced in the same manner.
  • the first step consists of reacting fatty alcohols with epichlorohydrin to produce alkyl chloroglyceryl ethers.
  • fatty alcohols with alkyl radicals of predominantly 16 or 18 carbon atoms are used; fatty alcohols with alkyl radicals chiefly of 12 or 14 carbon atoms are used in the preparation of the more readily water soluble anionic synthetic detergents.
  • the alkyl chloroglyceryl ethers of step one are then sulfonated to produce the final alkyl glyceryl ether sulfonates.
  • Two sulfonation methods are commonly used. One method consists of reacting the alkyl chloroglyceryl ethers with sodium sulfite. The other method involves treating the alkyl chloroglyceryl ethers with a strong caustic soda solution which forms alkyl glycidyl ethers which in turn are separated from the salt-solution and treated with benzene sulfonates especially those of the types described in U.S.
  • Patents 2,220,099 and 2,477,383 in which the alkyl groups contain from about 9 to about 15 carbon atoms; sodium, potassium or ammonium alkyl sulfates, especially those derived by sulfation of higher alcohols produced by reduction of glycerides of coconut oil; sodium coconut oil fatty acid monoglyceride sulfates and sulfonates; sodium, potassium and ammonium salts of sulfuric acid esters of the reaction product of one mole of coconut oil fatty alcohol and about 3 moles of ethylene oxide or of one mole of tallow fatty alcohol and about 10 moles of ethylene oxide; alkali metal salts of alkyl ethylene oxide ether sulfate which have an average of one unit of ethylene oxide per molecule; the reaction product of fatty acids esterified with isethionic acid and neutralized with sodium hydroxide where, for example, the fatty acids are derived from coconut oil; alkali metal salts of fatty acid amide of a methyl tau
  • the synthetic detergents preferred for use as the basic active cleaning agent in the compositions of this invention include the water soluble alkali metal salts, such as the sodium, potassium, or ammonium alkyl ethylene oxide ether sulfates which have an average of three ethylene oxide units per molecule, alkyl sulfates, alkyl glyceryl ether sulfonates and alkyl benzene sulfonates and mixtures thereof.
  • the basic synthetic detergents can be present in the liquid composition of this invention in percentages of about 5% to 45% by weight although the preferred range is about 15% to 30%.
  • Sufficient alkyl glyceryl ether sulfonate opacifying agent is dissolved in a heated detergent mixture so that from 0.5% to about 10% by weight is insoluble at room temperature. 0.5% of opacifier is about the minimum amount permissible for a satisfactory opaque product; heating to about F. dissolves the opacifier at such concentrations.
  • the presence of about 3% of the in soluble opacifier at room temperature is preferred to re.- tain a proper opacity up to about Above this .facture. .is one of the least soluble of the salts (approximately 6% s temperature this amount of opacifiercompletely dissolves.
  • the top limit of opacifier content is .not critical and up to about 10% or more of the opacifier can be utilized in the practice of this invention although heating the liquid detergent composition to about 180 F. and above is required to dissolve such amounts of opacifier. While other ingredients of the compositions of this invention often exert a slight solubilizing effect on the opacifier, it is merely necessary to add enough of the substantially insoluble alkyl glyceryl ether sulfonate so that at least about 0.5% exists as undissolved suspended crystals at room temperature, generally averaging about 80 F.
  • opacifier and active synthetic detergents used in the practice of this invention result in a product that is thick or viscous when combined only with water, it is often desirable to thin the mixture with a suitable water soluble organic solvent.
  • Ethanol, propanol, isopropanol, ethylene glycol and propylene glycol are useful in this respect and the amounts used are from about to about 25% (ordinarily about 3%-20%) by weight of the composition.
  • Up to about 5% sodium or potassium toluene or benzene sulfonate can also be used as a hydrotrope in conjunction with the above mentioned solvents.
  • water soluble organic solvents also increases the solubility of the active synthetic detergents in water, the solubility increasin in substantially direct proportion to the amount of solvent used.
  • the practical limit of the solubility of common active synthetic detergent salts in water alone is about 25%.
  • up to about 45% of these detergent salts can be used in the liquid compositions of this invention when about 25% of any of the above-mentioned water soluble organic solvents are added.
  • Satisfactory viscosities for the liquid compositions of this invention are in the range of about 150 to about 3000 centipoises at room temperature.
  • Preferred viscos- -ities are in the range of about 200 to 800 centipoises at room temperature.
  • the suspended crystals of the alkyl glyceryl ether sulfonate in the composition of this invention have a high degree of stability against gravitational separation. Tendencies for the crystals to settle can be decreased, for example, by increasing the specific gravity of the solution or by dispersion of the opacifier in very fine crystalline form.
  • the specific gravity of the solution can be increased by the inclusion of sodium salts such as sodium chloride, sodium sulfate, sodium acetate or other compatible salts in the formulation. Thus, the difference between the specific gravity of the solution and that of the suspended crystals can be decreased.
  • the salts may be added in amounts up to the limit of their solubility in the detergent composition. Some salts are presentin the composition as by-products from the synthetic detergent manu- Additional :salts can be added. Sodium sulfate at room temperature) although mixtures of it and other more soluble salts allow an electrolyte content in the compositions of about 2 to 15% by Weight.
  • Corresponding potassium salts can be used with potassium salts of the opacifier and synthetic detergent with similar results.
  • suds stabilizer additives which can be used in the ,preparation of the-detergent compositions of this invention, but which are not necessary, are the monoand diethanolamides of coconut fatty acids.
  • Example I Three moles of ethylene oxide were reacted with one mole of a middle cut coconut fatty alcohol which contained about 65% dodecanol, the balance being essentially fatty alcohols with 14 to 16 carbons.
  • the reaction product was sulfated with chlorosulfonic acid and then neutralized with caustic soda.
  • the resulting alkyl ethylene oxide ether sulfate had an average of three units of ethylene oxide per molecule.
  • the same middle cut coconut alcohol was reacted with 15% excess epichlorohydrin.
  • the chloroglyceryl ether thus formed was sulfonated with sodium sulfite, forming an alkyl glyceryl ether sodium sulfonate.
  • a sodium tallow alkyl glyceryl ether sulfonate was made by the process described above, using a fatty alcohol mixture derived by the reduction of tallow and containing about 65% C alcohol, about 33% C alcohol and about 2% C alcohol.
  • a liquid detergent was made by dissolving the following amounts of ingredients in the water shown at about F.
  • alkyl ethylene oxide ether sodium sulfate derived from the middle cut coconut alcohol 4 parts alkyl glyceryl ether sodium sulfonate derived from the middle cut coconut alcohol 2.5 parts alkyl glyceryl ether sodium sulfonate derived from tallow fatty alcohol 3 parts monoethanolamide of coconut fatty acids 7 parts ethanol 1.5 parts sodium chloride 6 parts sodium sulfate 56 parts water to make 100 parts
  • the formula was rapidly cooled to about 35 F. by passing it through a Votator. It is not necessary to cool as low as 35 F. Passing the detergent solution through a heat exchanger, so that the temperature is brought down to room temperature, about 80 F. rapidly, also produces good appearance and stability.
  • This preparation performed very well in dishpan and fine fabric sudsing and detergency and had the desired pearly opacity and opalescent sheen.
  • alkyl glyceryl ether sulfonate is derived solely from C fatty alcohol or C fatty alcohol instead of tallow fatty alcohol mixture in the above example, sub stantially equal results are obtained.
  • Example 1I The following materials were prepared in the same manner as those in Example I and were dissolved in the water shown below at about F.
  • the sodium alkyl glyceryl ether sulfonates shown below were prepared by the method described in Example I.
  • Sodium alkyl glyceryl ether sulfonate derived from tallow fatty alcohol was prepared as shown in Example I.
  • Example IV The following materials were dissolved in the water shown below at about 120 F.
  • the sodium alkyl glyceryl ether sulfonate was prepared using fatty alcohols derived by the reduction of tallow and containing about 65% C 33% C and 2% C alcohols.
  • polypropylene averaging about 12 carbons 13 parts diethanolamide of coconut fatty acids 19 parts ethanol 2.5 parts sodium tallow alkyl glyceryl ether sulfonate prepared as described in Example I 2.0 parts of a mixture of sodium chloride and sodium sulfate occurring in the synthetic detergents employed 45.5 parts water to make 100 parts After being cooled by passage through a heat exchanger, this preparation was an excellent detergent for dishwashing and had a pleasing opaque appearance with a viscosity of about 400 centipoises. If isopropanol is substituted for the ethanol, substantially equalresults are obtained.
  • Example V The following ingredients were added to the water shown below at about 120 F. and then cooled to form a white opaque rather viscous liquid which was pourable, performed excellently as a detergent and foaming agent.
  • the alkyl glyceryl ether sulfonate was prepared from a mixture of fatty alcohols derived from the reduction of coconut oil and containing about 65% C 25% C and C alcohols.
  • Example V1.A composition of the following ingredicuts was prepared by first effecting substantially complete solution of the solid constituents in the liquid constituents at slightly elevated temperature about 125 F. and then cooling to room temperature, about F. in a heat exchanger. An opaque product having an opalescent sheen and excellent detergency and sudsing properties resulted.
  • Example VII 5 and 10 parts sodium polypropylene benzene sulfonate described in Example IV 5 and 10 parts sodium alkyl phenol ethylene oxide ether sulfate in which there was an average of four ethylene oxide units per molecule and in which the alkyl radical contained about 9 carbon atoms 10 and 20 parts potassium alkyl ethylene oxide ether sulfate produced by reacting one mole of ethylene oxide with one mole of the fatty alcohol mixture as described in this Example VI 5 and 10 parts coconut fatty acid ester of sodium isethionate produced commercially under the trade name Igepon AC-78 20 parts ammonium salt of the alkyl ethylene oxide ether sulfate prepared as described in this Example VI Example VII.A liquid detergent composition was prepared by dissolving the following ingredients in water:
  • Example I 20 parts sodium alkyl ethylene oxide ether sulfate desribed in Example I 3 parts monoethanolamide of coconut fatty acids 7 parts ethanol 1.5 parts of a mixture of sodium chloride and sodium sulfate occurring in the synthetic detergents employed 62 parts water 4 parts of sodium alkyl glyceryl ether sulfonate prepared from coconut'oil fatty alcohol as described in Example VI and 2.5 parts of sodium alkyl glyceryl ether sulfonate prepared from tallow fatty alcohol as described in Examp e I was dispersed in the above composition in a colloidal mill at 60 F. An excellent opaque liquid dishwashing detergent resulted.
  • Example VIII An opaque, fairly viscous, liquid detergent composition was prepared by dissolving the fol lowing ingredients in the water shown at about 150 F. and cooling the composition to room temperature.
  • This invention results in a stable, eificient, light duty detergent with a highly desirable appearance. It is intended mainly for dishwashing and the washing of fine fabrics but can also be used as a hair shampoo and as a detergent for laundry and other general household requirements.
  • an aqueous vehicle containing in solution about to about 25% by weight of a water soluble anionic non-soap synthetic detergent salt and suspended therein about 0.5% to by weight of a crystalline opacifying agent selected from the group consisting of sodium and potassium salts of an alkyl glyceryl ether sulfonate with alkyl radicals ranging in chain length from C to C and which is substantially insoluble in the composition at room temperature.
  • a crystalline opacifying agent selected from the group consisting of sodium and potassium salts of an alkyl glyceryl ether sulfonate with alkyl radicals ranging in chain length from C to C and which is substantially insoluble in the composition at room temperature.
  • an aqueous vehicle containing in solution about 5% to 25% by weight of a water-soluble anionic synthetic detergent salt selected from the group consisting of anionic sulfate and sulfonate synthetic detergents and mixtures thereof, and suspended therein at least about 0.5% to 10% by weight of a crystalline opacifying agent selected from the group consisting of sodium and potassium salts of an alkyl g yceryl ether sulfonate with alkyl radicals ranging in chain length from C to C and which is substantially insoluble in the composition at room temperature.
  • a water-soluble anionic synthetic detergent salt selected from the group consisting of anionic sulfate and sulfonate synthetic detergents and mixtures thereof, and suspended therein at least about 0.5% to 10% by weight of a crystalline opacifying agent selected from the group consisting of sodium and potassium salts of an alkyl g yceryl ether sulfonate with alkyl radicals ranging in chain length from C to C and which is substantially in
  • An opaque liquid detergent composition comprising essentially about 5% to 45% by weight of a water-soluble anionic synthetic detergent salt selected from the group consisting of anionic sufate and sulfonate synthetic detergents and mixtures thereof, about 0.5% to 10% by weight of a suspension of an opacifying agent selected from the group consisting of sodium and potassium salts of an alkyl glyceryl ether sulfonate with alkyl radicals ranging in chain length from C to C and which is substantially insoluble in the composition at room temperature, about 25% to 85% by weight of water and about 0% to 25% by weight of a water-soluble organic solvent selected from the group consisting of ethanol, propanol, isopropanol, ethylene glycol, propylene glycol and mixtures thereof.
  • the opacifying agent is a sodium alkyl glyceryl ether sulfonate in which the alkyl radicals are derived from a fatty alcohol derived by the reduction of tallow.
  • An opaque liquid detergent composition comprising essentially, in an aqueous vehic e, about 15% to 30% by weight of a water-soluble anionic synthetic detergent salt selected from the group consisting of alkyl sulfate, alkyl benzene sulfonate, alkyl ethylene oxide ether sulfate, alkyl glyceryl ether sulfonate and mixtures thereof, about 0.5% to 10% by weight, as an opacifying agent, of a suspension of a sodium salt of an alkyl glyceryl ether sulfonate in which the alkyl radicals are derived from a fatty alcohol derived by the reduction of tallow, at least 2% by weight of a sodium salt of an a kyl glyceryl ether sulfonate in which the alkyl radicals are derived from a mixture of coconut oil fatty alcohols, about 3% to 20% by weight of a water-soluble organic solvent selected from the group consisting of ethanol,
  • the process of preparing opaque liquid detergent compositions which comprises heating a mixture of water, about 5% to 45% by weight of water-soluble anionic synthetic detergent salts selected from the group consisting of anionic sulfate and sulfonate synthetic detergents and mixtures thereof, about 0% to 25% by weight of a water-soluble organic solvent selected from the group consisting of ethanol, propano isopropanol, ethylene glycol, propylene glycol and mixtures thereof, and an opacifying agent selected from the group consisting of sodium and potassium salts of an alkyl glyceryl ether sulfonate with alkyl radicals ranging in chain length from C to C to effect a solution of said mixture and cooling said mixture to at least room temperature to precipitate from about 0.5 to 10% by weight of said opacifying agent in the form of suspended crystals.
  • water-soluble anionic synthetic detergent salts selected from the group consisting of anionic sulfate and sulfonate synthetic detergents and mixtures thereof

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Abstract

Opaque liquid detergent compositions comprise (a) an aqueous solution of an anionic detergent, which contains, as an opacifying agent, (b) a crystalline suspension of an alkylglyceryl ether sulphonate containing 16-18 carbon atoms in the alkyl group, (a) preferably comprises 5-45% by weight of the total composition and may be a monoglyceride sulphate or sulphonate, a fatty acyl isethionate, or a fatty acyl-N-methyl taurine, but is most desirably a sodium, potassium, or ammonium alkyl sulphate, alkylbenzene sulphonate, alkylpolyglycol ether sulphate, alkylglyceryl ether sulphate or any mixture thereof. (b) is suitably a sodium or potassium salt and generally comprises 0.5-10% by weight of the total composition. The composition suitably also contains up to 25% of such organic solvents as ethanol, propanol, isopropanol, or ethylene or propylene glycol. Up to 5% by weight of sodium or potassium benzene- or toluenesulphonate, 2-15% of sodium or potassium chloride, sulphate, or acetate, or mixtures thereof, coconut fatty acid mono- or diethanolamide, perfumes, dyes, and fluorescent brighteners may also be included. Specifications 431,682, 596,560 and 614,044 are referred to.

Description

United States Patent 2 arrests OPAQUE mourn DETERGENT eoMrosrrroN William C. Krumrei, Springdale, and Joseph Blinka, Cincinnati, Ohio, assignors to The Procter dz Gamble Company, Cincinnati, Ohio, a corporation or fihio No Drawing. Filed Apr. 16, 1957, Ser.No. 653,052
'12 Claims. (Cl. 252-161) This invention relates to a liquid anionic organic synthetic detergent composition which gives good performance and which has a desirable nacreous appearance without the use of opacifiers that afiect stability or act as performance loads. The opacifying agent of this inven tion consists essentially of suspended crystals of an undissolved portion of an anionic organic synthetic detergent constituent and thus contributes to, rather than detracts from, the active detergent of the composition.
Translucent and transparent liquid synthetic detergents are common in the industry, but, from a consumer point of view, it has become desirable to develop an efiicient opaque product which has the appearance of liquefied white or colored bar soap. Opacity in a liquid product increases its sight appeal to the purchaser who associates the opacity with his favorite bar soap, powdered soap, or-hand lotion which he has been accustomed to over the years; a transparent or translucent product does not have this particular appeal.
Previous attempts to produce opacity in liquid soaps involved the use of inorganic solids or dispersible organic solids or liquids which did not contribute to detergency and which, in most instances, acted as performance inhibitors and resulted in products which were unstable against phase separation. Thus there is a demand for a mild, high sudsing good cleansing, concentrated liquid synthetic detergent composition which is opaque and which has favorable physical characteristics.
Common methods of producing opacity in liquids are the use of finely divided insoluble solids. These solids are dispersed in the liquid product and nearly always afiect the sudsing performance. In a product designed for dishwashing, for example, good sudsing and suds which last a long time are important because the housewife has come to associate sudsing with cleansing action and as an indicator of the presence of active detergent. The sudsing action of fatty acid soaps is functional, but the synthetic detergents common today generally do not require sudsing for adequate cleaning. However, because of the association of good sudsing with good cleaning quality, it is desirable to market synthetic detergents which suds well. An opacifier which would inhibit good sudsing would be undesirable since it would only add one marketing feature at the expense of another. Common opacifiers, finely divided organic solids such as wax or stearic acid, and organic liquids such as emulsified fats or oils, adversely affect the sudsing performance of the detergent. dirt particles which the detergent is designed to remove from the fabric and thus create a slightly greater detergency requirement for the product. While some substances such as wax may help produce bubbles, the bubbles are short lived and are unsuitable for dishwashing or laundry sudsing.
Opaque liquids are difiicult to prepare from the above mentioned opacifiers because the solids must often be very finelyground or finely ground and introduced into the liquid as a paste. Fine grinding is difiicult in the Inactive opacifying particles are similar to r case of some solids, but often is essential to reduce the tendency toward gravitational separation. Many of the opacifiers comomnly used such as titanium oxide and bentonite have a specific gravity greater than that of the vehicle in which the opacifier is suspended. This factor increases the tendency to settle. An opaque product, to be successful, must have a high degree of stability on standing.
In a highly competitive market, such as household dishwashing detergents, appearance is important. Since pearls and mother-of-pearl have been associated with desirability, product excellence, value and high quality, a pearliness and a satiny sheen is believed to enhance a products appearance. While opacity and an opalescent sheen give an appealing appearance, the product must meet other standards in that it must be uniform in composition and stable and must not afl'ect the sudsing and detergency performance.
An object of this invention is to provide a quality opaque liquid detergent in which the opacifier is also an active component.
A further object is to develop an opacifier in a liquid detergent composition which will act compatibly with the rest of the components to form a stable product.
A further object is to produce a liquid detergent with a desirable opalescent sheen.
The present invention is based on the. discovery that suspended crystals of a.kyl glyceryl ether sulfonates impart to concentrated liquid synthetic detergent solutions a desirable opaque appearance. Thus, in accordance with the present invention, the aqueous solution of synthetic detergent contains in suspension an alkali metal salt, such as a sodium or potassium salt, of an alkyl glyceryl ether sulfonate having from about 16 to about 18 carbon atoms in the alkyl radical. Electrolyte salts which usually accompany anionic organic sulfuric reaction products together with common water soluble organic solvents, can also be present in the detergent solution as more fully hereinafter defined.
The opacifier is normally suspended in the detergent solution by first dissolving a suitable alkyl glyceryl ether sulfonate salt in the detergent solution at a temperature at which the said salt is substantially completely soluble and then cooling the solution to a temperature, preferably room temperature, at which the alkyl glyceryl ether sulfonate salt is substantially insoluble. As the solution is cooled, the alkyl glyceryl ether sulfonate salt precipitates in the form of fine crystals which remain suspended in the detergent solution and which cause the product to have an over-all pearly white opacity. An orientation of the precipitated crystals and a slight crystal growth often causes an opalescent sheen which enhances the opaque appearance. A suitable composition can also be made by reducing the alkyl glyceryl ether sulionate salt to very small particle form in a colloidal mill and then appropriately suspending such particles in the detergent solution at room temperature, for example.
The specific gravity of the alkyl glyceryl ether sulfonate salts used as opacifiers in accordance with this invention is about 1.25, which is only slightly higher than the specific gravity of the detergent solutions (about 1.02 to 1.20). Thus, there is but little tendency toward the gravitational separation that is normally encountered in the use of conventional opacifying agents which present a greater specific gravity differential.
Although the opacifier is substantially insoluble in the concentrated detergent solution at room temperatures, it becomes dissolved when the detergent solution is diluted to the concentrations normally used in forming a washing solution. Thus, the opacifiers employed in the instant invention havethe additional advantage of ultimately becoming available as cleansing agents to contribute to the overall detergeney characteristics of the product.
It will be readily understood that while the liquid detergent compositions of this invention contain from about 25% to about 85% water, they are diluted 200 or more fold when added to water to form the conventional washing solution. This dilution is sufficient to effect substantially complete solution of the suspended opacifier of the detergent composition when the temperature of the wash water is within the temperature range normally employed, i.e., from about 90 F. to about 130 F. Thus, during use, the opacifier dissolves to become a part of the active detergent ingredient. plete solution of the alkyl glyceryl ether sulfonate opacifier is desirable for achieving maximum detergency benefit, it has been observed that any undissolved opacifier does not remain completely inert but rather enhances sudsing performance during the washing operation.
The substantially insoluble alkyl glyceryl ether sulfonates are those with alkyl chain lengths of about C to about C Alkyl glyceryl ether sulfonates with alkyl chain lengths of C or less are too soluble to be used as opacifiers but are, of course, used extensively as the substantially complete dissolved primary detergent in the present compositions.
In order to obtain the opalescent sheen in the opaqe composition of this invention it has been found that at least 2% by weight of alkyl glyceryl ether sulfonate having alkyl chains of C or less must be present. This portion of the more soluble alkyl glyceryl ether sulfonate is necessary to cause a slight crystal growth and an orientation of the suspended, precipitated, opacifying crystals.
Single alkyl glyceryl ether sulfonates with an alkyl radical of 16 or 18 carbon atoms, for example, can be employed in this invention; but it is ordinarily more Although comsodium sulfite and bisulfite to produce the sodium alkyl glyceryl ether sulfonate. To produce the potassium alkyl glyceryl ether sulfonate the corresponding potassium salts are used in the processes.
Many of the various synthetic sulfate and sulfonate detergents well knownin the art are useful as the basic active cleaning agent in the practice of this invention. The following examples of suitable water soluble anionic synthetic detergents are given only for the purpose of illustrating the wide variety of types of detergent compounds useful in the practice of the invention and it will be appreciated that the scope of the invention is not thereby limited.
The basic anionic synthetic detergents referred to in this invention are the substantially completely watersoluble (at room temperature) alkali metal (to be interpreted as including ammonium) salts of organic sulfuric recation products having in their molecular structure alkyl radicalshaving from'about 8 to about 18 carbon atoms and radicals selected from the group consisting of sulfonic acid and sulfurici acid ester radicals. The alkali metal salts of the sulfuric reaction products which find greatest utility are those which have from 10 to 14 carbon atoms and predominantly 12 carbon atoms in the alkyl radical, but since other constituents of the detergent molecule can be varied to increase the degree of solubility, the number of carbon atoms in the alkyl radical can also be adjusted upwardly in such instances to as high as 18, for example. Important examples of the synthetics which may be used in the composition of the present invention are the sodium or potassium lauryl glyceryl ether sulfonates made by the processes described above; sodium or potassium alkyl convenient and less expensive to use a mixture of such compounds in which the alkyl radicals are derived from readily available fatty alcohol mixtures. The higher alcohols derived from the reduction of tallow is a preferred source for the production of the opacifier used in the composition of this invention because they contain predominantly 16 and 18 carbon atoms. Another source is the higher molecular weight fraction from a fatty alcohol mixture derived from coconut oil or palm kernel oil. Such mixtures are commonly fractionated in the industry to produce a fraction consisting predominantly of C and C alcohols which have outstanding utility in the preparation of the more soluble synthetic detergents. A by-product of such fractionation is a mixture of alcohols commonly referred to as Stenol, a fatty alcohol mixture consisting predominantly of C and C These latter mixtures can also be employed as a source of alkyl radicals in the preparation of the opacifier of this composition.
The alkyl glyceryl ether sulfonates which are suitable for the opacifier of the composition of this invention and the more soluble alkyl glyceryl ether sulfonates which can be used as an active synthetic detergent of the composition are produced in the same manner. The first step consists of reacting fatty alcohols with epichlorohydrin to produce alkyl chloroglyceryl ethers. To produce the opacifier, fatty alcohols with alkyl radicals of predominantly 16 or 18 carbon atoms are used; fatty alcohols with alkyl radicals chiefly of 12 or 14 carbon atoms are used in the preparation of the more readily water soluble anionic synthetic detergents. The alkyl chloroglyceryl ethers of step one are then sulfonated to produce the final alkyl glyceryl ether sulfonates. Two sulfonation methods are commonly used. One method consists of reacting the alkyl chloroglyceryl ethers with sodium sulfite. The other method involves treating the alkyl chloroglyceryl ethers with a strong caustic soda solution which forms alkyl glycidyl ethers which in turn are separated from the salt-solution and treated with benzene sulfonates especially those of the types described in U.S. Patents 2,220,099 and 2,477,383 in which the alkyl groups contain from about 9 to about 15 carbon atoms; sodium, potassium or ammonium alkyl sulfates, especially those derived by sulfation of higher alcohols produced by reduction of glycerides of coconut oil; sodium coconut oil fatty acid monoglyceride sulfates and sulfonates; sodium, potassium and ammonium salts of sulfuric acid esters of the reaction product of one mole of coconut oil fatty alcohol and about 3 moles of ethylene oxide or of one mole of tallow fatty alcohol and about 10 moles of ethylene oxide; alkali metal salts of alkyl ethylene oxide ether sulfate which have an average of one unit of ethylene oxide per molecule; the reaction product of fatty acids esterified with isethionic acid and neutralized with sodium hydroxide where, for example, the fatty acids are derived from coconut oil; alkali metal salts of fatty acid amide of a methyl taurine in which the fatty acids, for example, are derived from coconut oil; and others known in the art, a number being specitically set forth in U.S. Patents 2,396,278, Lind; 2,486, 921, Byerly; and 2,486,922, Strain.
The synthetic detergents preferred for use as the basic active cleaning agent in the compositions of this invention include the water soluble alkali metal salts, such as the sodium, potassium, or ammonium alkyl ethylene oxide ether sulfates which have an average of three ethylene oxide units per molecule, alkyl sulfates, alkyl glyceryl ether sulfonates and alkyl benzene sulfonates and mixtures thereof. The basic synthetic detergents can be present in the liquid composition of this invention in percentages of about 5% to 45% by weight although the preferred range is about 15% to 30%.
Sufficient alkyl glyceryl ether sulfonate opacifying agent is dissolved in a heated detergent mixture so that from 0.5% to about 10% by weight is insoluble at room temperature. 0.5% of opacifier is about the minimum amount permissible for a satisfactory opaque product; heating to about F. dissolves the opacifier at such concentrations. The presence of about 3% of the in soluble opacifier at room temperature is preferred to re.- tain a proper opacity up to about Above this .facture. .is one of the least soluble of the salts (approximately 6% s temperature this amount of opacifiercompletely dissolves. The top limit of opacifier content is .not critical and up to about 10% or more of the opacifier can be utilized in the practice of this invention although heating the liquid detergent composition to about 180 F. and above is required to dissolve such amounts of opacifier. While other ingredients of the compositions of this invention often exert a slight solubilizing effect on the opacifier, it is merely necessary to add enough of the substantially insoluble alkyl glyceryl ether sulfonate so that at least about 0.5% exists as undissolved suspended crystals at room temperature, generally averaging about 80 F.
When the amounts of opacifier and active synthetic detergents used in the practice of this invention result in a product that is thick or viscous when combined only with water, it is often desirable to thin the mixture with a suitable water soluble organic solvent. Ethanol, propanol, isopropanol, ethylene glycol and propylene glycol are useful in this respect and the amounts used are from about to about 25% (ordinarily about 3%-20%) by weight of the composition. Up to about 5% sodium or potassium toluene or benzene sulfonate can also be used as a hydrotrope in conjunction with the above mentioned solvents.
The use of water soluble organic solvents also increases the solubility of the active synthetic detergents in water, the solubility increasin in substantially direct proportion to the amount of solvent used. For example, the practical limit of the solubility of common active synthetic detergent salts in water alone is about 25%. However, up to about 45% of these detergent salts can be used in the liquid compositions of this invention when about 25% of any of the above-mentioned water soluble organic solvents are added.
Satisfactory viscosities for the liquid compositions of this invention are in the range of about 150 to about 3000 centipoises at room temperature. Preferred viscos- -ities are in the range of about 200 to 800 centipoises at room temperature.
The suspended crystals of the alkyl glyceryl ether sulfonate in the composition of this invention have a high degree of stability against gravitational separation. Tendencies for the crystals to settle can be decreased, for example, by increasing the specific gravity of the solution or by dispersion of the opacifier in very fine crystalline form.
The specific gravity of the solution can be increased by the inclusion of sodium salts such as sodium chloride, sodium sulfate, sodium acetate or other compatible salts in the formulation. Thus, the difference between the specific gravity of the solution and that of the suspended crystals can be decreased. The salts may be added in amounts up to the limit of their solubility in the detergent composition. Some salts are presentin the composition as by-products from the synthetic detergent manu- Additional :salts can be added. Sodium sulfate at room temperature) although mixtures of it and other more soluble salts allow an electrolyte content in the compositions of about 2 to 15% by Weight. Corresponding potassium salts can be used with potassium salts of the opacifier and synthetic detergent with similar results.
The presence of electrolyte in the warmed clear detergent solution increases the tendency of the opacifier to form fine substantially insoluble crystals upon cooling. A rapid rate of cooling also tends to produce finer crystals of thesusp ended alkyl glyceryl ether sulfonate.
In the preparation of the mixture it should be heated to a temperature only high enough to dissolve all the opacifier, 120 F. to 160 F. is ordinarily sufficient. Cooling by allowing the mixture to stand at room temperature is sufficient to produce a satisfactory opaque product although finer crystals result when the mixture is cooled 'in a heat exchanger, especially one provided with a mechanical agitator, such as a Votator.
Examples of suds stabilizer additives which can be used in the ,preparation of the-detergent compositions of this invention, but which are not necessary, are the monoand diethanolamides of coconut fatty acids.
The following examples are given to illustrate the manner in which this invention may be practiced. Its scope is not limited to the ingredients named in the examples since it is apparent that some may be interchanged with each other or equivalents substituted. Likewise, its scope is not limited to the proportions shown in these examples since the proportions may be varied to modify the viscosity or active detergent concentration and to adjust for variations in properties of substituted equivalent ingredients. The main feature of the invention is the obtaining of a stable, pleasing appearing opacity in a liquid detergent with good cleaning and sudsing perform ance and controlable physical properties.
All parts are shown by weight.
Example I.Three moles of ethylene oxide were reacted with one mole of a middle cut coconut fatty alcohol which contained about 65% dodecanol, the balance being essentially fatty alcohols with 14 to 16 carbons. The reaction product was sulfated with chlorosulfonic acid and then neutralized with caustic soda. The resulting alkyl ethylene oxide ether sulfate had an average of three units of ethylene oxide per molecule.
The same middle cut coconut alcohol was reacted with 15% excess epichlorohydrin. The chloroglyceryl ether thus formed was sulfonated with sodium sulfite, forming an alkyl glyceryl ether sodium sulfonate.
A sodium tallow alkyl glyceryl ether sulfonate was made by the process described above, using a fatty alcohol mixture derived by the reduction of tallow and containing about 65% C alcohol, about 33% C alcohol and about 2% C alcohol.
A liquid detergent was made by dissolving the following amounts of ingredients in the water shown at about F.
20 parts alkyl ethylene oxide ether sodium sulfate derived from the middle cut coconut alcohol 4 parts alkyl glyceryl ether sodium sulfonate derived from the middle cut coconut alcohol 2.5 parts alkyl glyceryl ether sodium sulfonate derived from tallow fatty alcohol 3 parts monoethanolamide of coconut fatty acids 7 parts ethanol 1.5 parts sodium chloride 6 parts sodium sulfate 56 parts water to make 100 parts After complete solution of all the materials the formula was rapidly cooled to about 35 F. by passing it through a Votator. It is not necessary to cool as low as 35 F. Passing the detergent solution through a heat exchanger, so that the temperature is brought down to room temperature, about 80 F. rapidly, also produces good appearance and stability.
This preparation performed very well in dishpan and fine fabric sudsing and detergency and had the desired pearly opacity and opalescent sheen.
When the alkyl glyceryl ether sulfonate is derived solely from C fatty alcohol or C fatty alcohol instead of tallow fatty alcohol mixture in the above example, sub stantially equal results are obtained.
Example 1I.The following materials were prepared in the same manner as those in Example I and were dissolved in the water shown below at about F. The sodium alkyl glyceryl ether sulfonates shown below were prepared by the method described in Example I.
19.7 parts alkyl ethylene oxide ether sodium sulfate derived from the middle cut coconut alcohol described in Example I.
2.95 parts monoethanolamide of coconut fatty acids 3.09 parts alkyl glyceryl ether sodium sulfonate derived from a fractionated mixture of coconut fatty alcohols ao'rdes containing about 65% C 20% C and 15% C alcohols 4.92 parts propylene glycol 4.92 parts ethanol 2.95 parts sodium alkyl glyceryl ether sulfonate derived from a mixture of alcohols consisting essentially of C and C alcohols and derived as the high boiling cut in the fractionation of a mixture of coconut oil alcohols l parts of a mixture of sodium chloride and sodium sulfate 51.47 parts water to make 100 parts This preparation was cooled in a Votator to room temperature, about 80 F. and had good detergent and sudsing properties as well as the desired opaque opalescent sheen.
Example [IL-The following materials were dissolved the water shown below at about 160 F. Sodium alkyl glyceryl ether sulfonate derived from tallow fatty alcohol was prepared as shown in Example I.
37 parts ammonium salt of the sulfated middle cut coconut alcohol containing 65 dodecanol, the remainder consisting essentially of alcohols of 14 and 16 carbon atoms 12 parts monoethanolamide of coconut fatty acids 18 parts ethanol 6 parts sodium alkyl glyceryl ether sulfonate derived from tallow fatty alcohol as described in Example I 2 parts of a mixture of sodium chloride and sodium sulfate occurring in the synthetic detergents employed 25 parts water to make 100 parts This preparation had excellent detergent and sudsing properties and the desired white opacity.
If propanol is substituted for the ethanol, substantially equal results are obtained.
Example IV.The following materials were dissolved in the water shown below at about 120 F. The sodium alkyl glyceryl ether sulfonate was prepared using fatty alcohols derived by the reduction of tallow and containing about 65% C 33% C and 2% C alcohols.
18 parts sodium polypropylene benzene sulfonate, the
polypropylene averaging about 12 carbons 13 parts diethanolamide of coconut fatty acids 19 parts ethanol 2.5 parts sodium tallow alkyl glyceryl ether sulfonate prepared as described in Example I 2.0 parts of a mixture of sodium chloride and sodium sulfate occurring in the synthetic detergents employed 45.5 parts water to make 100 parts After being cooled by passage through a heat exchanger, this preparation was an excellent detergent for dishwashing and had a pleasing opaque appearance with a viscosity of about 400 centipoises. If isopropanol is substituted for the ethanol, substantially equalresults are obtained.
Example V.The following ingredients were added to the water shown below at about 120 F. and then cooled to form a white opaque rather viscous liquid which was pourable, performed excellently as a detergent and foaming agent. The alkyl glyceryl ether sulfonate was prepared from a mixture of fatty alcohols derived from the reduction of coconut oil and containing about 65% C 25% C and C alcohols.
15 parts potassium alkyl glyceryl ether sulfonate 10 parts ethylene glycol. 73 parts water '2 parts potassium chloride occurring in the synthetic detergents employed If two parts of potassium acetate or potassium sulfate are added to the composition in the above example, sub stantially equivalent results are obtained.
Example V1.A composition of the following ingredicuts was prepared by first effecting substantially complete solution of the solid constituents in the liquid constituents at slightly elevated temperature about 125 F. and then cooling to room temperature, about F. in a heat exchanger. An opaque product having an opalescent sheen and excellent detergency and sudsing properties resulted.
20 parts sodium alkyl ethylene oxide ether sulfate produced by reacting 3 moles of ethylene oxide with 1 mole of fatty alcohol containing about 65% C 20% C and 15% C alkyl radicals then sulfating and neutralizing the reaction product. v
4 parts sodium alkyl glyceryl ether sulfonate prepared using a mixture of fatty alcohols derived by the reduction of coconut oil and containing about C 5% C and 5% C alkyl radicals 3 parts sodium alkyl glyceryl ether sulfonate prepared as described in Example I using the fatty alcohol derived by the reduction of tallow 5 parts monoethanolamide of coconut fatty acids 2 parts sodium toluene sulfonate 7 parts ethanol 6 parts sodium acetate 6 parts sodium chloride 47 parts water In this example the following amounts of ingredients in separate compositions can be substituted for equal amounts of the alkyl ethylene oxide ether sulfate with substantially the same results:
5 and 10 parts sodium polypropylene benzene sulfonate described in Example IV 5 and 10 parts sodium alkyl phenol ethylene oxide ether sulfate in which there was an average of four ethylene oxide units per molecule and in which the alkyl radical contained about 9 carbon atoms 10 and 20 parts potassium alkyl ethylene oxide ether sulfate produced by reacting one mole of ethylene oxide with one mole of the fatty alcohol mixture as described in this Example VI 5 and 10 parts coconut fatty acid ester of sodium isethionate produced commercially under the trade name Igepon AC-78 20 parts ammonium salt of the alkyl ethylene oxide ether sulfate prepared as described in this Example VI Example VII.A liquid detergent composition was prepared by dissolving the following ingredients in water:
20 parts sodium alkyl ethylene oxide ether sulfate desribed in Example I 3 parts monoethanolamide of coconut fatty acids 7 parts ethanol 1.5 parts of a mixture of sodium chloride and sodium sulfate occurring in the synthetic detergents employed 62 parts water 4 parts of sodium alkyl glyceryl ether sulfonate prepared from coconut'oil fatty alcohol as described in Example VI and 2.5 parts of sodium alkyl glyceryl ether sulfonate prepared from tallow fatty alcohol as described in Examp e I was dispersed in the above composition in a colloidal mill at 60 F. An excellent opaque liquid dishwashing detergent resulted.
Example VIII.An opaque, fairly viscous, liquid detergent composition was prepared by dissolving the fol lowing ingredients in the water shown at about 150 F. and cooling the composition to room temperature.
10 parts sodium alkyl ethylene oxide ether sulfate described in Example I a 10 parts sodium. polypropylene benzene sulfonate described in Example IV 5 parts sodium alkyl glyceryl ether sulfonate described in Example I using tallow fatty alcohol 2 parts of a mixture of sodium chloride and sodium-sulfate occurring in the synthetic detergents employed 73 parts water to make parts Small amounts of perfumes and fluorescent brightening agents known in the art can be added to improve product appeal and performance. Since the nacreous opacity is the basic feature of the invention, dyes can be added to produce pastel shades which can greatly enhance the customer attraction to the product. If desired, sudsing depressing agents can be employed to yield products especially designed for uses where excessive foaming properties would interfere with the use of the product.
This invention results in a stable, eificient, light duty detergent with a highly desirable appearance. It is intended mainly for dishwashing and the washing of fine fabrics but can also be used as a hair shampoo and as a detergent for laundry and other general household requirements.
What is claimed is:
1. As an opaque liquid detergent composition an aqueous vehicle containing in solution about to about 25% by weight of a water soluble anionic non-soap synthetic detergent salt and suspended therein about 0.5% to by weight of a crystalline opacifying agent selected from the group consisting of sodium and potassium salts of an alkyl glyceryl ether sulfonate with alkyl radicals ranging in chain length from C to C and which is substantially insoluble in the composition at room temperature.
2. As an opaque liquid detergent composition an aqueous vehicle containing in solution about 5% to 25% by weight of a water-soluble anionic synthetic detergent salt selected from the group consisting of anionic sulfate and sulfonate synthetic detergents and mixtures thereof, and suspended therein at least about 0.5% to 10% by weight of a crystalline opacifying agent selected from the group consisting of sodium and potassium salts of an alkyl g yceryl ether sulfonate with alkyl radicals ranging in chain length from C to C and which is substantially insoluble in the composition at room temperature.
3. An opaque liquid detergent composition comprising essentially about 5% to 45% by weight of a water-soluble anionic synthetic detergent salt selected from the group consisting of anionic sufate and sulfonate synthetic detergents and mixtures thereof, about 0.5% to 10% by weight of a suspension of an opacifying agent selected from the group consisting of sodium and potassium salts of an alkyl glyceryl ether sulfonate with alkyl radicals ranging in chain length from C to C and which is substantially insoluble in the composition at room temperature, about 25% to 85% by weight of water and about 0% to 25% by weight of a water-soluble organic solvent selected from the group consisting of ethanol, propanol, isopropanol, ethylene glycol, propylene glycol and mixtures thereof.
4. The detergent composition of claim 3 in which the amount of water-soluble anionic synthetic detergent salts present, includes at least 2% by weight of an alkyl glyceryl ether sulfonate with an alkyl chain length not greater than C whereby an opaque opalescent sheen is obtained.
5. The detergent composition in accordance with claim 3 in which the opacifying agent is a sodium alkyl glyceryl ether sulfonate in which the alkyl radicals are derived from a fatty alcohol derived by the reduction of tallow.
6. The detergent composition in accordance with claim 3 in which the water-soluble anionic synthetic detergent salt is selected from the group consisting of alkyl sulfate, alkyl benzene sulfonate, alkyl ethylene oxide ether sulfate, alkyl glyceryl ether sulfonate and mixtures thereof.
7. The detergent composition in accordance with claim 3 in which there is included as an additional ingredient from 2 to percent by weight of a dissolved alkali metal salt selected from the group consisting of sodium and potassium chlorides, sulfates and acetates to increase the specific gravity of the liquid phase.
8. An opaque liquid detergent composition comprising essentially, in an aqueous vehic e, about 15% to 30% by weight of a water-soluble anionic synthetic detergent salt selected from the group consisting of alkyl sulfate, alkyl benzene sulfonate, alkyl ethylene oxide ether sulfate, alkyl glyceryl ether sulfonate and mixtures thereof, about 0.5% to 10% by weight, as an opacifying agent, of a suspension of a sodium salt of an alkyl glyceryl ether sulfonate in which the alkyl radicals are derived from a fatty alcohol derived by the reduction of tallow, at least 2% by weight of a sodium salt of an a kyl glyceryl ether sulfonate in which the alkyl radicals are derived from a mixture of coconut oil fatty alcohols, about 3% to 20% by weight of a water-soluble organic solvent selected from the group consisting of ethanol, propanol, isopropano ethylene glycol, propylene glycol and mixtures thereof, and about 2% to 15% of a dissolved electrolyte salt selected from the group consisting of sodium chloride, sodium sulfate, sodium acetate and mixtures thereof.
9. The process of preparing opaque liquid detergent compositions which comprises heating a mixture of water, about 5% to 45% by weight of water-soluble anionic synthetic detergent salts selected from the group consisting of anionic sulfate and sulfonate synthetic detergents and mixtures thereof, about 0% to 25% by weight of a water-soluble organic solvent selected from the group consisting of ethanol, propano isopropanol, ethylene glycol, propylene glycol and mixtures thereof, and an opacifying agent selected from the group consisting of sodium and potassium salts of an alkyl glyceryl ether sulfonate with alkyl radicals ranging in chain length from C to C to effect a solution of said mixture and cooling said mixture to at least room temperature to precipitate from about 0.5 to 10% by weight of said opacifying agent in the form of suspended crystals.
10. In the process of claim 9 the step of developing a slight growth and orientation of the suspended crystalsof opacifying agent whereby an opalescent sheen is obtained by including as a portion of said detergent salts at least 2% by weight of an alkyl glyceryl ether sulfonate with an alkyl chain length of not greater than C 11. In the process of claim 9 the step of increasing the specific gravity of said solution by dissolving in said mixture from about 2% to 15 by weight of an electrolyte salt selected from the group consisting of sodium chloride, sodium sulfate, sodium acetate and mixtures thereof.
12. In the process of claim 10 the step of increasing the specific gravity of said solution by dissolving in said mixture from about 2% to 15 by weight of an electrolyte salt selected from the group consisting of sodium chloride, sodium sulfate, sodium acetate and mixtures thereof.
References Cited in the file of this: patent UNITED STATES PATENTS 2,094,489 Hueter Sept. 28, 1937 2,527,077 Preston Oct. 24, 1950 2,607,740 Vitale et al Aug. 19, 1952 2,674,580 Henkin Apr. 6, 1954 2,770,599 Henkin Nov. 13, 1956 OTHER REFERENCES Modern Cosmetics, 1947, 3rd ed., publ. by Drug and Cosmetic Industry, page 36.
American Pharmacy, 2nd ed., 1948, publ. by J. B. Lippincott Co., pages 137-138.
Soap and Sanitary Chemicals; January 1951, pages 38-41, and 117; article by Lesser.

Claims (1)

1. AS AN OPAQUE LIQUID DETERGENT COMPOSITION AN AQUEOUS VEHICLE CONTAINING IN SOLUTION ABOUT 5% TO ABOUT 25% BY WEIGHT OF WATER SOLUBLE ANIONIC NON-SOAP SYNTHETIC DETERGENT SALT AND SUSPENDED THEREIN ABOUT 0.5% TO 10% BY WEIGHT OF A CRYSTALLINE OPACIFYING AGENT SELECTED FROM THE GROUP CONSISTING OF SODIUM AND PATASSIUM SALTS OF AN ALKYL GLYCERYL ETHER SULFONATE WITH ALKYL RADICALS RANGING IN CHAIN LENGTH FROM C16 TO C18 AND WHICH IS SUBSTANTIALLY INSOLUBLE IN THE COMPOSITION AT ROOM TEMPERATURE.
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US2527077A (en) * 1947-06-02 1950-10-24 Procter & Gamble Detergent composition
US2607740A (en) * 1950-05-03 1952-08-19 Colgate Palmolive Peet Co Liquid anionic-dialkylolamide detergent composition
US2674580A (en) * 1950-07-20 1954-04-06 Colgate Palmolive Co Liquid shampoo
US2770599A (en) * 1953-09-23 1956-11-13 Colgate Palmolive Co Stable liquid shampoos

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5310508A (en) * 1992-07-15 1994-05-10 Colgate-Palmolive Company Mild personal cleansing compositions containing sodium alcohol ethoxy glyceryl sulfonate
CN113789228A (en) * 2021-09-19 2021-12-14 浙江珂莉科技有限公司 Multi-effect degreasing dish towel and manufacturing method thereof

Also Published As

Publication number Publication date
FR1200847A (en) 1959-12-24
DE1081172B (en) 1960-05-05
BE566727A (en)
CH379672A (en) 1964-07-15
GB847712A (en) 1960-09-14
NL226933A (en)

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