US2952638A - Deaeration and purification of anionic detergent compositions - Google Patents

Deaeration and purification of anionic detergent compositions Download PDF

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Publication number
US2952638A
US2952638A US602046A US60204656A US2952638A US 2952638 A US2952638 A US 2952638A US 602046 A US602046 A US 602046A US 60204656 A US60204656 A US 60204656A US 2952638 A US2952638 A US 2952638A
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slurry
detergent
carbon atoms
water
alkyl
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US602046A
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Robert P Davis
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Procter and Gamble Co
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Procter and Gamble Co
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Priority to GB24298/57A priority patent/GB812249A/en
Priority to FR744794A priority patent/FR1279205A/fr
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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
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C11D11/02—Preparation in the form of powder by spray drying

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  • This invention relates to detergent compositions, and more particularly to a chemical process for deaerating detergent composition slurries from which a high density spray dried detergent composition can be produced.
  • nonionic polyether detergents to slurries containing sulfate and sulfonate anionic synthetic organic detergents and inorganic salts such as sodium sulfate and water-soluble alkali metal silicates effect a material and rapid reduction in the amount of entrained air in the slurry when the slurry is agitated, and that these chemically deacrated detergent slurries can be spray dried by conventional techniques to form a granular product having a desirable high product density.
  • the present invention is based on the observation that the nonionic component (nonionic compound or mixture of nonionic compounds) causes a separation of slurry, which contains sulfate and/or sullonate anionic synthetic organic detergents, and inorganic salts such as sodium sulfate and water-soluble alkali metal silicates, into two distinct phases, viz. a low viscosity continuous lye phase which contains the inorganic materials and a discontinuous sopc phase which contains the organic constituents of the slurry.
  • the word sope is used herein to designate one or more synthetic organic detergents.
  • the degree of agitation necessary for deaeration can be obtained in mixing vessels of the types which are usually employed for mixing moderately viscous liquids.
  • a bafllcd mixing vessel having a diameter of 30 inches and depth of 27 inches and equipped with a 15 inch turbine type agitator running at from 200 to 600 revolutions per minute has been found to be satisfactory for deaeration of a 400 pound detergent composition slurry.
  • the moderate degree of agitation provided by this mixing vessel is sufiicient to cause dispersal of the discontinuous sope phase but not so drastic as to pull air into the slurry.
  • a mixing vessel of this construction was employed in Examples I, I], and III, which follow.
  • FIG 2 is a photomicrograph of an anionic sulfonate detergent paste which is commonly used in the preparation of detergent compositions. Air bubbles are visibly dispersed throughout and entrapped within the homo geneous paste. in the normal spray drying operation these bubbles would tend to cause the formation of a low bulk density granular product.
  • the addition of silicate starts to break the tight emulsion as shown by the lines of lye phase in Figure 3, but very little air is released from the emulsion at this point.
  • the addition of nonionic detergent grains out the slurry and results in the formation of a continuous lye phase and a discontinuous sope phase (Figure 1). At this point the slurry actually appears to be boiling.
  • the air removal is usually not instantaneous and generally about 1 to 5 minutes of moderate agitation of the mixture are allotted for it to take place.
  • Detergent composition slurries such as set forth in Example I, which follows, normally have a density of about 0.9 to 1.1 and such slurries can be spray dried to form granules which have a bulk density on the order of about 0.29 to 0.35.
  • a completely dcaerated slurry such as this will have a density of about 1.35.
  • the chemical deaeration resulting from the addition of silicate and nonionic detergent to a detergent slurry having a density of about 0.9 to 1.1 increases the density of the slurry to about 1.25 to 1.3 and this increased density slurry can be spray dried by conventional techniques to form granules having a bulk density of about 0.41 to 0.44.
  • Detergent composition slurries such as set forth in Example I, which have been built with about 18 parts of sodium tripolyphosphate, have a density comparable to that of unbuilt slurries, i.e. about 0.9 to 1.1. Such slurries can be spray dried to a bulk density of about 0.31 to 0.39. However, when the slurry is chemically deacrated and the tripolyphosphate is subsequently incorporated therein with a minimum of agitation, a spray dried product having a maximum bulk density of from about 0.49 to 0.51 can be obtained.
  • heavy duty detergent compositions will result from the combination of synthetic anionic sulfate and sulfonate detergents and from about 1 to about 5 parts of alkali metal tripolyphosphate, for example, those described in Byerly, U.S.P. 2,486,921 and Strain U.S.P. 2,486,922. It is often desirable to incorporate into such heavy duty detergent compositions a material which will inhibit the corrosion of aluminum, and water-soluble alkali metal silicates are among the most satisfactory of the known aluminum corrosion inhibitors. It is therefore apparent that the processes of the present invention are particularly well adapted to the manufacture of heavy duty detergent compositions.
  • tripolyphosphate is advantageously added to the slurry subsequent to the addition of the nonionic detergent and after deaeration has occurred.
  • a part of the tripolyphosphate may be mechanically mixed in with the spray dried product obtained from a deaerated slurry; detergent compositions having very high bulk densities, e.g. over 0.6, can be obtained by this technique.
  • the nonionic compounds which effect the phase change essential for chemical deaeration of an agitated slurry containing anionic sulfate or sulfonate synthetic detergents and inorganic salts according to the present invention, may be broadly defined as compounds produced by the condensation of alkylene oxide groups (hydrophilic in nature) with an organic hydrophobic compound, which may be aliphatic or alkyl aromatic in nature.
  • alkylene oxide groups hydrophilic in nature
  • organic hydrophobic compound which may be aliphatic or alkyl aromatic in nature.
  • Pluronic a well known class of nonionics is made available on the market under the trade name of Pluronic. These compounds are formed by condensing ethylene oxide with a hydrophobic base formed by the condensation of propylene oxide with propylene glycol.
  • the hydrophobic portion of the molecule exhibits water insolubility. Its molecular Weight is of the order of 1500 to 1800.
  • the addition of polyoxyethylene radicals to this hydrophobic portion tends to increase the water solubility of the molecule as a whole. Liquid products are obtained up to the point where polyethylene content is about 50% of the total weight of the com densation product. Further increase in the relative content of polyoxycthylene to hydrophobic portion renders the final product wax-like or solid in consistency.
  • the molecular weights of Pluronic L61, L64, and F68, which find particular utility in the practice of the present invention are approximately 2000, 3000, and 8000 respectively.
  • Suitable nonionics also include the polyethylene oxide condensates of alkyl phenols. These include the condensation products of alkyl phenols having about 6 to about 12 carbon atoms, either straight chain or branch chain, in the alkyl group with ethylene oxide in amount equal to approximately to approximately 30 moles of ethylene oxide per mole of alkyl phenol.
  • the alkyl substituent in such compounds may be derived from polymerized propylene, di-isobutylene, octane, or nonane, for example.
  • Igepal CO-730 and Igepal CO-SSO which are understood to be nonyl phenol polyethylene oxide condensates having respectively, on the average, 15 and 30 moles of ethylene oxide per mole of nonyl phenol.
  • nonionics may be derived by the condensation of ethylene oxide with the product resulting from the reaction of propylene oxide and ethylene diamine.
  • a series of compounds may be produccd, depending on the desired balance between hydrophobic and hydrophilic elements.
  • compounds molecular weight from about 5000 to about 11,000
  • a hydrophobic base constituted of the reaction products of ethylene diamine and excess propylene oxide, said base having a molecular weight of the order of 2500 to 3000
  • This class of compounds is made commercially available under the trade name of Tetronics.
  • nonionics include the condensation products of aliphatic alcohols having from about 8 to about 18 carbon atoms, either straight chain or branch chain, with ethylene oxide in amount equal to approximately 10 to approximately 30 moles of ethylene oxide per mole of alcohol.
  • the alcohols may be derived from the higher alcohols produced by the reduction of tallow or coconut oil, for example.
  • a coconut alcohol ethylene oxide condensate having approximately 15 moles of ethylene oxide per mole of coconut alcohol and an average molecular weight of about 800 has been found to be particularly satisfactory.
  • the products which find use in the present invention have an overall molecular weight within the range of about 800 to about 11,000.
  • the preferred nonionics employed in the practice of the present invention are those which possess a hydrophilic polyoxyethylene radical in combination with a hydrophobic base consisting of the reaction product of an excess of propylene oxide and ethylene diamine.
  • the anioinic synthetic to which reference is made and which is a constituent of the dense heavy duty or unbuilt detergent granules which can be produced by the practice of the present invention, is generally referred to as a water-soluble salt of an organic sulfuric reaction product having in its molecular structure an alkyl radical having from about 8 to about 22 carbon atoms and a radical selected from the group consisting of sulfonic acid and sulfuric acid ester radicals.
  • Important examples of the anionic synthetics which form an active part in the chemical deaeration techniques of the present invention are the sodium or potassium alkyl benzene sulfonates, especially those of the types described in U.S.P.
  • alkyl groups contain from about 9 to 15 carbon atoms; sodium alkyl glyceryl ether sulfonates, especially those others of higher alcohols from tallow and coconut oil; sodium coconut oil fatty acid monoglyceride sulfates and sulfonates; sodium salts of sulfuric acid esters of the reaction product of one mole of a higher fatty alcohol (e.g. tallow or coconut oil alcohols) and about 3 moles of ethylene oxide; sodium alkyl sulfates obtained from the mixed higher alcohols produced by the reduction of coconut oil or tallow; and others known in the art, a number being specifically set forth in the Byerly and Strain patents.
  • sodium alkyl glyceryl ether sulfonates especially those others of higher alcohols from tallow and coconut oil
  • sodium coconut oil fatty acid monoglyceride sulfates and sulfonates sodium salts of sulfuric acid esters of the reaction product of one mole of a higher fatty
  • miscellaneous ingredients including coloring agents, fluorescent dyes, perfumes, carboxymethylcellulose, sodium carbonate and other alkaline salts, and other materials well known as constituents in detergent compositions can be present.
  • detergent composition slurries which can be deaerated according to this invention contain from about 40% to 60% of Water, from about 10% to 40% of anionic detergent, from about 5% to 25% of sodium sulfate, the weight ratio of sodium sulfate to anionic detergent being from about 1:7 to about 1:1, from about 5% to 15% of sodium silicate solids, and from about 1% to 4% of the nonionic compound.
  • the detergent composition slurry contained from 40% to 60% of water, from 15% to 20% of anionic detergent, from 15% to 20% of sodium sulfate, the weight ratio of sodium sulfate to anionic detergent being about 1:1, from 6% to 12% of sodium silicate and about 2% of the nonionic compounds. These percentages are also by weight, based on the slurry.
  • any of. the commercially available sodium silicate solutions having an Si0 /Na O ratio of from about 1:1 to about 3:1 is suitable for use in the practice of this invention, the preferred SiO /Na O ratio range is 1.511 to 20:1.
  • Example I A slurry was formed in the following manner. To a paste consisting of 73.6 parts of a mixture of 23.5% sodium alkyl benzene sulfonate (the alkyl radical averaging about 12 carbon atoms and being derived from polypropylene) 56% water, 20% of sodium sulfate and 0.5% of miscellaneous ingredients, including carboxyrnethylcellulose, a tarnish inhibitor, and a fluorescent brightening agent, were added in succession 24.2 parts of sodium silicate (having a solids content of 45% and a ratio of SiO /Na O of 2:1) and 2.2 parts of Pluronic F68 (the condensation product of ethylene oxide with a polyoxypropylene base having a molecular Weight of about 1500 to about 1800, the condensation product having a molecular weight of about 8000).
  • sodium silicate having a solids content of 45% and a ratio of SiO /Na O of 2:1
  • Pluronic F68 the condensation product of ethylene oxide
  • This slurry was mixed with moderate agitation at a temperature of 160 F., for about 3 minutes, during which time it was readily apparent both from the visible turbulence and the decrease in volume of the slurry that a considerable volume of air was being evolved.
  • Slurries such as this prior to deaeration, have a density on the Order of about 0.9 to about 1.1 and will spray dry to give a product having a bulk density of from about 0.29 to 0.35. After completion of dcaeration, at which time the density will have increased to as high as about 1.25 to 1.30, these slurries can be spray dried to give a product having a bulk density of about 0.41 to about 0.44.
  • Example II Following the procedure of Example I comparable results were obtained by substitution of the Pluronic F68 with an alkyl ethylene oxide condensate wherein the alkyl radical was derived from alcohols produced by the reduction of coconut oil fatty acids having from to 14 carbon atoms, said condensate having an average molecular weight of about 800.
  • Example II To a paste consisting of 40 parts of a mixture of 10% sodium alkyl benzene sulfonate (the alkyl radical averaging about 12 carbon atoms and being derived from polypropylene), 12% of sodium alkyl sulfate (the alkyl groups being derived from higher alcohols produced by the reduction of tallow), 55% Water, 22.5% of sodium sulfate and 0.5% of miscellaneous ingredients including carboxymethylcellulose, a tarnish inhibitor, and a fluorescent brightening agent, is added in succession 16 parts of sodium silicate (having a solids content of 45% and a ratio of SiO :Na O of 2:1), and 2 parts of Tetronic 707 (a commercially available nonionic condensation product understood to have a molecular weight of about 11,000,
  • the slurry thus formed is dcacrated with moderate agitation at a temperature of F. for about 2 minutes. Upon spray drying this slurry will produce granules having a bulk density of about 0.41 to 0.44.
  • Example III This example includes a comparison of otherwise comparable deaerated and undeaerated detergent composition slurries and demonstrates the elfect which chemical deaeration has on the bulk density of a spray dried built detergent composition.
  • Hyfac 431 a commercial fatty acid mixture derived from bydrogenated marine oil and reported to contain 8% myristic, 29% palmitic, 18% stearic, 26% arachidic, 17% behenic, and 2% oleic acids
  • the density became 0.97.
  • 21 parts of sodium sulfate and 56 parts of sodium tripolyphosphate the density changed to 0.99.
  • alkyl benzene sulfonatc type synthetic detergents having from 9 to 15 carbon atoms, averaging about 12 carbon atoms, in the alkyl radical, or such alkyl benzene sulfonate detergents in admixture with alkyl sulfates of the type derived from the sulfation of higher alcohols produced by the reduction of tallow; other sulfate or sulfonate synthetic detergents well known in the art can be substituted therefor with good results, alone or in admixture, in these examples.
  • sope and lye phases can be separated from each other, as by centrifugatio-n, to yield a lye phase consisting of water and a greater part of the electrolyte originally present in the slurry and a sope phase rich in anionic detergent and low in electrolyte.
  • a high density spray dried detergent composition from a homogeneous fluid slurry initially containing entrained air, and containing from about 40% to 60% of water, from about 10% to 40% of at least one water-soluble alkali metal salt of an anionic organic sulfuric reaction product having in its molecular structure an alkyl radical having from 8 to 22 carbon atoms and a radical selected from the group consisting of sulfonic acid and sulfuric acid ester radicals, the said salt having pronounced detergent power in aqueous solution, and from about to 25% of sodium sulfate, the weight ratio of sodium sulfate to said anionic product being fro-m 1:7 to 1:1, and from about 5% to 15% of sodium silicate having an SiO :Na O ratio of from about 1:1 to about 3:1, the steps of (1) causing the homogeneous slurry to separate into a continuous lye phase which contains the inorganic materials of the slurry and a discontinuous phase which contains the organic constituents of the slurry by adding
  • nonionic detergent is a nonyl phenol po-lyoxyethylene ether having on the average from about 15 to about 30 moles of ethylene oxide per mole of nonyl phenol.
  • nonionic detergent is a polyoxyethylene condensation product with a polyoxypropylene base, said polyoxypropylene base having a molecular weight from about 1500 to about 1800 and the said condensation product having an overall molecular weight from about 2000 to about 8000.
  • nonionic detergent is a polyoxy-ethylene condensation product with a hydrophobic base constituted of the reaction product of ethylene diamine and propylene oxide, said base having a molecular weight of from about 2500 to about 3000 and said nonionic compound having an overall molecular weight of from about 5000 to about 11,000.
  • nonionic detergent is a polyoxyethylene condensation product with the higher alcohols produced by the reduction of coconut oil and said nonionic compound has an average molecular weight of about 800.
  • nonionic detergent is a polyoxyethylene condensation product with a hydrophobic base constituted of the reaction product ,Of ethylene diamine and propylene oxide, said base having a molecular weight of about 3000 and said nonionic compound having an overall weight of about 11,000.

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  • Oil, Petroleum & Natural Gas (AREA)
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US602046A 1956-08-03 1956-08-03 Deaeration and purification of anionic detergent compositions Expired - Lifetime US2952638A (en)

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BE559413D BE559413A (en(2012)) 1956-08-03
US602046A US2952638A (en) 1956-08-03 1956-08-03 Deaeration and purification of anionic detergent compositions
GB24298/57A GB812249A (en) 1956-08-03 1957-07-31 Improvements in or relating to detergent compositions
FR744794A FR1279205A (fr) 1956-08-03 1957-08-02 Procédé pour la préparation d'une composition détersive à forte densité séchée par pulvérisation

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3177147A (en) * 1960-09-23 1965-04-06 Colgate Palmolive Co Detergent compositions and preparation thereof
US3242091A (en) * 1961-12-19 1966-03-22 Colgate Palmolive Co Spray dried detergent concentrate
US3248330A (en) * 1963-05-24 1966-04-26 Monsanto Co Process for preparing a stable, freeflowing dishwashing composition

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2213477A (en) * 1935-12-12 1940-09-03 Gen Aniline & Film Corp Glycol and polyglycol ethers of isocyclic hydroxyl compounds
US2515577A (en) * 1950-07-18 Noncaking alkaryl sulfonate
US2606156A (en) * 1950-06-09 1952-08-05 Purex Corp Ltd Deaeration and drying of watersoluble sulfonated detergent compositions
US2742436A (en) * 1956-04-17 Preparation of non-dusting organic

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2515577A (en) * 1950-07-18 Noncaking alkaryl sulfonate
US2742436A (en) * 1956-04-17 Preparation of non-dusting organic
US2213477A (en) * 1935-12-12 1940-09-03 Gen Aniline & Film Corp Glycol and polyglycol ethers of isocyclic hydroxyl compounds
US2606156A (en) * 1950-06-09 1952-08-05 Purex Corp Ltd Deaeration and drying of watersoluble sulfonated detergent compositions

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3177147A (en) * 1960-09-23 1965-04-06 Colgate Palmolive Co Detergent compositions and preparation thereof
US3242091A (en) * 1961-12-19 1966-03-22 Colgate Palmolive Co Spray dried detergent concentrate
US3248330A (en) * 1963-05-24 1966-04-26 Monsanto Co Process for preparing a stable, freeflowing dishwashing composition

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GB812249A (en) 1959-04-22

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