US2941948A - Detergent compositions - Google Patents

Detergent compositions Download PDF

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US2941948A
US2941948A US615827A US61582756A US2941948A US 2941948 A US2941948 A US 2941948A US 615827 A US615827 A US 615827A US 61582756 A US61582756 A US 61582756A US 2941948 A US2941948 A US 2941948A
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complex
detergent
sodium
sodium sulfate
sulfate
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US615827A
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Blinka Joseph
James E Henjum
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Procter and Gamble Co
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Procter and Gamble Co
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Priority to BE561238D priority Critical patent/BE561238A/xx
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Priority to US615827A priority patent/US2941948A/en
Priority to FR1187072D priority patent/FR1187072A/fr
Priority to GB32078/57A priority patent/GB823653A/en
Priority to DEP19486A priority patent/DE1102330B/de
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    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/04—Water-soluble compounds
    • C11D3/06—Phosphates, including polyphosphates
    • C11D3/062—Special methods concerning phosphates
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/0047—Detergents in the form of bars or tablets
    • C11D17/0065—Solid detergents containing builders
    • C11D17/0069—Laundry bars

Definitions

  • the present invention relates to mechanically worked compositions consisting largely or entirely of inorganic salts and organic synthetic sulfate and sulfonate detergents and to a method for making such compositions.
  • Sodium soaps and some of the organic sulfate and sulfonate detergent salts have a high degree of plasticity when'within suitable ranges of temperature and moisture content, as is well known, and therefore lend themselves admirably to the manufacture of milled soaps and other milled detergents.
  • Inorganic salts are devoid of plasticity and can be incorporated only to a limited extent in milled soaps and milled detergent compositions.
  • a milled detergent is to be made from a synthetic detergent which is itself low in plasticity, or'substantially devoid of plasticity, the amount of ordinary inorganic salt which can be tolerated is quite low. If, in any given case, the amount of unplasticizable inorganic salt is excessive, the composition will lack cohesiveness and toughness, will tend to crumble, will be dull in surface appearance, and undesirable in texture.
  • plastic inorganic salt combination greatly increases the range of formulations of satisfactory milled synthetic detergents. It is particularly advantageous in that it includes tripolyphosphates which are recognized as excellent detergency builders for synthetic depanics synthetic organic detergents as ordinarily made.
  • This invention is based on the discovery of heretofore unrecognized crystalline plasticizable inorganic complexes and, in particular, a crystalline sodium sulfatesodium tripolyphosphate complex which under certain conditions becomes plastic in nature.
  • the plasticity of these complexes makes possible the production of mechanically worked water soluble, anionic, synthetic organic, detergent compositions containing large amounts of inorganic builder.
  • One means of accomplishing the mechanical working of the detergent compositions of the present invention is the process of milling.
  • the plastic detergent composition is passed between a series of rotating rolls, successive members of the series rotating at higher speeds and at lower clearances, the detergent composition being thus subjected to mechanical working, shearing and compacting.
  • the action of the milling rolls can be supplemented by plodding and extruding, whereby the detergent composition is mechanically worked, with shearing and compacting, by being forced through one or more orifices of restricted size by the pressure of an Archimedean screw revolving within a closed barrel.
  • the X-ray diffraction pattern shown in the drawing can be characterized by the spacings of the strong diffraction lines at the following approximate values of the angle 20: 18.9", 22.8, 25.4", 3l.9, 33.2 and 46.7. These values of the angle 26 correspond respectively to the following values of interplanar spacing of: 4.69 A., 3.90 A., 3.50 A., 2.80 A., 2.70 A. and 1.94 A.
  • a crystalline plasticizable inorganic complex can be made by roll drying or spray drying aqueous solutions containing to 40% of dissolved Na SO and wherein x is a value in me range of from 4 to S, with the optimum ratio of Na SO to Na H .P O being initially about 7:3 by moles.
  • the complex has been made using the following tripolyphosphate salts:
  • the degree of co-crystallization of sodium sulfate and Na H P O is greatly influenced by drying rate.
  • drying rate When roll drying is employed, considerable amounts of complex are formed with a drying time of one minute.
  • the drying time is increased to 10 or minutes only moderate amounts of complex are formed.
  • a drying time of 22 minutes results in the formation of relatively minor amounts of complex, and no complex is formed when the drying time is increased to 40 minutes.
  • the drying time should not exceed about 5 minutes and preferably will not exceed about one minute.
  • the word drying is intended to mean the driving off of water until the inorganic constituents have substantially entirely crystallized from solution to form the complex.
  • the complex can be made by rapid precipitation of the salts from solution. Formation of the complex by this precipitation method, of interest mainly as a means of studying the complex, may be described as follows: A fresh aqueous solution containing 40% dissolved in a 7:3 molar ratio is poured suddenly into a 5 to fold larger volume of very hot ethylene glycol, so that the final mixture is at 230 F. or higher. The precipitate is formed very rapidly and can be filtered off so quickly that the inorganic ingredients need not be hot for more than 'a minute or two and excessive hydrolysis of the tripolyphosphate will not occur.
  • the complex can be further defined as being of a tripolyphosphate salt chosen from s a io i a m s s m, -i 3 10 and mixtures of any of these and of an inorganic sulfate salt chosen from Na SO and K 80
  • the sodium tripoly'phosphate-sodium sulfate inorganic builder will have the X-ray diffraction pattern set forth in the drawing. Although this pattern usually will be superimposed on other patterns, the presence of the complex may nevertheless be determined without difficulty by those skilled in the art.
  • a crutcher To a crutcher are added at least one water-soluble anionic synthetic sulfate or sulfonate detergent, sodium sulfate (taking into account any sodium sulfate which accompanies the anionic detergent by reason of a neutralization step), and a sodium salt of a tripolyphosphate or a mixture of tripolyphosphates having the following generalformula Na H P O wherein x is a value in the range of from 4 to 5. Water is then added to the crutcher mixture in an amount suflicient to put the inorganic constituents substantially entirely into solution,
  • the inorganic constituents, and particularly the tripolyphosphates, should be in solution. High moisture content of the paste minimizes the formation of suspended lization is essential for formation of the complex.
  • the crutcher mixture which is to be dried contains undissolved sodium sulfate or Na I-l P O the product obtained upon drying will contain in addition to.the Na P O -6H O, other undesirable crystal species such as Na S0 N21 P O and Na P O These suspended crystals have an adverse effect upon the subsequent mechanical working of the detergent compositions.
  • the mixture is generally heated, although this operation is not essential. We have employed temperatures in the range of from about 70 F.
  • the tripolyphosphates may hydrolyze to form pyrophosphate and orthophosphate, neither of which W111 combine with sodium sulfate to form a plasticizable complex.
  • the stock can be continuously fed to mechanical Working equipment or it can be stored and at a later time be mechanically worked. Continuous operation is preferable since frequently a large part of the amorphous acid impurities which are formed by hydrolysis of the tripolyphosphate crystallize out as a result of exposure of the product to the atmosphere (e.g. crystalline Na HP O -H O), without, however, afiecting the amount of complex present. There may also be an increase in the crystal size of the crystalline complex. In addition, if the stock is held at too high a water content for too long a period of time, the complex may dissociate with the formation of Na SO and tripolyphosphate hexahydrate.
  • the amount of Water initially present in the dried product which is to be mechanically worked will vary considerably depending upon the nature of the synthetic detergent which is used. As noted hereinbefore some synthetic detergents possess some degree of plasticity. As a general proposition, it may be stated that the greater the plasticity of the synthetic detergent, the lower is the percentage of water which the dried product need contain for optimum mechanical working efliciency. For example, if the active synthetic detergent consists of alkyl benzene sulfonate, which possesses a relatively high degree of placticity, the initial water level could be reduced to as low as about 2% by weight of total product. However, if the active synthetic detergent is relatively devoid of plasticity (e.g.
  • alkyl glyceryl ether sulfonate an initial water level as high as 12% by weight of total product may be necessary.
  • suitable water level range will vary depending upon the type of mechanical working equipment which is employed, the duration of mechanical working, and the temperature of 6 the product during mechanical working. Generally fllj dried product will contain initially from'about 6% to' about 10% by weight of water.
  • the final step in the manufacture of the milled flake which comprises a part of the present invention is the; mechanical working of the plastic stock. Assuming nopretreatment other than moisture and temperature adjustment, double milling is desirable to produce a well milled uniform flake.
  • One milling step may be omitted by plodding the stock prior to milling.
  • the surface temperatures of the first rolls be at about from 110 F. to 130 F.
  • the temperature on the first rolls can be as high as about 175 F. if there is sufiicient cooling on the last roll to prevent the cut flakes from deforming. Removing cut flakes from the mills requires a shift from the plasticsticky range to a non-plastic, or semi-plastic, non-sticky range.
  • the temperature of the last roll may have to be as low as 50 F. when the temperature of first rolls substantially exceeds 130 F.
  • Water soluble salts of sulfonic acids which exhibit detergent eifect such as the higher alkylated benzene sulfonic acids-(e.g. sodium salt of the sulfonic acid derived from the condensation product of benzene and a chlorinated kerosene fraction containing predominantly twelve carbon atoms per molecule, or the sodium salt of the sulfonic acid derived from the condensation product of benzene and polypropylenes having from 9 to 15 carbon atoms and averaging 12 carbon atoms) maybe employed in the practice of the invention.
  • water-soluble salts of higher mono fatty acid esters of 1,2-dihydroxypropane-B-sulfonic acid will find use in the practice 'of this invention.
  • water-soluble salts of higher fatty acid monoesters'of lower molecular weight hydroxy alkyl sulfoni'c acids e.g. oleic acid ester of the sodium salt of isethionic acid
  • water-soluble salts of thehigher fatty acid amides of lower molecular alkyl sulfonic acids e.g. ammonium salt of oleic acid amide of N-methyl taur-ine
  • mechanically worked detergent compositions containing large amounts of inorganic salts may be preparedfrom synthetic detergents such as the water-soluble salts of the higher alcohol esters of sulfocarboxylic acids. (e.g. sodium salt of the lauryl alcohol ester of sulfoaceticacid), ethers'of high molecularalcohols and lower hy-v droxy sulfonic acids (e.g. monolauryl ether of 1,2-dihydroxy propane-B-sodium sulfonate), and the water soluble alkyl glyceryl ether sulfonates in which the alkyl group contains from 10 to 1'8 carbot'n atoms (e.g. the sulfonated and neutralized reaction product obtained by reacting epichlorohydrin and coconut fatty alcohols containing from 10 to 18 carbon atoms).
  • synthetic detergents such as the water-soluble salts of the higher alcohol esters of sulfocarboxylic acids. (e
  • sodium alkyl sulfate obtained from the mixed higher alcohols produced by the reduction of coconut oil, palm kernel oil, or other oils of the coconut oil group a group of tropical nut oils characterized by their high content of combined fatty acids having from ten to fourteen carbon atoms) tallow or sperm oil.
  • watersoluble salts of sulfuric acid esters of higher fatty acid monoglycerides eg sodium salt of the coconut oil fatty acid monoester of 1,2-dihydroxy propane-3-sulfuric acid ester
  • the sulfated higher fatty acid alkylolamides e.g. sodium salt of sulfated coconut oil fatty acid ethanolamide
  • water-soluble salts of higher alkyl polyethylene oxide sulfuric acid esters e.g. the sulfated and neutralized reaction product of about three moles of ethylene oxide with one mole of the higher alcohols produced by the reduction of coconut oil fatty acids having 10 to 14 carbon atoms.
  • sulfate and sulfonate detergents may be used singly or in combination in the practice of the present invention.
  • the above examples are merely specific illustrations of the numerous detergents which can be incorporated into milled detergent compositions in the presence of large amounts of inorganic salts, and are not intended to be limitations.
  • the molar ratio of Na SO to Na H P O in the crutcher mix should be in the range of from about 2:1 to about 3: I.
  • the molar ratio of Na S to Na H P O in the mechanically worked product will generally not be the same as the molar ratio of the inorganic salts which were put into the crutcher mix, because of the loss of some of the tripolyphosphate by hydrolysis.
  • the experimental work which has been completed indicates that the molar ratio of sodium sulfate to tripolyphosphate in the complex is about 3:1. If a 3:1 ratio is added to the crutcher, there will usually be some free sodium sulfate in the final product, assuming some loss of tripolyphosphate by hydrolysis.
  • the mechanically worked detergent compositions of the present invention contain from about 10% to about by weight, based on total product, of active synthetic detergent and from about 30% to about 70% by weight, based on total product, of sodium sulfate and Na H P O
  • these compositions will contain from about 15% to about 30% by weight of detergent, based on total product, and from about 40% to about by weight of sodium sulfate and Na H P O based on total product.
  • the ratio of sodium sulfate to Na H P O in the final product will usually range from about 2:1 to 4:1.
  • a preponderance of the sodium sulfate and Na H P O should be inthe form of a complex having the X-ray diifraction pattern' shown in the drawing.
  • substantially all of the sodium sulfate and tripolyphosphate in the composition will have combined to form the complex in the 3:1 molar ratio of sodium sulfate to Na H P O as demonstrated by an X-ray diifraction analysis showing only complex and no uncombined sodium sulfate and tripolyphosphate.
  • the complex can be prepared in pure form, i.e. free of all other material either crystalline or non-crystalline for making X-ray calibration curves and its composition proved constant, the amount of complex present in any given detergent composition cannot be determined by direct analysis for complex.
  • the procedure which can be used for measuring the amounts of Na SO V present in a given preparation can be adapted from the one set forth by Klug and Alexander (op. cit.) beginning at p. 422.
  • an internal standard is mixed with Na SO V, in a fixed proportion.
  • Magnesium oxide has proved to be a satisfactory internal standard for use in quantitative determination of the free Na SO V in a preparation which contained tripolyphosphate, and the diffraction line at a spacing of 2.11 A. (429 26) produced by the magnesium oxide was selected for measuring the intensity ratio of Na S0 V to the internal standard.
  • the amount of Na SO V present in a preparation is.
  • auxiliary materials in synthetic detergent compositions.
  • the detergent compositions of the present invention may include any of these substances employed by the art in admixture with such detergent compositions generally, provided that the use of any such materials does not adversely affect the plastic properties of the mix during the mechanical working step.
  • These auxiliary materials may be inorganic or organic in structure and may be mixed with the active detergent,
  • phosphates e.g. metaphosphate, pyrophosph'ate, orthophosphate
  • Suitable organic materials may be added, such as glycerol, carboxymethylcellulose, organic suds builders (such as coconut ethanolamide, i.e. the monoethanol amide of coconut oil fatty acids), tarnish inhibitors, fluorescent brightening agents, perfumes, coloring matter etc.
  • the addition of soap to the synthetic detergent compositions is not essential to provide these compositions with the plasticity necessary for mechanical working.
  • the inorganic complex by itself provides sufflcient plasticity. However, it may be desirable that soap be present in the synthetic detergent compositions of this invention as a supplemental and less expensive washing agent and as a low temperature sudsing agent.
  • compositions made according to this invention are truly remarkable, even after extended periods of time. It would normally be expected that detergent flakes containing up to 60% of inorganic salts would, after a period of time, crack, crumble, acquire a hard crystalline feel, and lose whatever coherent properties they might have originally possessed. However, the detergent flake compositions of this invention after ageing for up to two years still retain their original form, waxy feel, and glossy appearance. Furthermore, the brittleness of these flakes is about equal to that of substantially pure mechanically worked soap flakes stored under similar conditions for the same period of time.
  • Example I 'A detergent composition is prepared by crutching at 170 F. about a 40% solids water solution containing on a solids basis, about 30% pentasodium tripolyphosphate, 33.5% sodium sulfate, 6% sodium silicate (SiO /Na O, 1.6), 1.6% sodium chloride, alkyl glyceryl ether sulfonate (the sulfonated and neutralized product obtained by reacting epichlorohydrin and coconut fatty alcohols containing 10 to 14 carbon atoms), 10% tallow alkyl sulfate (the sodium alkyl sulfate obtained from the mixed higher alcohols produced by the reduction of tallow), 4% coconut ethanolamide (the monoethanolamide of coconut oil fatty acids), 4% of the sodium soap derived from castor oil, and 0.4% glycerol.
  • alkyl glyceryl ether sulfonate the sulfonated and neutralized product obtained by reacting epichlorohydr
  • the solution is roll dried for five minutes using steam pressure of 25 pounds per square inch, gage.
  • the resulting composition which contains about 8% water by weight, is adjusted in temperature to 130 F. and extruded through a pellet-forming plodder.
  • the extruded stock is then put through a three roll milling device with the surface temperature of the first rolls being 120 F. and the surface temperature of the final roll being 75 F.
  • the cooled non-plastic, non-sticky sheets are then cut into ribbons and these ribbons into flakes as they are removed from the rolls.
  • the milled detergent composition coming from the final roll may be fed to a plodder, extruded in continuous bar form, cut into individual cakes, stamped (or pressed) into desired shape and pattern and the cakes wrapped and packed; orthe milling may be omitted altogether and the bar formed by simply extruding the crutcher mix in bar form.
  • Example II A detergent composition is prepared by crutching at 180 F. about a 30% solids water solution containing on a solids basis about 35% pentasodium tripolyphosphate, 31% sodium sulfate, 14% alkyl glyceryl ether sulfonate (the sulfonated and neutralized reaction product obtained by reacting epichlorophydrin and coconut fatty alcohols containing 10 to carbon atoms), 14% tallow alkyl sulfate (the sodium alkyl sulfate obtained front the mixed higher alcohols produced by the reduction of tallow), and 6% of the sodium soap derived from castor oil.
  • the crutcher mixture is then spray dried to a moisture level of about 5% by weight of the product, the
  • exit air temperature being 250 F.
  • the moisture level of the spray dried product is then adjusted to 7% by weight of the product, and the temperature is adjusted to F.
  • This product is then put through a three roll mill with the surface temperature of the first rolls being 110 F. and the surface temperature of the final roll being 75 F. This milling operation is then repeated under the same temperature conditions.
  • the cooled nonplastic, non-sticky sheets are then cut into ribbons and these out into flakes and the flakes removed from the rolls.
  • Example 111 Percent Sodium coconut alkyl sulfate (the sulfated and neutralized product obtained from the mixed higher alcohols produced by the reduction of coconut oil fatty acids having 10 to 14 carbon atoms) l-5 Alkyl benzene sulfonate (the sodium salt of the sulfonic acid derived from the condensation product of benzene and polypropylenes having from 9 to 15 carbon atoms and averaging 12 carbon atoms) 20 Na HP O 23 Sodium sulfate 20 coconut ethanolamide (same as in Example I) 4 Sodium silicate 6 Sodium chloride -,4 Water 8
  • Example IV Percent Alkyl glyceryl ether sulfonate (the sulfonated and neutralized reaction product obtained by reacting epichlorohydrin and coconut fatty alcohols conv taining 10 to 14 carbon atom
  • a is a value in the range of from 4 to 5, and at least one water-soluble anionic synthetic organic detergent salt selected from the group consisting of anionic sulfate and sulfonate synthetic detergents, the steps which comprise: (1) blending a mixture of water, from about 10% to about 50% by weight of total solids of said synthetic detergent salt, and from about 30% to about 70% by weight of total solids of said sodium sulfate and Na H P O the molar ratio of sodium sulfate to Na H P O being from about 2:1 to about 3:1 and the Water content beingsuch that the inorganic constituents are substantially entirely in solution, (2) drying the mixture until said inorganic constituents have substantially entirely crystallized from solution and over a period of time not exceeding about five minutes, thereby promoting co-crystallization of the sodium sulfate and Na H P O to form a complex having an X-ray diffraction pattern corresponding to that shown in the drawing characterized by strong diffraction line values of the angle 20 of 18.9, 228, 25
  • step 3 The process of claim 1 in which the molar ratio of sodium sulfate to Na H P O in step 1 is from about 2:1 to about 3:1 and the water level in step 3 is from about 6% to about by weight of total product.
  • steps which comprise: (1) blending a mixture of from about 15% to about by weight of total solids of said synthetic detergent salts, from about 40% to about 60%.
  • a coherent mechanically worked synthetic detergent composition comprising essentially from about 10% to about 50% of at least one detergent salt selected from the group consisting of water soluble synthetic organic sulfate and sulfonate detergents and from about 30% to about 70% of inorganic salts consisting of Na SO and molar ratio range of 2:1 to 4:1, with a preponderance of V the inorganic salts being in the form of a complex having complex having a molar ratio of said inorganic sulfate to phosphate salts of about 3:1, and the above percentages being by weight of the total product, said values of the angle 20 corresponding respectively to values of interplanar spacing d of 4.69 A., 3.90 A., 3.50 A., 2.80 A., 2.70 A. and 1.94 A.
  • a coherent mechanically worked synthetic detergent composition comprising essentially from about 10% to about 50% of at least one detergent salt selected from the group consisting of water soluble synthetic organic sulfate and sulfonate detergents and from about 30% to about 70% of inorganic salts consisting of Na SO and Na H P O wherein x is avalue in the range of from 4 to 5, within a molar ratio range of 2:1 to 4: 1, the sum of the said detergent salt and inorganic salts being at least 60% of the total product and a preponderance of the inorganic salts being in the form of a complex which exhibits an X-ray diffraction pattern characterized by strong diffraction line values of the angle 20 of 18.9", 22.8, 25.4, 31.9", 332 and 46.7 as shown in the drawing, said complex having a molar ratio of said inorganic sulfate to phosphate salts of about 3:1, the above percentages being by weight of total product, said values of the angle 20 corresponding respectively to values of interplanar spacing
  • a coherent mechanically worked synthetic detergent composition comprising essentially from about 15% to about 30% of at least one detergent salt selected from the group consisting of water soluble synthetic organic sulfate and sulfonate detergents and from about 40% to about 60% of inorganic salts consisting of Na SO and Na H P O wherein x is a value in the range of from 4 to 5, in a molar ratio of about 3:1, substantally all of said inorganic salts being in the form of a complex having salt comprises approximately equal parts by weight of the sulfated and neutralized fatty alcohols produced by the reduction of tallow and alkyl glyceryl ether sulfonate wherein the alkyl group contains from 10 to 18 carbon atoms.
  • a coherent mechanically worked synthetic detergent composition from ingredients comprising essentially, water,. an inorganic sulfate salt selected from the group consisting of Na SO and K 50 an inorganic tripolyphosphate salt selected from the group consisting of Na P O Na HP O K P O K HP O and mixtures of any of these, and at least one water-soluble anionic synthetic organic detergent salt selected from the group consisting of anionic sulfate and sulfonate synthetic detergents, the steps which comprise: 1) blending a mixture of water, from about 10% to about 50% by weight of total solids of said synthetic detergent salt, and from about 30% to about 70% by weight of total solids of said sulfate salt and said tripolyphosphate' salt, the molar ratio of sulfate salt to tripolyphosphate salt being from about 2:1 to about 3:1 andthe water content being such that the inorganic constituents are substantially entirely in solution, (2) drying the mixture until said inorganic constituents have substantially entirely crystallized from solution and over a period of

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US615827A 1956-10-15 1956-10-15 Detergent compositions Expired - Lifetime US2941948A (en)

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Application Number Priority Date Filing Date Title
BE561238D BE561238A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) 1956-10-15
US615827A US2941948A (en) 1956-10-15 1956-10-15 Detergent compositions
FR1187072D FR1187072A (fr) 1956-10-15 1957-10-02 Produit détersif travaillable mécaniquement
GB32078/57A GB823653A (en) 1956-10-15 1957-10-14 Improvements in and relating to detergent compositions and salts used therein
DEP19486A DE1102330B (de) 1956-10-15 1957-10-15 Pilierte, synthetische Wasch- und Reinigungsmittel

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3337468A (en) * 1966-02-17 1967-08-22 Monsanto Co Alkali metal tripolyphosphate products
US3639286A (en) * 1968-05-28 1972-02-01 Mario Ballestra Synthetic detergent in bar or cake form and the method to manufacture same
US4454293A (en) * 1981-11-20 1984-06-12 Phillips Petroleum Company Polymerization using partially hydrolyzed silicate treatment of catalyst support
US4543204A (en) * 1983-08-17 1985-09-24 Colgate-Palmolive Company Sodium higher fatty alkyl sulfate detergent laundry bars and process for manufacture thereof
US4806273A (en) * 1986-03-06 1989-02-21 Colgate-Palmolive Company Breakage resistant higher fatty alcohol sulfate detergent laundry bars
EP0328880A1 (en) * 1988-01-19 1989-08-23 Colgate-Palmolive Company Built synthetic organic detergent composition extrudate in particulate and patty forms, and processes for manufacture and uses thereof
US5089174A (en) * 1989-01-19 1992-02-18 The Procter & Gamble Company Laundry detergent bars free of C12 -C18 fatty acids and containing an alkylbenzene sulfonate, an alkyl sulfonate and a fatty alcohol
US5571287A (en) * 1993-01-11 1996-11-05 Colgate-Palmolive Company Soap composition containing sodium pyrophosphate

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DE4104664A1 (de) * 1991-02-15 1992-08-20 Sebapharma Gmbh & Co Feste, im wesentlichen trockene waschstuecke zur hautreinigung
RU2390846C2 (ru) 2004-08-04 2010-05-27 НКсП Б.В. Система пассажирских перевозок и способ получения билетов в такой системе
WO2010122050A2 (en) 2009-04-24 2010-10-28 Unilever Plc Manufacture of high active detergent particles

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US2618604A (en) * 1949-11-25 1952-11-18 Procter & Gamble Polyphosphate-containing detergent compositions having decreased corrosivity toward aluminum
US2620511A (en) * 1950-07-15 1952-12-09 Micro Proc Equipment Inc Method and apparatus for cold milling soap and other materials

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3337468A (en) * 1966-02-17 1967-08-22 Monsanto Co Alkali metal tripolyphosphate products
US3639286A (en) * 1968-05-28 1972-02-01 Mario Ballestra Synthetic detergent in bar or cake form and the method to manufacture same
US4454293A (en) * 1981-11-20 1984-06-12 Phillips Petroleum Company Polymerization using partially hydrolyzed silicate treatment of catalyst support
US4543204A (en) * 1983-08-17 1985-09-24 Colgate-Palmolive Company Sodium higher fatty alkyl sulfate detergent laundry bars and process for manufacture thereof
US4806273A (en) * 1986-03-06 1989-02-21 Colgate-Palmolive Company Breakage resistant higher fatty alcohol sulfate detergent laundry bars
EP0328880A1 (en) * 1988-01-19 1989-08-23 Colgate-Palmolive Company Built synthetic organic detergent composition extrudate in particulate and patty forms, and processes for manufacture and uses thereof
AU630596B2 (en) * 1988-01-19 1992-11-05 Colgate-Palmolive Company, The Built synthetic organic detergent composition extrudate in particulate and patty forms, and processes for manufacture and uses thereof
US5089174A (en) * 1989-01-19 1992-02-18 The Procter & Gamble Company Laundry detergent bars free of C12 -C18 fatty acids and containing an alkylbenzene sulfonate, an alkyl sulfonate and a fatty alcohol
US5571287A (en) * 1993-01-11 1996-11-05 Colgate-Palmolive Company Soap composition containing sodium pyrophosphate

Also Published As

Publication number Publication date
FR1187072A (fr) 1959-09-07
GB823653A (en) 1959-11-18
BE561238A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
DE1102330B (de) 1961-03-16

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