EP0918843B1 - Process for making high density detergent - Google Patents

Process for making high density detergent Download PDF

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Publication number
EP0918843B1
EP0918843B1 EP97935094A EP97935094A EP0918843B1 EP 0918843 B1 EP0918843 B1 EP 0918843B1 EP 97935094 A EP97935094 A EP 97935094A EP 97935094 A EP97935094 A EP 97935094A EP 0918843 B1 EP0918843 B1 EP 0918843B1
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Prior art keywords
detergent
densifier
speed mixer
shaft
agglomerates
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EP97935094A
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German (de)
English (en)
French (fr)
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EP0918843A1 (en
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Paul Anthony Zaffiro
William Garrett Halvorsen
Scott William Capeci
Antonio Williams
Larry Vincent Dalton
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Procter and Gamble Co
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Procter and Gamble Co
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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
    • C11D11/0082—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
    • 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 high density detergent compositions. More particularly, the invention is directed to a continuous process during which high density detergent agglomerates are produced by feeding a surfactant paste and dry starting detergent material into a mixer/densifier having a centrally positioned rotating shaft with minimal vibration. The process produces a free flowing, high density detergent composition which can be commercially sold as a low dosage or "compact" detergent composition.
  • the first type of process involves spray-drying an aqueous detergent slurry in a spray-drying 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.
  • Patent 5,516,448 Beerse et al, U.S. Patent No. 5,108,646 (Procter & Gamble); Hollingsworth et al, European Patent Application 351,937 (Unilever); and Swatling et al, U.S. Patent No. 5,205,958.
  • the present invention meets the aforementioned needs in the art by providing a process which continuously produces a high density detergent composition via a process during which high density detergent agglomerates are produced by feeding a surfactant paste and dry starting detergent material into a mixer/densifier having a centrally positioned rotating shaft with minimal vibration.
  • tuned dampers have been mounted on the centrally rotating shaft in the mixer/densifier unexpectedly resulting in a process which produces a high density detergent composition with minimal mechanical vibration and repair expenses normally associated such vibration.
  • the process produces a free flowing, high density detergent composition which can be commercially sold as a low dosage or "compact" detergent composition.
  • agglomerates refers to particles formed by agglomerating starting detergent ingredients 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 a crisp, free flowing, high density detergent composition comprises the steps of:
  • another continuous process for producing a high density detergent composition comprises the steps of: (a) continuously mixing spray-dried detergent granules into a moderate speed mixer/densifier, wherein the speed mixer/densifier includes a centrally rotating shaft on which a tuned damper apparatus is mounted such that the peak vibration of the shaft is from about -1.0G to about 1.0G in a frequency range of from about 10 Hz to about 20 Hz at the mid-span length of the shaft; and (b) drying the detergent agglomerates so as to form the detergent composition.
  • the detergent compositions made by any of the processes described herein is also provided by the invention.
  • the present process can be used in the production of low dosage, high density detergent compositions containing agglomerates produced directly from starting detergent ingredients as well as compositions containing conventional spray-dried granules that have undergone "post-tower” densification.
  • spray-dried granules we mean porous granules that have been made by drying an aqueous slurry of detergent ingredients including surfactant, builder and other standard adjunct detergent ingredients. Typically, the drying is completed by spraying the aqueous slurry into a tower having a counter current hot air stream.
  • post-tower densification, we mean those detergent granules which have been processed through a conventional spray-drying tower or similar apparatus, and thereafter, through mixer/densifiers as described herein.
  • Fig. 1 presents a flow chart illustrating the instant process and various embodiments thereof.
  • the invention entails continuously mixing into a high speed mixer/densifier 10 several streams of starting detergent ingredients including a surfactant paste stream 12 and a dry starting detergent material stream 14.
  • the surfactant paste 12 preferably comprises 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.
  • the dry starting detergent material 14 comprises 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 or zeolite builder, and from about 10% to about 40%, preferably from about 15% to about 30% and, most preferably from about 15% to about 25% of a sodium carbonate.
  • the surfactant paste 12 and the dry starting detergent material 14 are continuously mixed within the ratio ranges described herein so as to insure production of the desired free flowing, crisp, high density detergent composition.
  • the ratio of the surfactant paste 12 to the dry starting detergent material 14 is from about 1:10 to about 10:1, more preferably from about 1:4 to about 4:1 and, most preferably from about 2:1 to about 2:3.
  • high speed mixer/densifier 10 which preferably is a Lödige CB 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 100 rpm to about 2500 rpm, more preferably from about 300 rpm to about 1600 rpm.
  • the mean residence time of the detergent ingredients in the high speed mixer/densifier 10 is preferably in range from about 2 seconds to about 45 seconds, and most preferably from about 5 seconds to about 15 seconds.
  • the resulting detergent agglomerates formed in the high speed mixer/densifier 10 are then fed into a lower or moderate speed mixer/densifier 16 during which further build-up agglomeration is carried forth.
  • a single stream of spray-dried granules (not shown) is inputted directly into the moderate speed mixer/densifier, wherein the high speed mixer/densifier 10 is strictly optional for this particular embodiment of the invention.
  • the moderate speed mixer/densifier 16 used in the present process should include liquid distribution and agglomeration tools so that both techniques can be carried forth simultaneously.
  • the moderate speed mixer/densifier 16 is preferable to be, for example, a Lödige KM (Ploughshare) mixer, Drais® K-T 160 mixer or similar brand mixer.
  • the residence time in the moderate speed mixer/densifier 16 is preferably from about 0.5 minutes to about 15 minutes, most preferably the residence time is about 1 to about 10 minutes.
  • Fig. 2 a perspective partial cut-away view of moderate speed mixer/densifier 16 is depicted.
  • a centrally located shaft 18 rotates inside the moderate speed mixer/densifer 16 (e.g. Lödige KM (Ploughshare) mixer).
  • the moderate speed mixer/densifer 16 e.g. Lödige KM (Ploughshare) mixer.
  • at least one tuned damper 20 is mounted on the rotating shaft 18.
  • the moderate speed mixer/densifer 16 accomplishes liquid distribution via cutters 22 mounted on the inside wall of the mixer/densifier 16 and are generally smaller in size than the rotating shaft 18.
  • the cutters typically operate at least about 3600 rpm.
  • the moderate speed mixer/densifer 16 also has ploughs 24 that are mounted to the centrally rotating shaft 18 to aid in the mixing/densifying operations in the process and a pair of inlet ports 21 and 23 that are capable of receiving detergent material from the high speed mixer/densifier 10.
  • Fig. 3 discloses a partial side cross-sectional view of the tuned damper 20 and Fig. 4 shows an end view of shaft 18 with the tuned damper 20 mounted thereon. It can be seen from Figs. 3 and 4 that the tuned damper 20 includes four cylinder-shaped damping apparatus 26 to minimize the shaft 18 mechanical vibration.
  • the tuned damper 20 includes at least two, and preferably four, of these so-called cylinder-shaped damping apparatus 26, which are mounted about every 90° on the shaft 18 and connected via connecting bars 23.
  • the damping apparatus 26 can be attached to the rotating shaft 18 by any known convenient mechanical apparatus such as a split ring assembly that is then enclosed by a cover casing 21 as depicted in Figs. 2, 3 and 4.
  • the outer casing 21 of the damping apparatus of the tuned damper 20 is preferably made of a material able to withstand the environment to which it is exposed. In the current process, the environment is detergent ingredients which permits the outer casing 21 to be made from plastic.
  • the damping apparatus 26 includes a pair of tuning rods 28 and 30 mounted adjacent to a pair of flexible or spring-like members 32 and 34.
  • the flexible members 32 and 34 may be made of any flexible material such as an elastomeric material including nitrile, natural or synthetic butyl rubbers (e.g. from Ilene Industries, Inc.) or can be molded to the final shape by a supplier (e.g. Forsheda AB, Sweden).
  • the flexible members 32 and 34 contact a weight 35 which is instrumental in damping the mechanical vibration resulting from the continuous rotating speed of the shaft 18.
  • the tuned damper 20 is adjusted via manipulation and mounting location of the damping apparatus 26 such that the peak vibration of the shaft 18 is within a selected range.
  • the tuned damper 20 is adjusted via sizing of the flexible members 32 and 34 to achieve the desired natural frequency of the tuned damper 20.
  • the tuned damper 20 is tuned such that its natural frequency is about 95% of the shaft 18 natural frequency. If more than one tuned damper 20 is used, the natural frequency of each tuned damper 20 mounted on shaft 18 can be distributed at several frequencies in the 10 HZ to 20 Hz range, or can all be tuned to the same frequency.
  • the preferred peak vibration range for the shaft 18 is from about -1.0G to about 1.0G, more preferably from about -0.5G to about 0.5G, and most preferably from about -0.25G to about 0.25G, in a frequency range of from about 10 Hz to about 20 Hz as measured at the mid-span length of the shaft 18.
  • Such peak vibration ranges represent a dramatic improvement over peak vibrations typically experienced in commercial scale manufacturing facilities which can be on the order of ⁇ 3.5G.
  • the peak vibration is preferably measured using 90 second intervals. As those skilled in the art will appreciate, such peak vibration measurements are easily completed using a conventional accelerometer (available from PCB 308B ICP Company, Buffalo, NY).
  • the vibration of shaft 18 is recorded using the accelerometer attached to a power supply (e.g., PCB 480E090 from ICP Company, and a battery operated digital tape recorder such as the Sony TCD-D3 DAT recorder).
  • a power supply e.g., PCB 480E090 from ICP Company, and a battery operated digital tape recorder such as the Sony TCD-D3 DAT recorder.
  • the recorder and power supply are mounted in a waterproof, shock proof enclosure (such as the Carlon CJ1085 Enclosure).
  • the sensor is attached to the shaft 18 by means of dental cement or other rigid adhesive and is positioned such that radial shaft vibration is measured.
  • the vibration is recorded for at least 2 hours, preferably for 4 hours.
  • the tape recorder is removed from the enclosure and played back.
  • the data is plotted in 90 second intervals on either a digital or analog plotting device (such as the Hewlett-Packard 3560A or 35670A analyzers).
  • the peak and rms values of the vibration can be determined from a PC-based software program such as Excel or Matlab.
  • the negative peak vibrations associated with the moderate speed mixer/densifer 16 are especially exacerbated when the so-called "detergent wall" is present on the inner surface of the mixer/densifier 16.
  • an optional detergent coating or wall of at least about a 1 mm can cover a portion of the inner wall surface of the moderate speed mixer/densifer 16.
  • the portion of the inner wall covered by this coating having a minimum thickness of 1 mm can be substantial (up to 100% of the inner surface covered) or a mere 50% can be covered.
  • This detergent coating provides an irregular surface contour against which the ploughs 24 are contacted during rotation of the shaft 18 of the moderate speed mixer/densifier 16. This irregular surface results in the shaft 18 being subjected to irregular forces, thereby further enhancing the overall mechanical vibration.
  • the preferred density of the resulting detergent agglomerates, or spray-dried granules of the alternative embodiment, exiting the moderate speed mixer/densifier 16 is at least 650 g/l, more preferably from about 700 g/l to about 800 g/l.
  • the particle porosity of the resulting detergent agglomerates of the composition is preferably in a range from about 5% to about 20%, more preferably at about 10%. While the detergent agglomerates or spray-dried granules exiting the moderate speed mixer/densifer 16 are ready for packaging and sale as a low dosage, compact detergent product at this point, they can be subjected to one or more optional processing steps.
  • the detergent agglomerates may be dried in a fluid bed dryer 36 or similar apparatus.
  • the detergent agglomerates exiting the fluid bed dryer 36 are further conditioned by cooling the agglomerates in a fluid bed cooler 38 or similar apparatus as are well known in the art.
  • Another optional process step involves adding a coating agent to improve flowability and/or minimize over agglomeration of the detergent composition in one or more of the following locations of the instant process: (1) the coating agent can be added directly after the fluid bed cooler 38 as shown by coating agent stream 40 (preferred); (2) the coating agent may be added between the fluid bed dryer 36 and the fluid bed cooler 38 as shown by coating agent stream 42; (3) the coating agent may be added between the fluid bed dryer 36 and the moderate speed mixer/densifier 16 as shown by stream 44; and/or (4) the coating agent may be added directly to the moderate speed mixer/densifier 16 and the fluid bed dryer 36 as shown by stream 46. It should be understood that the coating agent can be added in any one or a combination of streams 40, 42, 44, and 46 as shown in Fig. 1. The coating agent stream 40 is the most preferred in the instant process.
  • the coating agent is preferably selected from the group consisting of aluminosilicates, silicates, carbonates and mixtures thereof.
  • the coating agent not only enhances the free flowability of the resulting detergent composition which is desirable by consumers in that it permits easy scooping of detergent during use, but also serves to control agglomeration by preventing or minimizing over agglomeration, especially when added directly to the moderate speed mixer/densifier 16. As those skilled in the art are well aware, over agglomeration can lead to very undesirable flow properties and aesthetics of the final detergent product.
  • the process can comprises the step of spraying an additional binder in one or both of the mixer/densifiers 10 and 16.
  • 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.
  • suitable binder materials including those listed herein are described in Beerse et al, U.S. Patent No. 5,108,646 (Procter & Gamble Co.).
  • finishing step 50 entails finishing the resulting detergent agglomerates by a variety of processes including spraying and/or admixing other conventional detergent ingredients, collectively referenced as the finishing step 50 in Fig. 1.
  • the finishing step encompasses spraying perfumes, brighteners and enzymes onto the finished agglomerates to provide a more complete detergent composition.
  • Such techniques and ingredients are well known in the art.
  • the detergent surfactant paste used in the process is preferably in the form of an aqueous viscous paste, although forms are also contemplated by the invention.
  • 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 20% water. The viscosity is measured at 70°C and at shear rates of about 10 to 100 sec. -1 .
  • 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, in the 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.
  • 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, Murphy, issued December 16, 1980.
  • anionics and nonionics are preferred and anionics are most preferred.
  • Nonlimiting examples of the preferred anionic surfactants useful in the surfactant paste include the conventional C 11 -C 18 alkyl benzene sulfonates ("LAS"), primary, branched-chain and random C 10 -C 20 alkyl sulfates (“AS”), the C 10 -C 18 secondary (2,3) alkyl sulfates of the formula CH 3 (CH 2 ) x (CHOSO 3 - M + ) CH 3 and CH 3 (CH 2 ) y (CHOSO 3 - M + ) CH 2 CH 3 where x and (y + 1) are integers of at least about 7, preferably at least about 9, and M is a water-solubilizing cation, especially sodium, unsaturated sulfates such as oleyl sulfate, and the C 10 -C 18 alkyl alkoxy sulfates ("AE x S"; especially EO 1-7 ethoxy sulfates).
  • LAS C 11 -C 18 alkyl benz
  • exemplary surfactants useful in the paste of the invention include and C 10 -C 18 alkyl alkoxy carboxylates (especially the EO 1-5 ethoxycarboxylates), the C 10-18 glycerol ethers, the C 10 -C 18 alkyl polyglycosides and their corresponding sulfated polyglycosides, and C 12 -C 18 alpha-sulfonated fatty acid esters.
  • the conventional nonionic and amphoteric surfactants such as the C 12 -C 18 alkyl ethoxylates ("AE") including the so-called narrow peaked alkyl ethoxylates and C 6 -C 12 alkyl phenol alkoxylates (especially ethoxylates and mixed ethoxy/propoxy), C 12 -C 18 betaines and sulfobetaines ("sultaines"), C 10 -C 18 amine oxides, and the like, can also be included in the overall compositions.
  • the C 10 -C 18 N-alkyl polyhydroxy fatty acid amides can also be used. Typical examples include the C 12 -C 18 N-methylglucamides. See WO 9,206,154.
  • sugar-derived surfactants include the N-alkoxy polyhydroxy fatty acid amides, such as C 10 -C 18 N-(3-methoxypropyl) glucamide.
  • the N-propyl through N-hexyl C 12 -C 18 glucamides can be used for low sudsing.
  • C 10 -C 20 conventional soaps may also be used. If high sudsing is desired, the branched-chain C 10 -C 16 soaps may be used. Mixtures of anionic and nonionic surfactants are especially useful. Other conventional useful surfactants are listed in standard texts.
  • the starting dry detergent material of the present process preferably comprises a detergent aluminosilicate builder which are referenced as aluminosilicate ion exchange materials and sodium carbonate.
  • 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 theory, 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 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 exchange rate and capacity as provided by the sodium form.
  • the aluminosilicate ion exchange material preferably is in over dried 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 detergent builders.
  • particle size diameter represents the average particle size diameter 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 [(AlO 2 ) z .(SiO 2 ) y ]xH 2 O 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 Na 12 [(AlO 2 ) 12 .(SiO 2 ) 12 ]xH 2 O wherein x is from about 20 to about 30, preferably about 27.
  • These preferred 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 aluminosilicates used herein are further characterized by their ion exchange capacity which is at least about 200 mg equivalent of CaCO 3 hardness/gram, calculated on an anhydrous basis, and which is preferably in a range from about 300 to 352 mg equivalent of CaCO 3 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 ++ /gallon/minute/-gram/gallon to about 6 grains Ca ++ /gallon/minute/-gram/gallon.
  • the starting dry detergent material in the present process can include additional detergent ingredients and/or, any number of additional ingredients can be incorporated in the detergent composition during subsequent steps of the present process.
  • adjunct ingredients include other detergency builders, bleaches, bleach activators, suds boosters or suds suppressers, 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..
  • 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.
  • alkali metal especially sodium, salts of the above.
  • Preferred for use herein are the phosphates, carbonates, C 10-18 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 amorphous 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 O 2x+1 .yH 2 O 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 NaMSi 2 O 5 .yH 2 O wherein M is sodium or hydrogen, and y is from about 0 to about 20.
  • 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-1, 1-diphosphonic acid and the sodium and potassium salts of ethane, 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.
  • nonphosphorus, inorganic builders are tetraborate decahydrate and silicates having a weight ratio of SiO 2 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 and 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, 1967.
  • Such materials include the water-soluble salts of homo- and copolymers of aliphatic carboxylic acids such as maleic acid, itaconic acid, mesaconic acid, fumaric acid, aconitic acid, citraconic acid and methylene malonic 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.
  • These 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.
  • 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. 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 . 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..
  • 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.
  • 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.
  • This Example illustrates the process of the invention which produces free flowing, crisp, high density detergent composition.
  • Two feed streams of various detergent starting ingredients are continuously fed, at a rate of 2800 kg/hr, into a Lödige CB-30 mixer/densifier, one of which comprises a surfactant paste containing surfactant and water and the other stream containing starting dry detergent material containing aluminosilicate and sodium carbonate.
  • the rotational speed of the shaft in the Lödige CB-30 mixer/densifier is about 1400 rpm and the mean residence time is about 10 seconds.
  • the contents from the Lödige CB-30 mixer/densifer are continuously fed into a Lödige KM 600 mixer/densifer for further agglomeration during which the mean residence time is about 6 minutes.
  • the Lödige KM 600 mixer/densifier includes four tune dampers connected by a central ring.
  • the tuned dampers are located midway down the length of the mixer and are placed around the shaft in 90° intervals.
  • Each mass or weight element weighs 30 lbs. and the flexible elements in the tuned dampers are sized and tuned to about 25 Hz. All four tune dampers are then enclosed in a single cover casing.
  • the resulting detergent agglomerates are then fed to a fluid bed dryer and then to a fluid bed cooler, the mean residence time being about 10 minutes and 15 minutes, respectively.
  • a coating agent, aluminosilicate is fed about midway down the moderate speed mixer/densifier 16 to control and prevent over agglomeration.
  • the detergent agglomerates are then screened with conventional screening apparatus resulting in a uniform particle size distribution.
  • the composition of the detergent agglomerates exiting the fluid bed cooler is set forth in Table I below: Component % Weight of Total Feed C 14-15 alkyl sulfate/alkyl ethoxy sulfate 29.1
  • the density of the resulting detergent composition is 796 g/l, the mean particle size is 613 microns.
  • This Example illustrates another process in accordance with the invention in which granules are first spray dried then mixed in a moderate speed mixer/densifier.
  • the composition of the detergent in Table III below is made in a 10 foot diameter spray drying tower with counter current air at 300°C at a rate of 2800 lb/hr.
  • the granules are fed into a Lödige KM-600 with a residence time of about 12 minutes.
  • the Lödige KM 600 includes four tune dampers connected by a central ring.
  • the tuned dampers are located midway down the length of the mixer and are placed around the shaft in 90° intervals. Each mass or weight element weighs 30 lbs. and the flexible elements are sized and tuned to about 25.Hz.
  • the density of the resulting detergent composition is 822 g/l.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Detergent Compositions (AREA)
EP97935094A 1996-08-14 1997-07-30 Process for making high density detergent Expired - Lifetime EP0918843B1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US2390296P 1996-08-14 1996-08-14
US23902P 1996-08-14
PCT/US1997/012948 WO1998006816A1 (en) 1996-08-14 1997-07-30 Process for making high density detergent

Publications (2)

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EP0918843A1 EP0918843A1 (en) 1999-06-02
EP0918843B1 true EP0918843B1 (en) 2002-09-11

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EP97935094A Expired - Lifetime EP0918843B1 (en) 1996-08-14 1997-07-30 Process for making high density detergent

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EP (1) EP0918843B1 (pt)
JP (1) JP3696889B2 (pt)
CN (1) CN1120230C (pt)
AR (1) AR009078A1 (pt)
AT (1) ATE223962T1 (pt)
BR (1) BR9713167A (pt)
CA (1) CA2263748C (pt)
DE (1) DE69715428T2 (pt)
ES (1) ES2179357T3 (pt)
WO (1) WO1998006816A1 (pt)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1179030C (zh) 1998-08-20 2004-12-08 宝洁公司 包括中速混合器/密化器的制备高密度洗涤剂的方法
CN1200999C (zh) * 1999-06-21 2005-05-11 宝洁公司 制造粒状洗涤剂组合物的方法
EP1832648A1 (en) 2006-03-08 2007-09-12 Unilever Plc Laundry detergent composition and process

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE68925938T2 (de) * 1988-11-02 1996-08-08 Unilever Nv Verfahren zur Herstellung einer körnigen Reinigungsmittelzusammensetzung mit hoher Schüttdichte
GB8907187D0 (en) * 1989-03-30 1989-05-10 Unilever Plc Detergent compositions and process for preparing them
GB9008013D0 (en) * 1990-04-09 1990-06-06 Unilever Plc High bulk density granular detergent compositions and process for preparing them
US5516448A (en) * 1994-09-20 1996-05-14 The Procter & Gamble Company Process for making a high density detergent composition which includes selected recycle streams for improved agglomerate
US5554587A (en) * 1995-08-15 1996-09-10 The Procter & Gamble Company Process for making high density detergent composition using conditioned air

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WO1998006816A1 (en) 1998-02-19
DE69715428T2 (de) 2003-08-07
JP3696889B2 (ja) 2005-09-21
ATE223962T1 (de) 2002-09-15
DE69715428D1 (de) 2002-10-17
ES2179357T3 (es) 2003-01-16
CA2263748C (en) 2002-09-24
CN1232494A (zh) 1999-10-20
CN1120230C (zh) 2003-09-03
CA2263748A1 (en) 1998-02-19
JP2000500816A (ja) 2000-01-25
EP0918843A1 (en) 1999-06-02
AR009078A1 (es) 2000-03-08
BR9713167A (pt) 2000-02-01

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