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EP0723581A1 - Procede continu pour produire un detergent granulaire a haute densite - Google Patents

Procede continu pour produire un detergent granulaire a haute densite

Info

Publication number
EP0723581A1
EP0723581A1 EP94930796A EP94930796A EP0723581A1 EP 0723581 A1 EP0723581 A1 EP 0723581A1 EP 94930796 A EP94930796 A EP 94930796A EP 94930796 A EP94930796 A EP 94930796A EP 0723581 A1 EP0723581 A1 EP 0723581A1
Authority
EP
European Patent Office
Prior art keywords
detergent
densifier
agglomerates
mixer
process according
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP94930796A
Other languages
German (de)
English (en)
Inventor
Scott William Capeci
David Robert Nassano
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Procter and Gamble Co
Original Assignee
Procter and Gamble Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Procter and Gamble Co filed Critical Procter and Gamble Co
Publication of EP0723581A1 publication Critical patent/EP0723581A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02—Inorganic compounds ; Elemental compounds
    • C11D3/12—Water-insoluble compounds
    • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
    • C11D3/1246—Silicates, e.g. diatomaceous earth
    • C11D3/128—Aluminium silicates, e.g. zeolites
    • 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
    • C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
    • C11D11/0088—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads the liquefied ingredients being sprayed or adsorbed onto solid particles
    • 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
    • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
    • C11D17/065—High-density particulate detergent compositions

Definitions

  • the present invention generally relates to a process for producing detergent agglomerates. More particularly, the invention is directed to a continuous process during which high density detergent agglomerates are produced using a single moderate speed mixer/densifier, such as a Lodige KMTM (Ploughshare) mixer.
  • the process produces free flowing agglomerates having a density of at least 650 g 1 and are thus particularly useful in producing low dosage detergent compositions.
  • the first type of process involves spray-drying an aqueous detergent slurry in a spray-diying tower to produce highly porous detergent granules.
  • the various detergent components are dry mixed after which they are agglomerated with a binder such as a nonionic or anionic surfactant.
  • a binder such as a nonionic or anionic surfactant.
  • the most important factors which govern the density of the resulting detergent granules are the density, porosity and surface area of the various starting materials and their respective chemical composition. These parameters, however, can only be varied within a limited range. Thus, a substantial bulk density increase can only be achieved by additional processing steps which lead to densification of the detergent granules.
  • Curtis European patent application No. 451,894 (Unilever), discloses a process for preparing high density detergent granules by using two mixers in series. In particular, the starting materials are fed into a high speed mixer/densifier after which the materials are fed into a moderate speed mixer/densifier to increase the bulk density further.
  • Curtis initially requires a high speed mixer/densifier to pulverize the detergent granules and then a second moderate speed mixer/densifier to increase the density to the desired level.
  • the Hollingsworth et al process is only a batch process which does not facilitate large-scale production as currently required. While the Hollingsworth et al process provides high density detergent granules by way of a high speed, single- mixer batch process, it would be desirable to have a continuous process in which low or moderate speed mixers can be used to decrease operating costs.
  • Beerse et al U.S. Patent No. 5,108,646 (commonly assigned), relates to a process for agglomerating detergent builders by mixing zeolite and/or layered silicates in a mixer to form free flowing agglomerates. While Beerse et al suggest that their process can be used to produce detergent agglomerates, they do not provide a mechanism by which a high active surfactant paste consisting of a relatively high amount of surfactant and a low amount of liquid (e.g.
  • the present invention meets the aforementioned needs in the art by providing a process which continuously produces high density detergent agglomerates having a density of at least 650 g/1 in a single moderate speed mixer/densifier which is horizontally positioned tc facilitate continuous processing.
  • the process achieves the desired high density detergent agglomerates without unnecessary process parameters, such as the use of spray drying techniques, relatively high operating temperatures, and a plurality of mixer/densifiers, all of which increase manufacturing costs.
  • the term "agglomerates” refers to particles formed by agglomerating more porous starting detergent ingredients (particles) which typically have a smaller mean particle size than the formed agglomerates. All percentages and ratios used herein are expressed as percentages by weight (anhydrous basis) unless otherwise indicated. All viscosities referenced herein are measured at 70°C ( ⁇ 5°C) and at shear rates of about 10 to 100 sec -1 .
  • a process for preparing high density detergent agglomerates comprises the step of continuously mixing into a moderate speed mixer/densifier the following starting detergent ingredients: (i) from about 25% to about 50% of a detergent surfactant; (ii) from about 20% to about 50% of an aluminosilicate builder, and (iii) from about 10% to about 40% of an powdered material.
  • the ratio of the builder to the powdered material is from about 1: 1 to about 3.5:1.
  • the agglomerates exiting the mixer/densifier have a density of at least 650 g/1.
  • the process further may include one or more additional processing steps such as spraying an additional binder or adding a coating agent in the mixer/densifier to facilitate agglomeration. Thereafter, the agglomerates are dried to obtain high density granular detergent agglomerates which are ready for packaging as a low dosage detergent. Further, the invention provides another r»" ess in which free flowing, crisp, high density detergent agglomerates are produced from a visa....-; surfactant paste among other starting detergent ingredients.
  • This process comprises the step of continuously mixing into a moderate speed mixer/densifier the following starting detergent ingredients: (i) from about 25% to about 50% of a detergent surfactant in the form of an aqueous paste having a viscosity of from about 5,000 cps to about 100,000 cps; (ii) from about 20% to about 50% of an aluminosilicate builder, and (iii) from about 10% to about 40% of a sodium carbonate.
  • the ratio of the aluminosilicate builder to carbonate is from about 1:1 to about 3.5:1 and the agglomerates exiting the mixer/densifier have a density of at least 650 g/1. Thereafter, the agglomerates are dried to obtain high density granular detergent agglomerates which are ready for packaging as a low dosage detergent.
  • the present invention is directed to a process which continuously produces high density detergent agglomerates having a density of at least 650 g/1.
  • the process produces the desired high density detergent agglomerates from starting detergent ingredients without unnecessary process parameters which increase manufacturing costs and result in an undesirable detergent product.
  • the need for deformable, spray dried detergent granules, high operating temperatures in the mixer/densifier, and more than one mixer/densifier, all of which increase manufacturing costs, are no longer required by the present process.
  • post-tower detergent granules we mean those detergent granules which have been processed through a conventional spray-drying tower or similar apparatus.
  • the process of the invention allows for production of low dosage detergents in an environmentally conscious manner in that the use of spray drying techniques and the like which typically emit pollutants though their towers or stacks into the atmosphere is eliminated.
  • This feature of the process invention is extremely desirable in geographic areas which are especially sensitive to emission of pollutants into the atmosphere.
  • the invention entails continuously mixing into a moderate speed mixer/densifier the following starting detergent ingredients: (i) from about 25% to about 65%, preferably from about 35% to about 55% and, most preferably from about 38% to about 44%, of a detergent surfactant in an aqueous paste form; (ii) from about 20% to about 50%, preferably from about 25% to about 45% and, most preferably from about 30% to about 40% of an aluminosilicate builder, and (iii) from about 10% to about 40%, preferably from about 15% to about 30% and, most preferably from about 15% to about 25% of a powdered material.
  • the surfactant component level is preferably from about 25% to about 50%. It should be understood that additional detergent ingredients may also be mixed as described herein without departing from the scope of the process invention. However, at a minimum, the detergent surfactant, aluminosilicate builder and powdered material should be continuously mixed so as to insure production of the desired free flowing, crisp detergent agglomerates. The specifics of the various essential starting detergent ingredients as well as optional detergent ingredients are described hereinafter.
  • the ratio of the builder to the powdered material is from about 1:1 to about 3.5: 1, most preferably from about 2: 1 to about 3.5: 1.
  • the preferred builder is an aluminosilicate and the preferred powdered material is sodium carbonate
  • other less preferred materials as described hereinafter can be used in the process without departing from the scope of the invention.
  • detergent agglomerates having the desired properties are formed.
  • the detergent agglomerates exiting the mixer/densifier used herein will have a density of at least 650 g/1, more preferably from about 700 g/1 to about 800 g/1. Thereafter, the agglomerates are dried to obtain high density granular detergent agglomerates which are ready for packaging as a low dosage detergent.
  • the mean residence time of the various starting detergent ingredients in the low or moderate speed mixer/densifier is preferably in range from about 0.5 minutes to about 15 minutes, most preferably the residence time is about 1 to about 5 minutes. In this way, the density of the resulting detergent agglomerates is at the desired level.
  • the particle porosity of the resulting detergent agglomerates is preferably in a range from about 5% to about 20%, more preferably at about 10%.
  • a low porosity detergent agglomerate provides a dense or low dosage detergent product, to which the present process is primarily directed.
  • an attribute of dense or densified detergent agglomerates is the relative particle size.
  • the present process typically provides agglomerates having a mean particle size of from about 400 microns to about 700 microns, and more preferably from about 450 microns to about 500 microns.
  • mean particle size refers to individual agglomerates and not individual particles or detergent granules.
  • Such a feature is especially useful in the production of low dosage laundry detergents as well as other granular compositions such as dishwashing compositions.
  • the agglomerates are conditioned by either drying or adding a coating agent to improve flowability after they exit the moderate speed mixer/densifier to obtain the high density granular detergent agglomerates produced by the process which are in shippable or packagable form.
  • a coating agent to improve flowability after they exit the moderate speed mixer/densifier to obtain the high density granular detergent agglomerates produced by the process which are in shippable or packagable form.
  • apparatus such as a fluidized bed can be used for drying while an airlift can be used for cooling should it be necessary. Since the moderate speed mixer/densifier can be operated at relatively low temperatures, the need for cooling apparatus is not required by the present process, which thereby further reduces manufacturing costs of the final product.
  • the particular moderate speed mixer/densifier used in the present process should include pulverizing or grinding and agglomeration tools so that both techniques can be carried forth simultaneously in a single mixer.
  • the first processing step can be successfully completed, under the process parameters described herein, in a Lodige KMTM (Ploughshare) 600 mixer or similar brand mixer.
  • These types of mixers essentially consist of a horizontal, hollow static cylinder having a centrally mounted rotating shaft around which several plough-shaped blades are attached.
  • the shaft rotates at a speed of from about 15 ⁇ m to about 140 ⁇ m, more preferably from about 80 ⁇ m to about 120 ⁇ m.
  • the grinding or pulverizing is accomplished by cutters, generally smaller in size than the rotating shaft, which preferably operate at about 3600 ⁇ m.
  • Other mixers similar in nature which are suitable for use in the process include the Lodige PloughshareTM mixer and the Drais® K-T 160 mixer.
  • the moderate speed mixer/densifier preferably imparts a requisite amount of energy to form the desired agglomerates. More particularly, the moderate speed mixer/densifier imparts from about 5 ⁇ 10 ⁇ erg/kg to about 2 x 10 ⁇ erg/kg at a rate of from about 3 x 10 8 erg/kg-sec to about 3 x 10 9 erg/kg-sec to form free flowing high density detergent agglomerates.
  • the energy input and rate of input can be determined by calculations from power readings to the moderate speed mixer/densifier with and without granules, residence time of the granules in the mixer/densifier, and the mass of the granules in the mixer/densifier.
  • the process can comprises the step of spraying an additional binder in the mixer/densifier used in the agglomeration step to facilitate production of the desired detergent agglomerates.
  • a binder is added for purposes of enhancing agglomeration by providing a "binding" or "sticking" agent for the detergent components.
  • the binder is preferably selected from the group consisting of water, anionic surfactants, nonionic surfactants, polyethylene glycol, polyvinyl pyrrolidone polyacrylates, citric acid and mixtures thereof.
  • Other suitable binder materials including those listed herein are described in Beerse et al, U.S. Patent No. 5,108,646 (Procter & Gamble Co.), the disclosure of which is inco ⁇ orated herein by reference.
  • Another optional processing step includes continuously adding a coating agent such as zeolites and fumed silica to the mixer/densifier to facilitate free flowability of the resulting detergent agglomerates and to prevent over agglomeration.
  • a coating agent such as zeolites and fumed silica
  • the detergent starting materials can be fed into a pre-mixer, such as a Lodige CB mixer or a twin-screw extruder, prior to entering in the mixer/densifier described herein.
  • This step although optional, does indeed facilitate agglomeration.
  • Other optional steps contemplated by the present process include additional conditioning of the detergent agglomerates by subjecting the agglomerates to additional drying and/or addition of coating agents to improve flowability after they exit the mixer/densifier used in agglomeration.
  • the phrase "powdered material” refers to a material in the form of fine grains, generally having a particle size within a range of from about 2 microns to about 700, more typically from about 50 microns to about 100 microns.
  • the preferred powdered material used in the process is added in an optimum ratio with the aluminosilicate builder so as to provide structure and integrity in the resulting detergent agglomerates.
  • the resulting detergent agglomerates produced according to the process are "crisp" agglomerates as they are commonly referred to by those skilled in the art.
  • the powdered material can, and preferably does, add alkalinity to the detergent mixture, a condition necessary for optimum cleaning performance.
  • the powdered material is selected from the group consisting of carbonates, sulfates, carbonate/sulfate complexes, phosphates, polyethylene glycol and mixtures thereof.
  • the preferred powdered material is sodium carbonate which has been found to facilitate agglomeration especially well. While not intending to be limiting, specific suitable powdered materials include powdered tripolyphosphate, powdered tetrasodium pyrophosphate, powdered citrate, powdered sodium carbonate, powdered potassium carbonate, and powdered sodium sulfate.
  • the detergent surfactant used in the process can be in liquid, powdered or paste form.
  • the surfactant is in the form of a paste, it is an aqueous viscous paste.
  • This so-called viscous surfactant paste has a viscosity of from about 5,000 cps to about 100,000 cps, more preferably from about 10,000 cps to about 80,000 cps, and contains at least about 10% water, more preferably at least about 16% water.
  • the viscosity is measured at 70°C and at shear rates of about 10 to 100 sec. * -'.
  • the surfactant paste if used, preferably comprises a detersive surfactant in the amounts specified previously and the balance water and other conventional detergent ingredients.
  • the surfactant itself upon use alone or in the form of a viscous surfactant paste, is preferably selected from anionic, nonionic, zwitterionic, ampholytic and cationic classes and compatible mixtures thereof.
  • Detergent surfactants useful herein are described in U.S. Patent 3,664,961, Norris, issued May 23, 1972, and in U.S. Patent 3,919,678, Laughlin et al., issued December 30, 1975, both of which are incorporated herein by reference.
  • Useful cationic surfactants also include those described in U.S.
  • Patent 4,222,905 Cockrell, issued September 16, 1980, and in U.S. Patent 4,239,659, Mu ⁇ hy, issued December 16, 1980, both of which are also incorporated herein by reference.
  • anionics and nonionics are preferred and anionics are most preferred.
  • detergent surfactants useful in the present surfactant paste.
  • Water-soluble salts of the higher fatty acids i.e., "soaps" are useful anionic surfactants in the compositions herein.
  • Soaps can be made by direct saponification of fats and oils or by the neutralization of free fatty acids.
  • Particularly useful are the sodium and potassium salts of the mixtures of fatty acids derived from coconut oil and tallow, i.e., sodium or potassium tallow and coconut soap.
  • Additional anionic surfactants which suitable for use herein include the water-soluble salts, preferably the alkali metal, ammonium and alkylolammonium salts, of organic sulfuric reaction products having in their molecular structure an alkyl group containing from about 10 to about 20 carbon atoms and a sulfonic acid or sulfuric acid ester group.
  • alkyl is the alkyl portion of acyl groups.
  • this group of synthetic surfactants are the sodium and potassium alkyl sulfates, especially those obtained by sulfating the higher alcohols (C g ⁇ g carbon atoms) such as those produced by reducing the glycerides of tallow or coconut oil; and the sodium and potassium alkylbenzene sulfonates in which the alkyl group contains from about 9 to about 15 carbon atoms, in straight chain or branched chain configuration, e.g., those of the type described in U.S. Patents 2,220,099 and 2,477,383.
  • Especially valuable are linear straight chain alkylbenzene sulfonates in which the average number of carbon atoms in the alkyl group is from about 11 to 13, abbreviated as Cu_i3 LAS.
  • anionic surfactants suitable for use herein are the sodium alkyl glyceryl ether sulfonates, especially those ethers of higher alcohols derived from tallow and coconut oil; sodium coconut oil fatty acid monoglyceride sulfonates and sulfates; sodium or potassium of ethylene oxide per molecule and wherein the alkyl groups contain from about 8 to about 12 carbon atoms; and sodium or potassium salts of alkyl ethylene oxide ether sulfates containing about 1 to about 10 units of ethylene oxide per molecule and wherein the alkyl group contains from about 10 to about 20 carbon atoms.
  • suitable anionic surfactants include the water-soluble salts of esters of alpha-sulfonated fatty acids containing from about 6 to 20 carbon atoms in the fatty acid group and from about 1 to 10 carbon atoms in the ester group; water-soluble salts of 2-acyloxyalkane-l-sulfonic acids containing from about 2 to 9 carbon atoms in the acyl group and from about 9 to about 23 carbon atoms in the alkane moiety; water-soluble salts of olefin and paraffin sulfonates containing from about 12 to 20 carbon atoms; and beta-alkyloxy alkane sulfonates containing from about 1 to 3 carbon atoms in the alkyl group and from about 8 to 20 carbon atoms in the alkane moiety.
  • Preferred anionic surfactants are C . Q linear alkylbenzene sulfonate and C n 0 alkyl lU-lo 10-18 sulfate.
  • low moisture (less than about 25% water) alkyl sulfate paste can be the sole ingredient in the surfactant paste.
  • Most preferred are C. ft ._ alkyl sulfates, linear or branched, and any of primary, secondary or tertiary.
  • a preferred embodiment of the present invention is wherein the surfactant paste comprises from about 20% to about 40% of a mixture of sodium C n linear alkylbenzene sulfonate and sodium C._ .
  • alkyl sulfate in a weight ratio of " , ut 2:1 to 1:2.
  • Another preferred embodiment of the detergent composition includes a mixt ; of C j o-i ⁇ alkyl sulfate and C ⁇ Q-18 - ⁇ ethoxy sulfate in a weight ratio of about 80:20.
  • Water-soluble nonionic surfactants are also useful in the instant invention. Such nonionic materials include 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. The length of the polyoxyalkylene group which is condensed with any particular hydrophobic group can be readily adjusted to yield a water-soluble compound having the desired degree of balance between hydrophilic and hydrophobic elements.
  • Suitable nonionic surfactants include the polyethylene oxide condensates of alkyl phenols, e.g., the condensation products of alkyl phenols having an alkyl group containing from about 6 to 15 carbon atoms, in either a straight chain or branched chain configuration, with from about 3 to 12 moles of ethylene oxide per mole of alkyl phenol. Included are the water-soluble and water-dispersible condensation products of aliphatic alcohols containing from 8 to 22 carbon atoms, in either straight chain or branched configuration, with from 3 to 12 moles of ethylene oxide per mole of alcohol.
  • nonionics suitable for use herein are semi-polar nonionic surfactants which include water-soluble amine oxides containing one alkyl moiety of from abut 10 to 18 carbon atoms and two moieties selected from the group of alkyl and hydroxyalkyl moieties of from about 1 to about 3 carbon atoms; water-soluble phosphine oxides containing one alkyl moiety of about 10 to 18 carbon atoms and two moieties selected from the group consisting of alkyl groups and hydroxyalkyl groups containing from about 1 to 3 carbon atoms; and water-soluble sulfoxides containing one alkyl moiety of from about 10 to 18 carbon atoms and a moiety selected from the group consisting of alkyl and hydroxyalkyl moieties of from about 1 to 3 carbon atoms.
  • Preferred nonionic surfactants are of the formula R (OC,H .) OH, wherein R is a
  • Particularly preferred are condensation products of C..-C. , alcohols with from about 5 to about 20 moles of ethylene oxide per mole of alcohol, e.g., C..-C.. alcohol condensed with about 6.5 moles of ethylene oxide per mole of alcohol.
  • nonionic surfactants include polyhydroxy fatty acid amides of the formula
  • R— C— N— Z wherein R is a C9.17 alkyl or alkenyl, R j is a methyl group and Z is glycityl derived from a reduced sugar or alkoxylated derivative thereof. Examples are N-methyl N-1-deoxyglucityl cocoamide and N- methyl N-1-deoxyglucityl oleamide. Processes for making polyhydroxy fatty acid amides are known and can be found in Wilson, U.S. Patent No. 2,965,576 and Schwartz, U.S. Patent No. 2,703,798, the disclosures of which are incorporated herein by reference.
  • Ampholytic surfactants include derivatives of aliphatic or aliphatic derivatives of heterocyclic secondary and tertiary amines in which the aliphatic moiety can be straight chain or branched and wherein one of the aliphatic substituents contains from about 8 to 18 carbon atoms and at least one aliphatic substituent contains an anionic water-solubilizing group.
  • Zwitterionic surfactants include derivatives of aliphatic, quaternary, ammonium, phosphonium, and sulfonium compounds in which one of the aliphatic substituents contains from about 8 to 18 carbon atoms.
  • Cationic surfactants can also be included in the present invention.
  • Cationic surfactants comprise a wide variety of compounds characterized by one or more organic hydrophobic groups in the cation and generally by a quaternary nitrogen associated with an acid radical. Pentavalent nitrogen ring compounds are also considered quaternary nitrogen compounds. Suitable anions are halides, methyl sulfate and hydroxide. Tertiary amines can have characteristics similar to cationic surfactants at washing solution pH values less than about 8.5. A more complete disclosure of these and other cationic surfactants useful herein can be found in U.S. Patent 4,228,044, Cambre, issued October 14, 1980, incorporated herein by reference.
  • Cationic surfactants are often used in detergent compositions to provide fabric softening and/or antistatic benefits.
  • Antistatic agents which provide some softening benefit and which are preferred herein are the quaternary ammonium salts described in U.S. Patent 3,936,537, Baskerville, Jr. et al., issued February 3, 1976, the disclosure of which is incorporated herein by reference.
  • the starting detergent surfactant ingredient can also be a secondary (2,3) alkyl sulfate surfactant as described herein.
  • the secondary (2,3) alkyl sulfates used herein will be distinguished from conventional alkyl sulfate surfactants where appropriate.
  • Conventional primary alkyl sulfate surfactants have the general formula
  • ROS03-M+ wherein R is typically a linear C10-C20 hydrocarbyl group and M is a water-solubilizing cation.
  • Branched-chain primary alkyl sulfate surfactants i.e., branched-chain "PAS" having 10-20 carbon atoms are also known; see, for example, European Patent Application 439,316, Smith et al, filed 21.01.91, the disclosure of which is incorporated herein by reference.
  • Secondary alkyl sulfate surfactants are those materials which have the sulfate moiety distributed randomly along the hydrocarbyl "backbone" of the molecule. Such materials may be depicted by the structure
  • the selected secondary (2,3) alkyl sulfate surfactant sjd herein comprise structures of formulas A and B - ? .:
  • x and (y+l) are, respectively, integers >f at least about 6, and can range from about 7 to about 20, preferably about 10 to about 16.
  • M is a cation, such as an alkali metal, ammonium, alkanolammonium, alkaline earth metal, or the like. Sodium is typical for use as M to prepare the water-soluble (2,3) alkyl sulfates, but ethanolammonium, diethanolammonium, triethanolammonium, potassium, ammonium, and the like, can also be used.
  • the physical/chemical properties of the foregoing types of alkyl sulfate surfactants are unexpectedly different, one from another, in several aspects v - are important to formulators of various types of detergent compositions, for example, the primary alkyl sulfates can disadvantageously interact with, and even be precipitated by, metal cations such as calcium and magnesium.
  • metal cations such as calcium and magnesium.
  • water hardness can negatively affect the primary alkyl sulfates to a greater extent than the secondary (2,3) alkyl sulfates herein.
  • the secondary (2,3) alkyl sulfates have now been found to be preferred for use in the presence of calcium ions and under conditions of high water hardness, or in the so-called "under-built" situation which can occur when nonphosphate builders are employed.
  • the solubility of the primary alkyl sulfates is not as great as the secondary (2,3) alkyl sulfates.
  • the formulation of high-active surfactant particles has now been found to be simpler and more effective with the secondary (2,3) alkyl sulfates than with the primary alkyl sulfates.
  • the secondary (2,3) alkyl sulfates are exceptionally easy to formulate as heavy-duty granular laundry detergents.
  • the random secondary alkyl sulfates i.e., secondary alkyl sulfates with the sulfate group at positions such as the 4, 5, 6, 7, etc. secondary carbon atoms
  • such materials tend to be tacky solids or, more generally, pastes.
  • the random alkyl sulfates do not afford the processing advantages associated with the solid secondary (2,3) alkyl sulfates when formulating detergent granules.
  • the secondary (2,3) alkyl sulfates herein provide better sudsing than the random mixtures. It is preferred that the secondary (2,3) alkyl sulfates be substantially free (i.e., contain less than about 20%, more preferably less than about 10%, most preferably less than about 5%) of such random secondary alkyl sulfates.
  • 2,3-disulfates may also be present, but generally comprise no more than 5% of the mixture of secondary (2,3) alkyl mono-sulfates.
  • Such materials are available as under the name "DAN”, e.g., "DAN 200" from Shell Oil Company.
  • solubility of the "crystalline" secondary (2,3) alkyl sulfate surfactants is desired, the formulator may wish to employ mixtures of such surfactants having a mixture of alkyl chain lengths.
  • a mixture of C ⁇ -Cj alkyl chains will provide an increase in solubility over a secondary (2,3) alkyl sulfate wherein the alkyl chain is, say, entirely C ⁇ .
  • the solubility c c he secondaiy (2,3) alkyl sulfates can also be enhanced by the addition thereto of other surfacL ⁇ ..s such as the material which decreases the crystallinity of the secondary (2,3) alkyl sulfates.
  • Such crystallinity-interrupting materials are typically effective at levels of 20%, or less, of the secondary (2,3) alkyl sulfate.
  • the starting detergent ingredients of the present process also comprise a detergent aluminosilicate builder which are referenced as aluminosilicate ion exchange materials.
  • the aluminosilicate ion exchange materials used herein as a detergent builder preferably have both a high calcium ion exchange capacity and a high exchange rate. Without intending to be limited by ieory, it is believed that such high calcium ion exchange rate and capacity are a function of several interrelated factors which derive from the method by which the aluminosilicate ion exchange material is produced.
  • the aluminosilicate ion exchange materials used herein are preferably produced in accordance with Corkill et al, U.S. Patent No. 4,605,509 (Procter & Gamble), the disclosure of which is incorporated herein by reference.
  • the aluminosilicate ion exchange material is in "sodium" form since the potassium and hydrogen forms of the instant aluminosilicate do not exhibit the as high of an ex: nge rate and capacity as provided by the sodium form.
  • the aluminosilicate ion exchange material preferably is in overdried form so as to facilitate production of crisp detergent agglomerates as described herein.
  • the aluminosilicate ion exchange materials used herein preferably have particle size diameters which optimize their effectiveness as deterg Guilders.
  • particle size diameter represents the average particle size diame of a given aluminosilicate ion exchange material as determined by conventional analytical techniques, such as microscopic determination and scanning electron microscope (SEM).
  • the preferred particle size diameter of the aluminosilicate is from about 0.1 micron to about 10 microns, more preferably from about 0.5 microns to about 9 microns. Most preferably, the particle size diameter is from about 1 microns to about 8 microns.
  • the aluminosilicate ion exchange material has the formula Na z [(A10 2 ) z .(Si0 2 )y]xH 2 0 wherein z and y are integers of at least 6, the molar ratio of z to y is from about 1 to about 5 and x is from about 10 to about 264. More preferably, the aluminosilicate has the formula
  • aluminosilicates are available commercially, for example under designations Zeolite A, Zeolite B and Zeolite X.
  • Naturally-occurring or synthetically derived aluminosilicate ion exchange materials suitable for use herein can be made as described in Krummel et al, U.S. Patent No. 3,985,669, the disclosure of which is incorporated herein by reference.
  • the aluminosilicates used herein are further characterized by their ion exchange capacity which is at least about 200 mg equivalent of CaC ⁇ 3 hardness/gram, calculated on an anhydrous basis, and which is preferably in a range from about 300 to 352 mg equivalent of CaC03 hardness/gram. Additionally, the instant aluminosilicate ion exchange materials are still further characterized by their calcium ion exchange rate which is at least about 2 grains Ca ++ /gallon/minute/-gram/gallon, and more preferably in a range from about 2 grains Ca "H" /gallon/minute/-gram/gallon to about 6 grains Ca ⁇ /gallon/minuteZ-gram/gallon .
  • the starting or entering detergent components in the present process can also include any number of additional ingredients. These include other detergency builders, bleaches, bleach activators, suds boosters or suds suppressors, anti-tarnish and anticorrosion agents, soil suspending agents, soil release agents, germicides, pH adjusting agents, non-builder alkalinity sources, chelating agents, smectite clays, enzymes, enzyme-stabilizing agents and perfumes. See U.S. Patent 3,936,537, issued February 3, 1976 to Baskerville, Jr. et al., incorporated herein by reference.
  • Other builders can be generally selected from the various water-soluble, alkali metal, ammonium or substituted ammonium phosphates, polyphosphates, phosphonates, polyphosphonates, carbonates, borates, polyhydroxy sulfonates, polyacetates, carboxylates, and polycarboxylates.
  • the alkali metal especially sodium, salts of the above.
  • Preferred for use herein are the phosphates, carbonates, ]0 -. discipline fatty acids, polycarboxylates, and mixtures thereof. More preferred are sodium tripolyphosphate, tetrasodium pyrophosphate, citrate, tartrate mono- and di-succinates, and mixtures thereof (see below).
  • crystalline layered sodium silicates exhibit a clearly increased calcium and magnesium ion exchange capacity.
  • the layered sodium silicates prefer magnesium ions over calcium ions, a feature necessary to insure that substantially all of the "hardness" is removed from the wash water.
  • These crystalline layered sodium silicates are generally more expensive than amo ⁇ hous silicates as well as other builders. Accordingly, in order to provide an economically feasible laundry detergent, the proportion of crystalline layered sodium silicates used must be determined judiciously.
  • the crystalline layered sodium silicates suitable for use herein preferably have the formula NaMSi x 0 2x+ i.yH 2 0 wherein M is sodium or hydrogen, x is from about 1.9 to about 4 and y is from about 0 to about 20. More preferably, the crystalline layered sodium silicate has the formula
  • inorganic phosphate builders are sodium and potassium tripolyphosphate, pyrophosphate, polymeric metaphosphate having a degree of polymerization of from about 6 to 21, and orthophosphates.
  • polyphosphonate builders are the sodium and potassium salts of ethylene diphosphonic acid, the sodium and potassium salts of ethane 1-hydroxy-l, 1 -diphosphonic acid and the sodium and potassium salts of ethane,
  • 1,1,2-triphosphonic acid 1,1,2-triphosphonic acid.
  • Other phosphorus builder compounds are disclosed in U.S. Patents 3,159,581; 3,213,030; 3,422,021; 3,422,137; 3,400,176 and 3,400,148, all of which are incorporated herein by reference.
  • nonphosphorus, inorganic builders are tetraborate decahydrate and silicates having a weight ratio of SiO. to alkali metal oxide of from about 0.5 to about 4.0, preferably from about 1.0 to about 2.4.
  • Water-soluble, nonphosphorus organic builders useful herein include the various alkali metal, ammonium and substituted ammonium polyacetates, carboxylates, polycarboxylates and polyhydroxy sulfonates.
  • polyacetate and polycarboxylate builders are the sodium, potassium, lithium, ammonium ar... substituted ammonium salts of ethylene diamine tetraacetic acid, nitrilotriacetic acid, oxydisuccinic acid, mellitic acid, benzene polycarboxylic acids, and citric acid.
  • Polymeric polycarboxylate builders are set forth in U.S. Patent 3,308,067, Diehl, issued March 7, 19 the disclosure of which is incorporated herein by reference.
  • Such materials include the water-soluble salts of homo- and copolymers of aliphatic carboxylic acids such as maleic acid, itaconic acid, mesaconic acid, rumaric acid, aconitic acid, citraconic acid and methylenemalonic acid.
  • Some of these materials are useful as the water-soluble anionic polymer as hereinafter described, but only if in intimate admixture with the non-soap anionic surfactant.
  • polycarboxylates for use herein are the polyacetal carboxylates described in U.S. Patent 4,144,226, issued March 13, 1979 to Crutchfield et al, and U.S. Patent 4,246,495, issued March 27, 1979 to Crutchfield et al, both of which are incorporated herein by reference.
  • polyacetal carboxylates can be prepared by bringing together under polymerization conditions an ester of glyoxylic acid and a polymerization initiator. The resulting polyacetal carboxylate ester is then attached to chemically stable end groups to stabilize the polyacetal carboxylate against rapid depolymerization in alkaline solution, converted to the corresponding salt, and added to a detergent composition.
  • Particularly preferred polycarboxylate builders are the ether carboxylate builder compositions comprising a combination of tartrate monosuccinate and tartrate disuccinate described in U.S. Patent 4,663,071, Bush et al., issued May 5, 1987, the disclosure of which is incorporated herein by reference.
  • Bleaching agents and activators are described in U.S. Patent 4,412,934, Chung et al., issued November 1, 1983, and in U.S. Patent 4,483,781, Hartman, issued November 20, 1984, both of which are incorporated herein by reference.
  • Chelating agents are also described in U.S. Patent 4,663,071, Bush et al., from Column 17, line 54 through Column 18, line 68, incorporated herein by reference.
  • Suds modifiers are also optional ingredients and are described in U.S. Patents 3,933,672, issued January 20, 1976 to Bartoletta et al., and 4,136,045, issued January 23, 1979 to Gault et al., both incorporated herein by reference.
  • Suitable smectite clays for use herein are described in U.S. Patent 4,762,645, Tucker et al, issued August 9, 1988, Column 6, line 3 through Column 7, line 24, incorporated herein by reference.
  • Suitable additional detergency builders for use herein are enumerated in the Baskerville patent, Column 13, line 54 through Column 16, line 16, and in U.S. Patent 4,663,071, Bush et al, issued May 5, 1987, both incorporated herein by reference.
  • EXAMPLE I This Example illustrates the process of the invention which produces free flowing, crisp, high density detergent agglomerates.
  • Several feed streams of various detergent starting ingredients are continuously fed, at a rate of 660 kg/hr, into a Lodige KMTM (Ploughshare) 600 mixer/densifier, which is a horizontally-positioned moderate speed mixer/densifier.
  • the rotational speed of the shaft in the mixer/densifier is about 100 ⁇ m and the rotational speed of the cutters is about 3600 ⁇ m.
  • the relative proportion of each starting detergent ingredient in the total feed stream fed into the mixer/densifier (the phrase "total feed stream” meaning the aggregate of all the individual feed streams being fed into the mixer/densifier) is presented in Table I below:
  • Polyethylene glycol (MW 4000) 1.3
  • the starting detergent ingredients are continuously passed through a Lodige CB 30 pre- mixer and then into a Lodige KMTM (Ploughshare) 600 mixer/densifier, their mean residence time in the mixer/densifier is about 2-3 minutes.
  • a water binder is continuously fed into the Lodige KMTM 600 mixer/densifier to aid in the agglomeration process.
  • the agglomerates from the mixer/densifier are dried in a conventional fluidized bed dryer after they exit the Lodige KMTM 600 mixer/densifier to obtain the high density granular detergent agglomerates produced by the process.
  • the density of the resulting detergent agglomerates is 796 g/1 and the mean particle size is 613 microns.
  • EXAMPLE II This Example also illustrates the process of the invention and incorporates the parameters of Example I. Accordingly, several feed streams of various detergent starting ingredients are continuously fed, at a rate of 660 kg/hr, into a Lodige KMTM (Ploughshare) 600 mixer/densifier, which is a horizontally-positioned moderate speed mixer/densifier. The rotational speed of the shaft in the mixer/densifier is about 100 ⁇ m and the rotational speed of the cutters is about 3600 ⁇ m. The relative proportion of each starting detergent ingredient in the total feed stream fed into the mixer/densifier is presented in Table IT below:
  • Polyethylene glycol (MW 4000) 1.3
  • While the starting detergent ingredients are continuously passed into a Lodige KMTM (Ploughshare) 600 mixer/densifier, their mean residence time in the mixer/densifier is about 2-3 minutes.
  • a water binder is continuously fed into the Lodige KMTM 600 mixer/densifier to aid in the agglomeration process.
  • the agglomerates from the mixer/densifier are dried in a conventional fluidized bed dryer after they exit the Lodige KMTM 600 mixer/densifier to obtain the high density granular detergent agglomerates produced by the process.
  • the density of the resulting detergent agglomerates is 700 g/1 and a mean particle size of 550 microns.

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Abstract

L'invention concerne un procédé pour produire un détergent granulaire à haute densité, c'est-à-dire une masse volumique d'au moins 650 g/l. Le procédé comprend l'étape consistant à mélanger en continu à vitesse modérée dans un appareil mélangeur/appareil de densification les ingrédients pour détergent suivants: (i) de 25 % environ à 50 % environ d'un tensioactif pour détergent; (ii) de 20 % environ à 50 % environ d'adjuvant pour détergents et (iii) de 10 % environ à 40 % environ d'un produit pulvérulent. Le rapport de l'adjuvant pour détergent sur le produit pulvérulent se situe entre 1:1 environ et 3,5:1 environ. Les agglomérats sortant de l'appareil mélangeur/appareil de densification ont une masse volumique d'au moins 650g/l. Le procédé peut en outre comporter une ou plusieurs étapes additionnelles, comme par exemple la pulvérisation d'un liant ou l'addition d'un agent d'enrobage dans l'appareil mélangeur/appareil de densification pour faciliter l'agglomération. Ensuite, les agglomérats sont séchés, ce qui permet d'obtenir un détergent granulaire utilisé à faible dose.
EP94930796A 1993-10-15 1994-10-14 Procede continu pour produire un detergent granulaire a haute densite Withdrawn EP0723581A1 (fr)

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US13787793A 1993-10-15 1993-10-15
US137877 1993-10-15
PCT/US1994/011759 WO1995010595A1 (fr) 1993-10-15 1994-10-14 Procede continu pour produire un detergent granulaire a haute densite

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US5733862A (en) * 1993-08-27 1998-03-31 The Procter & Gamble Company Process for making a high density detergent composition from a sufactant paste containing a non-aqueous binder
US5633224A (en) * 1994-07-14 1997-05-27 The Procter & Gamble Company Low pH granular detergent composition
BR9610191A (pt) * 1995-09-04 1998-12-15 Unilever Nv Processo para a preparação por um procedimento n o de secagem por pulverização de uma composição ou componente detergente em partículas a respectiva composição ou componente detergente em partículas e uso de uma pré-mistura aquosa de um polímero
CA2232071C (fr) * 1995-09-14 2001-10-30 The Procter & Gamble Company Procede de fabrication d'une composition detergente haute densite a partir d'une pate de tensioactif contenant un liant non aqueux
JP3305327B2 (ja) * 1996-10-04 2002-07-22 ザ、プロクター、エンド、ギャンブル、カンパニー 非塔式製造法による低密度洗剤組成物の製造法
US6143711A (en) * 1996-10-04 2000-11-07 The Procter & Gamble Company Process for making a detergent composition by non-tower process
BR112012000460A2 (pt) * 2009-07-09 2016-02-16 Procter & Gamble processo contínuo para produção de uma composição detergente para lavagem de roupas

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GB8810821D0 (en) * 1988-05-06 1988-06-08 Unilever Plc Detergent compositions & process for preparing them
CA2001535C (fr) * 1988-11-02 1995-01-31 Peter Willem Appel Methode d'elaboration d'un produit detersif granulaire a haute densite
JP2636036B2 (ja) * 1989-03-06 1997-07-30 花王株式会社 高密度洗剤粒子の連続造粒方法及び装置
GB8907187D0 (en) * 1989-03-30 1989-05-10 Unilever Plc Detergent compositions and process for preparing them

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See references of WO9510595A1 *

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CA2173108A1 (fr) 1995-04-20

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