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US2859182A - Heavy duty liquid detergent composition - Google Patents

Heavy duty liquid detergent composition Download PDF

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US2859182A
US2859182A US619930A US61993056A US2859182A US 2859182 A US2859182 A US 2859182A US 619930 A US619930 A US 619930A US 61993056 A US61993056 A US 61993056A US 2859182 A US2859182 A US 2859182A
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sulfonate
sodium
potassium
liquid detergent
heavy duty
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Frank E Carroll
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Lever Brothers Co
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Lever Brothers Co
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    • 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
    • C11D1/22Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
    • 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
    • C11D1/38Cationic compounds
    • C11D1/52Carboxylic amides, alkylolamides or imides or their condensation products with alkylene oxides
    • C11D1/523Carboxylic alkylolamides, or dialkylolamides, or hydroxycarboxylic amides (R1-CO-NR2R3), where R1, R2 or R3 contain one hydroxy group per alkyl group
    • 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
    • C11D1/38Cationic compounds
    • C11D1/52Carboxylic amides, alkylolamides or imides or their condensation products with alkylene oxides
    • C11D1/526Carboxylic amides (R1-CO-NR2R3), where R1, R2 or R3 are polyalkoxylated
    • 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
    • C11D3/02Inorganic compounds ; Elemental compounds
    • C11D3/04Water-soluble compounds
    • C11D3/06Phosphates, including polyphosphates
    • 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
    • C11D3/16Organic compounds
    • C11D3/34Organic compounds containing sulfur
    • C11D3/3418Toluene -, xylene -, cumene -, benzene - or naphthalene sulfonates or sulfates

Definitions

  • Powdered detergent compositions are generally prepared by spray drying or drum drying which are costly operations. When used in washing, the powdered detergent compositions must be dissolved to form dilute aqueous washing solutions. This step of dissolving or dispersing the powdered detergent compositions in the wash water is time consuming. Frequently the powdered detergent compositions are ditficultly dispersed, since they may tend to form lumps. Powdered. detergent compositions, moreover, tend to vary greatly in density unless particular care is taken in their preparation. Such a variation in density makes it diificult to determine the exact amount thereof to be employed during washing.
  • Heavy duty liquid detergent compositions may contain one or more synthetic detergents and a polyphosphate in an aqueous medium.
  • the presence of a considerable amount of polyphosphate in these compositions causes the synthetic detergents to separate from solution at room temperature, thereby making the product commercially unattractive.
  • the major problem of preparing homogeneous heavy duty liquid deter gent compositions involves the discovery of means for laten ted Nov. ,4, 1958 preventing the synthetic detergents from separating out i of solution at room temperature or below in the presence of a considerable amount of polyphosphate.
  • alkali metalaryl sulfonate did not prove to be a solubilizing agent for-the potassium alkylaryl sulfonate in the presence of a considerable amount of tetrapotassium pyrophosphate nor did the alkylolamides.
  • alkylolamides were lauric isopropanolamide or lauric I diethanolamide or a mixture of the two.
  • the heavy duty liquid detergent compositions containing a potassium alkylaryl sulfonate and tetrapotassium pyrophosphate in an aqueous medium in the presence of an alkali metal aryl sulfonate or at least one alkylolamide were heterogeneous.
  • the potassium alkylaryl sulfonate separated out from solution in the presence of tetrapotassium pyrophosphate even when the composition contained an alkali metal aryl sulfonate or at least one alkylolamide.
  • these liquid detergent compositions were in the form of two layers with pasty solids of potassium alkylaryl sulfonate floating on top of the liquid.
  • Suitable potassium alkylaryl sulfonates include, for example, potassium tertiary-octyl benzene sulfonate, potassium keryl benzene sulfonates obtained by condensing kerosene with benzene and sulfonating the product, potassium nonylbenzene sulfonate, potassium nonyltoluene sulfonate, potassium dodecyltoluene sulfonate, potassium dodecylbenzene sulfonate, and the potassium phenyl polypropylene sulfonates, described in U. S. Patent No. 2,477,383 to Lewis, which are sulfonated phenyl alkanes in which the alkyl carbon at the benzene ring is tertiary:
  • the polyphosphate i. e., tetrapotassium pyrophosphate or pentapotassium tripolyphosphate, is employed in the composition to supply the heavy duty detergent feature of the liquid, and impart good soil removal properties thereto.
  • the amount of polyphosphate is increased, the amount of potassium alkylarylsulfonate is decreased.
  • the alkali metal aryl sulfonate also solubilizes the alkylolamides which are either insoluble in water or incompatible with aqueous solutions of polyphosphates. There is no advantage in adding more of the alkali metal aryl sulfonate than is necessary for its solubilizing effect, since this material appears to contribute nothing to' the detergent and dish-washing characteristics of the heavy duty liquid detergent oomposition.
  • the alkylolamide may be either a monoalkylolamide or a dialkylolamide.
  • suitable alkylolamides are lauric isopropanolamide, lauric diethanolamide, coconut monoethanolamide, capric diethanolamide, tallow diethanolamide, and the monoethanolamide of 1:1 mixttge of caprylic and capric acids.
  • the remaining component of the heavy duty liquid detergent composition is water which serves as a solvent for the components thereof.
  • the liquid detergent composition may contain minor portions of an alkali, such as potassium hydroxide, to neutralize any excess acid impurities present in the components of the composition.
  • minor portions of compatible perfumes, dyes, optical brighteners and other desirable adjuvants may be added to the composition.
  • a typical potassium alkylaryl TABLE HI sulfonate 1. e., potassium phenyl polypropylene sulfonate having 12 carbon atoms in the alkyl chain, was utilized.
  • Example No 11 18 The polyphosphate employed was tetrapotassium pyrophosphate although it will be appreciated that pentapotassium tripolyphosphate in an equal amount could also have been utilized with the same results.
  • a typical alkali metal aryl sulfonate was employed, namely a commerical sodium xylene sulfonate.
  • alkylolamides either monoalkylolamides or dialkylolamides or mixtures thereof, were utilized.
  • compositions were reexposed to room temperature for a number of hours they again became clear homogeneous liquids or opaque liquids or clear liquids containing suspended undissolved solids. In no instance did the com- .positions separate out into two or more layers upon reexposure to room temperature.
  • Examples 7 through 16 containing both an alkali metal aryl sulfonate and at least one alkylolamide with Examples 1 through 6 wherein the compositions contained only an alkali metal aryl sulfonate or at least one alkylolamide readily shows that the presence of both an alkali metal aryl sulfonate and at least one alkylolamide is necessary in order to prevent separation of the potassium alkylaryl sulfonate in the presence of a considerable amount of tetrapotassium pyrophosphate.
  • pentapotassium tripoiyphosphate can be used in lieu of the pyrophosphate with comparable results being obtained.
  • Examples 17 and 18 in Table III below show that an Pgltasslium Phenyl Polypropylene Sulionate (Cu Tetrapotassium Pyrophosphate Sodium Toluene Sullonate Sodium Tetralin Sulionate..
  • alkali metal toluene sulfonate or an alkali metal tetralin 70 g31, ff*' " at Temperature 5 3; g3 sulfonate may be substituted in an equal amount for an fi m 53 :33 alkali metal xylene sulfonate in the compositions of this Liquid Characteristics Alter Storage for 16 hours o a tie Opa lie invention.
  • this table also the amounts of the comgg g g g liquid Stored at F. and than ga g; ponents are presented in percent by weight of the total reexp sedto Room Temperature for2hours. liquid. liquid. composition. 7
  • the detergency and sudsing properties of these compositions are clearly illustrated by the following standardized dishwashing test.
  • the test involved the washing of specially soiled dishes with an aqueous solution of the soluble alkali metal silicate, such as sodium or potassium silicate.
  • the soluble alkali metal silicate such as sodium or potassium silicate.
  • the pH thereof must be adjusted to about 11.4 or above by the addition of free liquid detergent composition and counting the dishes alkali, such as potassium hydroxide, to keep the silicate which were washed before the suds disappeared.
  • the in solution Typical alkali metal silicates include the temperature of the wash water containing the liquid sodium or potassium silicates having the following alkali detergent composition was 115 F.
  • aqueous wash to silica ratios 1:3.92, 1:3.45, 1:2.4, 1:1.8, 1:2.5, and water solutions were prepared by mixing 10 gram and 1:2,0. 30 gram portions of the composition of Example in 10 A typical composition in percent by weight containing six quarts of water of 120 p. p. m. hardness.
  • an alkali metal silicate is set forth in Example 21.
  • Example 15 grams of the composition of Example 15 was employed E l 21 in the test, 19 dishes were washed before the suds disappeared, while a 30 gram portion of the composition of Potassium hen 1 1 m 1cm lf t Example 15 in the-wash water enabled more than 43 15 (Cu ifi ff MLv dishes to be washed before the suds disappeared. It will Tetrapotassium pymphosphate be appreciated that other typical examples of the com- Sodium xylene Sultanate (commercianu positions of this invention set forth above would give Laurie isopmpanolamide comparable results in this test.
  • the wash period was for 20 minutes at a temperneous m ature of 120 F.
  • the reflectance of the test cloth was measured by means of a Hunter Reflectometer before Further modifications of the compositions of the invenwashing and after washing. The gain in reflectance of tion showing other variations in components and the the soiled test cloths was used as a measure of the amount amounts thereof are set forth below. In all of these of soil removed from the cloth. examples the compositions were clear homogeneous This test was applied to a simple system of organic liquids at room temperature.
  • composition C a heavy duty liquid detergent composition of the invention
  • the tendency of polyphosphate detergents to corrode aluminum may be inhibited by the addition to the homogeneous heavy duty liquid detergent compositions of an amount up-to about 8% on a solids basis of a water- Examples 30-41 T o the following base formula there were added vary- 7 ing amounts of alkali metal aryl sulfonates as indicated below to form clear homogeneous heavy duty liquid detergent compositions which were still homogeneous after three or more months storage at room temperature
  • Components Percent by weight Potassium dodecylbenzene sulfonate ..v 10.
  • Marcel diethanolamide 3.8.. Laurie isopropanolamide 3.2.
  • Sodium silicate (Na OzsiOg of Alkali metal arylsulfonate As indicated below. Water-J-KOH to pH 12.2 Suflicient amount to make components total Total 100.
  • Example 30 contained 5.5 of sodium toluene sulfonate.
  • Example 31 contained 5.5% of sodium ethylbenzene sulfonate.
  • Example 32 contained 5.5% of sodium ortho-xylene sulon te.
  • Example 33 contained 7% of sodium isopropylbenzene sulfonate.
  • Example 34 contained 5.5% of sodium meta-xylene sulfonate.
  • Example 35 contained 7.5% of sodium tetralin sulfonate.
  • Example 36 contained 5.5% total of a mixture of 80% sodium toluene sulfonate and 20% sodium ethylbenzene sulfonate.
  • Example 37 contained 5.5% total of a mixture of 61% sodium ortho-xylcne sulfonate and 39% sodium isopropylbenzcnc sulfonate.
  • Example 38 contained 6% total of a mixture of 15% sodium ortho-xylcnc sulfonatc, 70% sodium metaxylene sulfonate, and 15% sodium para-xylene sulfonate.
  • Example 39 contained 6% total of a mixture of 47% sodium toluene sulfonate plus 53% of a mixture of 15% sodium ortho-xylene sulfonate, 70% sodium metaxylene sulfonatc, and 15% sodium para-xylene sulfonate.
  • Example 40 contained 7% total of a mixture of 22% sodium ortho-xylene sulfonate, 53% sodium metaxylene sulfonate, sodium para-xylene sulfonate, 18% sodium ethylbenzene sulfonate, and 2% sodium toluene sulfonate.
  • Example 41 contained 7% total of a mixture of sodium toluene sulfonate plus 90% of a mixture of 22% sodium ortho-xylene sulfonate, 53% sodium meta-xylene sulfonate, 5% sodium para-xylene sulfonate, 18% sodium ethyl'oenzene sulfonate, and 2% sodium toluene sulfonate.
  • a homogeneous heavy duty liquid detergent composition consisting essentially of an aqueous solution of from about 7% to about 16% of a potassium alkylaryl sulfonate having the general formula where R is an alkyl group containing from 1 to carbon atoms, at least one R having 8 to 15 carbon atoms, and x is a number from 1 to 5; from about 4% to about 12% total of alkali metal arylsulfonate selected from the group consisting of toluene sulfonate, tetralin sulfonate, ethylbenzene sulfonate, isopropylbenzene sulfonate, or-
  • a homogeneous heavy duty liquid detergent composition as set forth in claim 1 containing an amount up to about 8% on a solids basis of a water-soluble alkali metal silicate having an alkali to silica ratio of from 1:1.8 to 113.92, said composition having a pH of at least about 11.4;
  • potassium alkylaryl sulfonate is about 10%, the total amount of alkali metal arylsulfonate is about 7%, the amount of potassium polyphosphate is about 20%,
  • the total amount of the alkylolamide compounds is from about 4% to about 7%.
  • Example 16 Columns 5 and 6, Table II, Example 14, third item, for "6.5g” read I 6.5 same table, Example 16, lines 6 to 10 inclusive, insert leaders; Table III, Example l8, line :4, insert leaders; Table IV, Example 20, line 5, insert leaders, column '7, line 57, for "Pheny” read Phenyl Signed and sealed this 17th day of March 1959.
  • the homogeneous heavy duty liquid detergent composition of this invention is prepared ,by mixing the components thereof together in the aqueous medium. Heat may be conveniently utilized during the mixing of the components to increase the rate of dissolution thereof.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Inorganic Chemistry (AREA)
  • Detergent Compositions (AREA)

Description

in their opened containers.
HEAVY DUTY LIQUID DETERGENT coMPosrnoN Frank E. Carroll, Glen Rock, N. 1., assignmto Lever Biothers Company, New York, N. Y., a corporation Maine No Drawing. Application November 2, 1956 Serial No. 619,930
5 Claims. (Cl. 252-137) The present invention relates to detergent compositions and more particularly to homogeneous heavy duty liquid detergent compositions.
Many detergent compositions have heretofore been prepared, but they have primarily been in a powdered form and thereby have many disadvantages enumerated below. Powdered detergent compositions are generally prepared by spray drying or drum drying which are costly operations. When used in washing, the powdered detergent compositions must be dissolved to form dilute aqueous washing solutions. This step of dissolving or dispersing the powdered detergent compositions in the wash water is time consuming. Frequently the powdered detergent compositions are ditficultly dispersed, since they may tend to form lumps. Powdered. detergent compositions, moreover, tend to vary greatly in density unless particular care is taken in their preparation. Such a variation in density makes it diificult to determine the exact amount thereof to be employed during washing. In addition, powdered detergent compositions may be diificult to dispense, since they sometimes clog the orifices of a dispenser. Also powdered detergent compositions have a tendency to cake at high humidities upon standing Moreover, powdered detergent compositions being normally sold in cardboard containers are subject to spillage and waste in the event an opened container is accidentally knocked over. Furthermore, their dustiness may be bothersome, especially to persons who sufier from dust allergies.
All of these disadvantages of powdered detergent compositions can be obviated by employing liquid detergent compositions. While light duty liquid detergent compositions have been prepared, they have proved to be suitable only for dishwashing and the cleaning of fine fabrics. Light duty liquid detergent compositions are unsatisfactory for washing heavily soiled cotton fabrics, since such compositions have inadequate soil removal characteristics. Heavy. duty liquid detergent compositions, on the other hand, have excellent soil removal characteristics and are ideally suited for the washing of heavily soiled cotton fabrics and other fabrics. However, it has proved rather diflicult to prepare homogeneous heavy duty liquid detergent compositions.
Heavy duty liquid detergent compositions may contain one or more synthetic detergents and a polyphosphate in an aqueous medium. However, the presence of a considerable amount of polyphosphate in these compositions causes the synthetic detergents to separate from solution at room temperature, thereby making the product commercially unattractive. Hence, the major problem of preparing homogeneous heavy duty liquid deter gent compositions involves the discovery of means for laten ted Nov. ,4, 1958 preventing the synthetic detergents from separating out i of solution at room temperature or below in the presence of a considerable amount of polyphosphate.
In attemptying to solve this problem compositions were prepared eontaininga synthetic anionic nonsoap detergent and a polyphosphate in an aqueous medium to which were added various solubilizing agents. More speeifically,-compositions were prepared containing a potassium alkylaryl sulfonate and tetrapotassium vpyrophosphate in an aqueous medium to which were added either an alkali metal aryl sultonate or at least one alkylolamide as prospective solubilizing agents forthe anionic detergent-in an eitort to obtain a homogeneous heavy duty liquid detergent composition. However, the alkali metalaryl sulfonate did not prove to be a solubilizing agent for-the potassium alkylaryl sulfonate in the presence of a considerable amount of tetrapotassium pyrophosphate nor did the alkylolamides.
This is clearly illustrated in Examples 1 through 6 in Table I below wherein the components of the composition are given in percent by weight. In these examples a typical potassium alkylaryl sulfonate. was employed, i. e., potassium phenyl polypropylene sulfonate containing 12 carbon atoms in the alkyl chain. Thev alkali metal aryl sulfonate used as a prospective solubilizing agent was a commercial sodium xylene sulfonate.
The alkylolamides were lauric isopropanolamide or lauric I diethanolamide or a mixture of the two.
TABLE I Example No 1 2 3 4 5 0 Potassium Phen i Poiypropylmperature (-75 F.)
I Tim layers, ty solids floating on to of liquid. Partial separation. I Two lsyem pa sty solids floating on t p at liquid. Complete separa- From a study of the above examples it ean'be l2 to about 15 carbon atoms.
readily that the heavy duty liquid detergent compositions containing a potassium alkylaryl sulfonate and tetrapotassium pyrophosphate in an aqueous medium in the presence of an alkali metal aryl sulfonate or at least one alkylolamide were heterogeneous. The potassium alkylaryl sulfonate separated out from solution in the presence of tetrapotassium pyrophosphate even when the composition contained an alkali metal aryl sulfonate or at least one alkylolamide. At room temperature these liquid detergent compositions were in the form of two layers with pasty solids of potassium alkylaryl sulfonate floating on top of the liquid.
It was found, however, in accordance with the invention that when both an alkali metal aryl sulfonate and at least one alkylolamide were used together in the heavy duty liquid detergent compositions containing a potassium alkylaryl sulfonate and tetrapotassium pyrophosphate or pentapotassium tripolyphosphate in an aqueous medium that heavy duty liquid detergent compositions could be obtained which were homogeneous at room temperature. The homogeneous heavy duty liquid detergent compositions of the present invention therefore consist essentially of an aqueous solution of from about 7% to about 16%, and preferably about of a potassium alkylaryl sulfonate, from about 4% to about 12% total, and preferably about 7% total of one or more alkali metal aryl sulfonates, from about 27% to about 10%, and preferably about 20%," of tetrapotassium pyrophosphate or pentapotassium tripolyphosphate, and from about 2% to about total and preferably from about 4% to about 7% total, of at least one alkylolamide or an ethylene oxide condensation product thereof.
The potassium alkylaryl sulfonates have the general formula where R is an alkyl group, which may be saturated or unsaturated and straight or branched chain, having from 1 to 15 carbon atoms, at least one R having 8 to 15 carbon atoms, x is a number from 1 to 5, and may be an average number. Suitable potassium alkylaryl sulfonates include, for example, potassium tertiary-octyl benzene sulfonate, potassium keryl benzene sulfonates obtained by condensing kerosene with benzene and sulfonating the product, potassium nonylbenzene sulfonate, potassium nonyltoluene sulfonate, potassium dodecyltoluene sulfonate, potassium dodecylbenzene sulfonate, and the potassium phenyl polypropylene sulfonates, described in U. S. Patent No. 2,477,383 to Lewis, which are sulfonated phenyl alkanes in which the alkyl carbon at the benzene ring is tertiary:
where R and R taken together with the remainder of the polypropylene radical form an alkyl group having an average molecular weight corresponding to from about The potassium alkylaryl sulfonate anionic detergent is used in the composition to supply a portion of the foaming and wetting action necessary in a heavy duty liquid detergent product designed for household use.
The polyphosphate, i. e., tetrapotassium pyrophosphate or pentapotassium tripolyphosphate, is employed in the composition to supply the heavy duty detergent feature of the liquid, and impart good soil removal properties thereto. As the amount of polyphosphate is increased, the amount of potassium alkylarylsulfonate is decreased.
The alkali metal aryl sulfonate or mixtures thereof.
fonate, a mixture of 61% ortho-xylene sulfonate and 39% isopropylbenzene sulfonate, a mixture of 15% orthoxylene sulfonate, 70% meta-xylene sulfonate, and 15% para-xylene sulfonate, a mixture of 47% toluene sulfonate plus 53% of a mixture of 15% ortho-xylene sulphonate, 70% meta-xylene sulfonate, and 15% paraxylene sulfonate, a mixture of 22% ortho-xylene sulfonate, 53% meta-xylene sulfonate, 5% para-xylene sulfonate, 18% ethylbenzene sulfonate, and 2% toluene sulfonate, and a mixture of from about 1% to about 10% toluene sulfonate plus from about 99% to about of a mixture of 22% ortho-xylene sulfonate, 53% meta-xylene sulfonate, 5% para-xylene sulfonate, 18% ethylbenzene sulfonate, and 2% toluene sulfonate. The
alkali metal aryl sulfonate is employed in the heavy.
duty liquid detergent composition to aid in solubilizing the potassium alkylaryl sulfonate in the presence of a considerable amount of the polyphosphate and other inorganic materials. The alkali metal aryl sulfonate also solubilizes the alkylolamides which are either insoluble in water or incompatible with aqueous solutions of polyphosphates. There is no advantage in adding more of the alkali metal aryl sulfonate than is necessary for its solubilizing effect, since this material appears to contribute nothing to' the detergent and dish-washing characteristics of the heavy duty liquid detergent oomposition.
The alkylolamide may be either a monoalkylolamide or a dialkylolamide. Typical examples of suitable alkylolamides are lauric isopropanolamide, lauric diethanolamide, coconut monoethanolamide, capric diethanolamide, tallow diethanolamide, and the monoethanolamide of 1:1 mixttge of caprylic and capric acids. The
isopropanolamide in 7%.: amounts as the alkylolamide component of the composition causes the compositions to be opaque solids at room temperature rather than clear homogeneous liquids. Also it was found that sulfonated higher fatty acid amides or polyether alkylene compounds were not suitable for use in lieu of an alkylolamide as a solubilizer, since compositions prepared containing 7% of these compounds separated into two layers at room temperature and hence were not homoge- 1160!.18.
Other suitable alkylolamides which may also be employed include ethylene oxide condensation products thereof, for example, the condensation product of one mole of lauric monoethanolamide with one mole of ethylene oxide and the condensation product of one .mole of lauric isopropanolamide with one mole of ethylene oxide. All of the above alkylolamides may be used either singly or in suitable mixtures.
The remaining component of the heavy duty liquid detergent composition is water which serves as a solvent for the components thereof.
If desired, the liquid detergent composition may contain minor portions of an alkali, such as potassium hydroxide, to neutralize any excess acid impurities present in the components of the composition. In addition, minor portions of compatible perfumes, dyes, optical brighteners and other desirable adjuvants may be added to the composition.
TABLE 11 Example No 7 8 9 10 11 12 13 14 15 16 Potassium Phenyl Polypropylene Bullonate (C alkyl).
'Ietrapotassium Pyrophosphate Sodium Xylene Sullonate (Commercial).
Water a6 5 Laurie Isopmnnnnlamida Laurie Dipthnnnlamirlp Coconut Monoethauolamide Capric Diethanolamide Liquid Characteristics at Room Tempor- Clear ature (70-75 F.) homohomohomogeneous 881160 861160! 881180113 861180115 geneous 881190115 891180118 geneous B81190 liquid. liquid. liquid. liquid. liquid. liquid. liqduid. liquid. it did. llqllllld. LiquldCharacteristics After Storage for Opaque do Viscous Viscous do Opaque o Opa ue Coudy Bo da 16 hours at 40 F. lid. opaque o ue uid qui h0moseparate.
liquid. liq d. u Characteristics of liquid Stored at 40 F. Opaque Clear Clear Clear leer C ear Clear and then reexposed to Room Temperliquid. homoliquid liquid liquid liquid hornoature for 6 hours. geneous containigg in 2 3 $6 geneous liquid. d hours. hours. hour. liquid.
on solved solids. CloudPolnt( --6 -s --i2 -8 +3 +6. Clear Point 0.) 0 +21.
In the above examples a typical potassium alkylaryl TABLE HI sulfonate, 1. e., potassium phenyl polypropylene sulfonate having 12 carbon atoms in the alkyl chain, was utilized. Example No 11 18 The polyphosphate employed was tetrapotassium pyrophosphate although it will be appreciated that pentapotassium tripolyphosphate in an equal amount could also have been utilized with the same results. A typical alkali metal aryl sulfonate was employed, namely a commerical sodium xylene sulfonate. Various alkylolamides, either monoalkylolamides or dialkylolamides or mixtures thereof, were utilized.
These examples clearly illustrate that when a typical potassium alkylaryl sulfonate anionic detergent and a tetrapotassium pyrophosphate are suspended in an aqueous medium in the presence of a suitable alkali metal aryl suifonate and at least one alkylolamide in the correct proportions set forth above that heavy duty liquid detergent compositions are produced which are clear and homogeneous at room temperature. The detergent compositions in many instances are even clear homogeneous liquids after storage for 16 hours at F. In other instances the compositions when stored for 16 hours at 40 F. became opaque solids or opaque liquids or actually separated into a solid phase. However, when these compositions were reexposed to room temperature for a number of hours they again became clear homogeneous liquids or opaque liquids or clear liquids containing suspended undissolved solids. In no instance did the com- .positions separate out into two or more layers upon reexposure to room temperature.
A comparison of Examples 7 through 16 containing both an alkali metal aryl sulfonate and at least one alkylolamide with Examples 1 through 6 wherein the compositions contained only an alkali metal aryl sulfonate or at least one alkylolamide readily shows that the presence of both an alkali metal aryl sulfonate and at least one alkylolamide is necessary in order to prevent separation of the potassium alkylaryl sulfonate in the presence of a considerable amount of tetrapotassium pyrophosphate. As noted above pentapotassium tripoiyphosphate can be used in lieu of the pyrophosphate with comparable results being obtained.
Examples 17 and 18 in Table III below show that an Pgltasslium Phenyl Polypropylene Sulionate (Cu Tetrapotassium Pyrophosphate Sodium Toluene Sullonate Sodium Tetralin Sulionate..
Laurie Dii ha hiilamide 3.
Liquid Characteristics at Room Temperature Liquid Characteristics After Storage for 10 hours at 40 F.
Characteristics of Liquid Stored at 40 F. and then to Room Temperature for 1 hour.
Cloud Point C.)
In Examples 17 and 18 wherein sodium toluene suifonate or sodium tetralinsulfonate were substituted for' sodium xylene sulfonate as the alkali metal aryl sulfonate in the composition, the compositions were clear in the presence of a considerable amount of the poly;
Water Condensation product of one mole oi laur o ethanolamlde with one mole of eth lene oxide.
Condensation product of one mole of aurlc isopropanolamide with one mole oi ethylene oxide.
alkali metal toluene sulfonate or an alkali metal tetralin 70 g31, ff*'=" at Temperature 5 3; g3 sulfonate may be substituted in an equal amount for an fi m 53 :33 alkali metal xylene sulfonate in the compositions of this Liquid Characteristics Alter Storage for 16 hours o a tie Opa lie invention. In this table also the amounts of the comgg g g g liquid Stored at F. and than ga g; ponents are presented in percent by weight of the total reexp sedto Room Temperature for2hours. liquid. liquid. composition. 7
The detergency and sudsing properties of these compositions are clearly illustrated by the following standardized dishwashing test. The test involved the washing of specially soiled dishes with an aqueous solution of the soluble alkali metal silicate, such as sodium or potassium silicate. When a water-soluble alkali metal silicate is added to the composition, the pH thereof must be adjusted to about 11.4 or above by the addition of free liquid detergent composition and counting the dishes alkali, such as potassium hydroxide, to keep the silicate which were washed before the suds disappeared. The in solution. Typical alkali metal silicates include the temperature of the wash water containing the liquid sodium or potassium silicates having the following alkali detergent composition was 115 F. The aqueous wash to silica ratios: 1:3.92, 1:3.45, 1:2.4, 1:1.8, 1:2.5, and water solutions were prepared by mixing 10 gram and 1:2,0. 30 gram portions of the composition of Example in 10 A typical composition in percent by weight containing six quarts of water of 120 p. p. m. hardness. When 10 an alkali metal silicate is set forth in Example 21. grams of the composition of Example 15 was employed E l 21 in the test, 19 dishes were washed before the suds disappeared, while a 30 gram portion of the composition of Potassium hen 1 1 m 1cm lf t Example 15 in the-wash water enabled more than 43 15 (Cu ifi ff MLv dishes to be washed before the suds disappeared. It will Tetrapotassium pymphosphate be appreciated that other typical examples of the com- Sodium xylene Sultanate (commercianu positions of this invention set forth above would give Laurie isopmpanolamide comparable results in this test. Laurie diethanolamide eso l removal propertiesof the homogeneous heavy 20 Potassium silicate (30%) (Kaozsioa of I duty hqurd detergent COlTiPOSlflOnS of this invention are 1332) 12. shown by the following test. The soil removal test con- Water plus potassium hydroxide (pH sisted of washing eight cotton test cloths artificially soiled 121) with vacuum cleaner dust in a Terg-O-Tometer in water Percent silicate Solids in 5 hav ng a hardness of 180 p. p. m. calcium Vs mag- Liquid characteristics at room tempera, nesium) using 0.26% concentration of the product to be tum clemhomes? tested. The wash period was for 20 minutes at a temperneous m ature of 120 F. The reflectance of the test cloth was measured by means of a Hunter Reflectometer before Further modifications of the compositions of the invenwashing and after washing. The gain in reflectance of tion showing other variations in components and the the soiled test cloths was used as a measure of the amount amounts thereof are set forth below. In all of these of soil removed from the cloth. examples the compositions were clear homogeneous This test was applied to a simple system of organic liquids at room temperature.
TABLE V ltxampleNo -L --22 2a m 25 2a 27 2s 29 Potassium Dodecylbenaene Sulfua note m 10 10 10 6.1 15 10 1o Tetrapotasslum Pyroghosphatem..- 10 10- 2o 20 25.5 10 15 15. Lam'leDlethanolami e as as 2 1a 2.7 8.8 3.8 as Laurlclso ropanolamlde 8.2 8.2 -2.8 8.2 3.2 8.2 Sodium ylene Sultonate (Oommer s 4 6.5 0.5 7 a 7.5 7.6 Water-l- OHtopH12-.. 59 66.5 61.5 48.5 53.3 00 61.8 at Sodium Sflleate(Na 0: 8101 of 1:2.6) 2. 5 2. 6 Potassium Silicate (KsOzSlOr of detergents without a polyphosphate (Composition A), an aqueous solution of a polyphosphate (Composition B),
and a heavy duty liquid detergent composition of the invention (Composition C). The results of this test and the percent by weight of the componentsof these compositions are set forth below.
The tendency of polyphosphate detergents to corrode aluminum may be inhibited by the addition to the homogeneous heavy duty liquid detergent compositions of an amount up-to about 8% on a solids basis of a water- Examples 30-41 T o the following base formula there were added vary- 7 ing amounts of alkali metal aryl sulfonates as indicated below to form clear homogeneous heavy duty liquid detergent compositions which were still homogeneous after three or more months storage at room temperature Components: Percent by weight Potassium dodecylbenzene sulfonate ..v 10. Laurie diethanolamide 3.8.. Laurie isopropanolamide 3.2. Tetrapotassium pyrophosphate 20. Sodium silicate (Na OzsiOg of Alkali metal arylsulfonate As indicated below. Water-J-KOH to pH 12.2 Suflicient amount to make components total Total 100.
Example 30 contained 5.5 of sodium toluene sulfonate.
Example 31 contained 5.5% of sodium ethylbenzene sulfonate.
Example 32 contained 5.5% of sodium ortho-xylene sulon te.
Example 33 contained 7% of sodium isopropylbenzene sulfonate.
Example 34 contained 5.5% of sodium meta-xylene sulfonate.
Example 35 contained 7.5% of sodium tetralin sulfonate.
Example 36 contained 5.5% total of a mixture of 80% sodium toluene sulfonate and 20% sodium ethylbenzene sulfonate.
Example 37 contained 5.5% total of a mixture of 61% sodium ortho-xylcne sulfonate and 39% sodium isopropylbenzcnc sulfonate.
Example 38 contained 6% total of a mixture of 15% sodium ortho-xylcnc sulfonatc, 70% sodium metaxylene sulfonate, and 15% sodium para-xylene sulfonate.
Example 39 contained 6% total of a mixture of 47% sodium toluene sulfonate plus 53% of a mixture of 15% sodium ortho-xylene sulfonate, 70% sodium metaxylene sulfonatc, and 15% sodium para-xylene sulfonate.
Example 40 contained 7% total of a mixture of 22% sodium ortho-xylene sulfonate, 53% sodium metaxylene sulfonate, sodium para-xylene sulfonate, 18% sodium ethylbenzene sulfonate, and 2% sodium toluene sulfonate.
Example 41 contained 7% total of a mixture of sodium toluene sulfonate plus 90% of a mixture of 22% sodium ortho-xylene sulfonate, 53% sodium meta-xylene sulfonate, 5% sodium para-xylene sulfonate, 18% sodium ethyl'oenzene sulfonate, and 2% sodium toluene sulfonate.
This application is a continuation-in-part of applicants copcnding application Serial No. 580,712, filed April 26, 1956, now abandoned, which in turn is a continuationin-part of applicants application Serial No. 538,773, filed October 5, 1955, also now abandoned.
Various modifications and changes other than those set forth herein may be made in the composition of this invention without departing from the spirit thereof, and accordingly it will be understood that the invention is to be limited only within the scope of the appended claims.
I claim:
l. A homogeneous heavy duty liquid detergent composition consisting essentially of an aqueous solution of from about 7% to about 16% of a potassium alkylaryl sulfonate having the general formula where R is an alkyl group containing from 1 to carbon atoms, at least one R having 8 to 15 carbon atoms, and x is a number from 1 to 5; from about 4% to about 12% total of alkali metal arylsulfonate selected from the group consisting of toluene sulfonate, tetralin sulfonate, ethylbenzene sulfonate, isopropylbenzene sulfonate, or-
10 thoxylene sulfonate, meta-xylene sulfonate, a mixture of toluene sulfonate and 20% ethylbenzene sulfonate, a mixture of 61% ortho xylene sulfonate .and 39% isopropylbenzene sulfonate, a mixture of 15 ortho-xylene sulfonate, 70% meta-xylene sulfonate, and 15% paraxylene sulfonate, a mixture of 47% toluene sulfonate plus 53% of a mixture of 15% ortho-xylene sulfonate,
70% meta-xylene sulfonate, and 15% para-xylene sill-- fonate, a mixture of 22% ortho-xylene sulfonate, 53% meta-xylene sulfonate, 5% paraxylene sulfonate, 18% ethylbenzene sulfonate, and 2% toluene sulfonate, and a mixture of from about 1% to about 10% toluene sulfonate plus from about 99% to about of a mixture of 22% ortho-xylene sulfonate, 53% meta-xylene sulfonate, 5% para-xylene sulfonate, 18% ethylbenzene sulfonate, and 2% toluene sulfonate; from about 27% to about 10% of a potassium polyphosphate selected from the group consisting of tetrapotassium pyrophosphate and pentapotassium tripolyphosphate; and from about 2% to about 15% total of at least one compound selected from the group consisting of lauric isopropanolamide, lauric diethanolamide, coconut monoethanolamide, capric diethanolamide, tallow diethanolamide, the monoethanol amide of a 1:1 mixture of caprylic and capric acids, the
condensation product of one mole of lauric monoethanol- 3. A homogeneous heavy duty liquid detergent composition as set forth in claim 1 containing an amount up to about 8% on a solids basis of a water-soluble alkali metal silicate having an alkali to silica ratio of from 1:1.8 to 113.92, said composition having a pH of at least about 11.4; I
4. A homogeneous heavy duty liquid detergent composition as set forth in claim 1, wherein the amount of.
potassium alkylaryl sulfonate is about 10%, the total amount of alkali metal arylsulfonate is about 7%, the amount of potassium polyphosphate is about 20%,
and the total amount of the alkylolamide compounds is from about 4% to about 7%.
5. A homogeneous heavy duty liquid detergent composition as set forth in claim 3, wherein the silicateis a potassium silicate.
References Cited in the file of this patent UNITED STATES PATENTS Re. 23,840 Vitale June 15, 1954 2,581,677 Machlis Ian. 8, 1952 2,618,607 Sanders Nov. 18, 1952 2,741,599 McDonald Apr. 10, 1956 UNITED STATES PATENT OFFICE CERTIFICATE OF CORRECTION Patent No. 2,859,182 November 4, 1958 v I v Frank E. Carroll It is hereby certified that error appears in the printed specification of the above numbered patent requiring correction and that the said Letters Patent should read as corrected below.
Columns 5 and 6, Table II, Example 14, third item, for "6.5g" read I 6.5 same table, Example 16, lines 6 to 10 inclusive, insert leaders; Table III, Example l8, line :4, insert leaders; Table IV, Example 20, line 5, insert leaders, column '7, line 57, for "Pheny" read Phenyl Signed and sealed this 17th day of March 1959.
- (SEAL) Attest:
KARLH. AXL'INE Conmission'er bfpatents UNIl'ED STATES PATENT OFFICE 'CERTIFICATE OF CORRECTION Patent No. 2,859,182 November 4, 1958 Frank E. Carroll It is hereby certified that error app rs in the printed specification I of the above numbered -patent requiring correction and that the said letters Patent should read as corrected below.
Column 4, after line 75, and before TABLE II; in colmms 5 and 6, the following two paragraphs were inadvertently omitted and should be inserted as part oi the Letters Patent 1 The homogeneous heavy duty liquid detergent composition of this invention is prepared ,by mixing the components thereof together in the aqueous medium. Heat may be conveniently utilized during the mixing of the components to increase the rate of dissolution thereof.
Illustrative examples of the homogeneous heavy duty liquid detergent composition of this invention are presented below in Examples 7 through 1670i Table II. In this table the amount of the components in the com- 5 positions is expressed in percent by weight of the total I i; composition.
Signed and sealed this let day of Se tember 195% (SEAL) Attest:
KARL AXLINE p ROBERT c..'. WATSON: v Attesting- Officer Conmiasioner of Patents Y

Claims (1)

1. A HOMOGENEOUS HAVY DUTY LIQUID DETERGENT COMPOSITION CONSISTING ESSENTIALLY OF AN AQUEOUS SOLUTION OF FROM ABOUT 7% TO ABOUT 16% OF A POTASSIUM ALKYLARYL SULFONATE HAVING THE GENERAL FORMULA
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Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3021284A (en) * 1958-10-30 1962-02-13 Atlantic Refining Co Liquid detergent compositions
US3023168A (en) * 1958-11-25 1962-02-27 Atlantic Refining Co Heavy duty liquid detergent
US3037935A (en) * 1958-06-02 1962-06-05 Fmc Corp Clear high-foam liquid built detergent
US3066104A (en) * 1958-02-10 1962-11-27 Diamond Alkali Co Heavy duty liquid synthetic detergent composition
US3072578A (en) * 1958-06-02 1963-01-08 Fmc Corp Creamy high-foam liquid built detergent composition
US3150098A (en) * 1959-06-01 1964-09-22 Lever Brothers Ltd Liquid detergent
US3156655A (en) * 1960-08-02 1964-11-10 Lever Brothers Ltd Heavy duty liquid detergent composition
US3211660A (en) * 1961-02-03 1965-10-12 Colgate Palmolive Co Liquid detergent composition
US3234138A (en) * 1964-06-25 1966-02-08 Lever Brothers Ltd Clear, uniform liquid detergent composition
US3254028A (en) * 1961-02-06 1966-05-31 Colgate Palmolive Co Liquid detergent composition
US3265625A (en) * 1962-10-30 1966-08-09 C P Baker & Company Liquid detergent
US3272753A (en) * 1965-01-13 1966-09-13 Colgate Palmolive Co Detergent liquid
US3349038A (en) * 1962-04-24 1967-10-24 Stamford Chemical Ind Inc Detergent compositions
US3642506A (en) * 1969-11-28 1972-02-15 Swift & Co Method for improving the properties of hydraulic cementitious mixtures
US3856711A (en) * 1965-11-29 1974-12-24 Witco Chemical Corp Liquid detergent compositions
DE2855776A1 (en) * 1977-12-22 1979-06-28 Unilever Nv LIQUID DETERGENT
US4800037A (en) * 1987-06-05 1989-01-24 Lever Brothers Company Process for making a heavy duty liquid detergent composition
US5188769A (en) * 1992-03-26 1993-02-23 The Procter & Gamble Company Process for reducing the levels of fatty acid contaminants in polyhydroxy fatty acid amide surfactants

Citations (4)

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US2581677A (en) * 1952-01-08 Phosphate detergent composition in
US2618607A (en) * 1952-11-18 Liquid
USRE23840E (en) * 1950-05-03 1954-06-15 Liquid anionic-dialkylolamide
US2741599A (en) * 1952-04-28 1956-04-10 Kelite Corp Composition for cleaning and stripping paint from aluminum

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Publication number Priority date Publication date Assignee Title
US2581677A (en) * 1952-01-08 Phosphate detergent composition in
US2618607A (en) * 1952-11-18 Liquid
USRE23840E (en) * 1950-05-03 1954-06-15 Liquid anionic-dialkylolamide
US2741599A (en) * 1952-04-28 1956-04-10 Kelite Corp Composition for cleaning and stripping paint from aluminum

Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3066104A (en) * 1958-02-10 1962-11-27 Diamond Alkali Co Heavy duty liquid synthetic detergent composition
US3037935A (en) * 1958-06-02 1962-06-05 Fmc Corp Clear high-foam liquid built detergent
US3072578A (en) * 1958-06-02 1963-01-08 Fmc Corp Creamy high-foam liquid built detergent composition
US3021284A (en) * 1958-10-30 1962-02-13 Atlantic Refining Co Liquid detergent compositions
US3023168A (en) * 1958-11-25 1962-02-27 Atlantic Refining Co Heavy duty liquid detergent
US3150098A (en) * 1959-06-01 1964-09-22 Lever Brothers Ltd Liquid detergent
US3156655A (en) * 1960-08-02 1964-11-10 Lever Brothers Ltd Heavy duty liquid detergent composition
US3211660A (en) * 1961-02-03 1965-10-12 Colgate Palmolive Co Liquid detergent composition
US3254028A (en) * 1961-02-06 1966-05-31 Colgate Palmolive Co Liquid detergent composition
US3349038A (en) * 1962-04-24 1967-10-24 Stamford Chemical Ind Inc Detergent compositions
US3265625A (en) * 1962-10-30 1966-08-09 C P Baker & Company Liquid detergent
US3234138A (en) * 1964-06-25 1966-02-08 Lever Brothers Ltd Clear, uniform liquid detergent composition
US3272753A (en) * 1965-01-13 1966-09-13 Colgate Palmolive Co Detergent liquid
US3856711A (en) * 1965-11-29 1974-12-24 Witco Chemical Corp Liquid detergent compositions
US3642506A (en) * 1969-11-28 1972-02-15 Swift & Co Method for improving the properties of hydraulic cementitious mixtures
DE2855776A1 (en) * 1977-12-22 1979-06-28 Unilever Nv LIQUID DETERGENT
US4800037A (en) * 1987-06-05 1989-01-24 Lever Brothers Company Process for making a heavy duty liquid detergent composition
US5188769A (en) * 1992-03-26 1993-02-23 The Procter & Gamble Company Process for reducing the levels of fatty acid contaminants in polyhydroxy fatty acid amide surfactants

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