WO1998006816A1 - Procede de fabrication d'un detergent haute densite - Google Patents

Procede de fabrication d'un detergent haute densite Download PDF

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Publication number
WO1998006816A1
WO1998006816A1 PCT/US1997/012948 US9712948W WO9806816A1 WO 1998006816 A1 WO1998006816 A1 WO 1998006816A1 US 9712948 W US9712948 W US 9712948W WO 9806816 A1 WO9806816 A1 WO 9806816A1
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WIPO (PCT)
Prior art keywords
detergent
densifier
speed mixer
shaft
agglomerates
Prior art date
Application number
PCT/US1997/012948
Other languages
English (en)
Inventor
Paul Anthony Zaffiro
William Garrett Halvorsen
Scott William Capeci
Antonio Williams
Larry Vincent Dalton
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The Procter & Gamble Company
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 The Procter & Gamble Company filed Critical The Procter & Gamble Company
Priority to AT97935094T priority Critical patent/ATE223962T1/de
Priority to CA002263748A priority patent/CA2263748C/fr
Priority to EP97935094A priority patent/EP0918843B1/fr
Priority to JP50973998A priority patent/JP3696889B2/ja
Priority to DE69715428T priority patent/DE69715428T2/de
Priority to BR9713167-9A priority patent/BR9713167A/pt
Publication of WO1998006816A1 publication Critical patent/WO1998006816A1/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
    • C11D11/0082—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); Hoilingsworth 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 documents are incorporated herein by reference. 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: (a) continuously mixing a detergent surfactant paste and dry starting detergent material into a high speed mixer/densifier to obtain detergent agglomerates; (b) mixing the detergent agglomerates in a moderate speed mixer/densifier to further density and agglomerate the detergent agglomerates, wherein the moderate 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 -LOG to about LOG in a frequency range of from about 10 Hz to about 20 Hz at the mid-span length of the shaft; and (c) drying the detergent agglomerates so as to form the detergent composition.
  • 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.OG to about 1.OG 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.
  • Fig. 1 is a flow chart illustrating a preferred process in which two mixer/densifiers, a fluid bed dryer, a fluid bed cooler and screening apparatus are serially positioned in accordance with a highly preferred embodiment of the invention
  • Fig. 2 is a perspective partial cut-away view of a mixer/densifier used in accordance with the process which illustrates the tuned damper mounted on the centrally rotating shaft;
  • Fig. 3 is a side cross-sectional view of the centrally rotating shaft having a tuned damper mounted thereon;
  • Fig. 4 is an end view of the rotating shaft in the moderate speed mixer/densifier illustrating the tuned damper with four damping apparatus mounted about the shaft via connecting bars and clamps.
  • 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 L ⁇ dige 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 ixer/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 L ⁇ dige 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. L ⁇ dige KM (Ploughshare) mixer).
  • the moderate speed mixer/densifer 16 e.g. L ⁇ dige 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 - OG to about LOG, 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.
  • the presence of this detergent coating provides an irregular surface contour against which the ploughs 24 are contacted during rotation of the shaft 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/1, more preferably from about 700 g/1 to about 800 g/1.
  • 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.
  • 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.), the disclosure of which is incorporated herein by reference.
  • 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.'L
  • 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, 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, Murphy, issued December 16, 1980, both of which are also incorporated herein by reference.
  • 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 Cj j-C j alkyl benzene sulfonates ("LAS"), primary, branched-chain and random C 10-C20 alky ] sulfates (“AS”), the Ci Q-Ci secondary (2,3) alkyl sulfates of the formula CH 3 (CH2) x (CHOS0 " M + ) CH3 and CH3 (CH 2 ) y (CHOS0 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 Cjo-C j g alkyl alkoxy sulfates ("AE X S”; especially EO 1-7 ethoxy sulfates).
  • LAS Cj j-C j alkyl
  • exemplary surfactants useful in the paste of the invention include and Cjo-C j alkyl alkoxy carboxylates (especially the EO 1-5 ethoxycarboxylates), the C
  • the conventional nonionic and amphoteric surfactants such as the C ⁇ -Cjg alkyl ethoxylates ("AE") including the so-called narrow peaked alkyl ethoxylates and Cg-Ci 2 alkyl phenol alkoxylates (especially ethoxylates and mixed ethoxy/propoxy), C t ⁇ -Cjg betaines and sulfobetaines ("sultaines"), C
  • Q-C]g amine oxides, and the like, can also be included in the overall compositions.
  • the C J Q- Cjg N-alkyl polyhydroxy fatty acid amides can also be used. Typical examples include the Ci2-C ] g N-methylglucamides.
  • sugar-derived surfactants include the N-alkoxy polyhydroxy fatty acid amides, such as Ci ⁇ -Ci N-(3-methoxypropyl) glucamide.
  • the N-propyl through N-hexyl C12-C1 g glucamides can be used for low sudsing.
  • C10-C20 conventional soaps may also be used. If high sudsing is desired, the branched-chain C10-C1 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 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 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
  • the aluminosilicate has the formula
  • 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 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 CaC0 3 hardness/gram, calculated on an anhydrous basis, and which is preferably in a range from about 300 to 352 mg equivalent of CaC0 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/-grarn/gallon to about 6 grains Ca ++ /gaIlon 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., 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.
  • alkali metal especially sodium, salts of the above.
  • Preferred for use herein are the phosphates, carbonates, Cjo-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
  • the crystalline layered sodium silicate has the formula
  • NaMS.2O5.yH2O 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, 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 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, 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, 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.
  • polyacetal carboxylates 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.
  • These polyacetal carboxylates can be prepared by bringing together under polymerization conditions an ester of glyoxylic acid and a polymerization initiator. The resulting polyacetal carboxyiate 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.
  • Cheiating 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 Baskervilie 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 composition.
  • Two feed streams of various detergent starting ingredients are continuously fed, at a rate of 2800 kg/hr, into a L ⁇ dige 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 L ⁇ dige CB-30 mixer/densifier is about 1400 rpm and the mean residence time is about 10 seconds.
  • the contents from the L ⁇ dige CB-30 mixer/densifer are continuously fed into a L ⁇ dige KM 600 mixer/densifer for further agglomeration during which the mean residence time is about 6 minutes.
  • the L ⁇ dige 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:
  • Polyethylene glycol (MW 4000) 1.3
  • the density of the resulting detergent composition is 796 g/1, the mean particle size is 613 microns.
  • EXAMPLE II 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 HI 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 L ⁇ dige KM-600 with a residence time of about 12 minutes.
  • the L ⁇ dige 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. All four tune dampers are then enclosed in a single cover casing.

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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)

Abstract

L'invention concerne un procédé pour produire des compositions détergentes haute densité. Ce procédé est un procédé continu permettant de produire des agglomérats de détergent haute densité. Ce procédé consiste à placer une pâte tensioactive et un produit de départ détergent sec dans un mélangeur/densificateur. Ce dernier possède un arbre de rotation, placé en son centre, dont les vibrations sont maintenues à une valeur minimale par des amortisseurs synchronisés fixés sur cet arbre. Ce procédé permet d'obtenir une composition détergente haute densité, s'écoulant librement, qui peut être commercialisée comme composition détergente 'compacte' ou à faible dosage.
PCT/US1997/012948 1996-08-14 1997-07-30 Procede de fabrication d'un detergent haute densite WO1998006816A1 (fr)

Priority Applications (6)

Application Number Priority Date Filing Date Title
AT97935094T ATE223962T1 (de) 1996-08-14 1997-07-30 Verfahren zur herstellung von waschmitteln mit hoher dichte
CA002263748A CA2263748C (fr) 1996-08-14 1997-07-30 Procede de fabrication d'un detergent haute densite
EP97935094A EP0918843B1 (fr) 1996-08-14 1997-07-30 Procede de fabrication d'un detergent haute densite
JP50973998A JP3696889B2 (ja) 1996-08-14 1997-07-30 高密度洗剤を製造するためのプロセス
DE69715428T DE69715428T2 (de) 1996-08-14 1997-07-30 Verfahren zur herstellung von waschmitteln mit hoher dichte
BR9713167-9A BR9713167A (pt) 1996-08-14 1997-07-30 Processo para a fabricação de detergente de alta densidade.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US2390296P 1996-08-14 1996-08-14
US60/023,902 1996-08-14

Publications (1)

Publication Number Publication Date
WO1998006816A1 true WO1998006816A1 (fr) 1998-02-19

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Application Number Title Priority Date Filing Date
PCT/US1997/012948 WO1998006816A1 (fr) 1996-08-14 1997-07-30 Procede de fabrication d'un detergent haute densite

Country Status (10)

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

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000011131A1 (fr) * 1998-08-20 2000-03-02 The Procter & Gamble Company Procede de fabrication de detergent haute densite comportant un melangeur/densificateur a vitesse moderee
JP2003503548A (ja) * 1999-06-21 2003-01-28 ザ、プロクター、エンド、ギャンブル、カンパニー 顆粒洗剤組成物の製造方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1832648A1 (fr) 2006-03-08 2007-09-12 Unilever Plc Composition de détergent à lessive et procédé

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0451894A1 (fr) * 1990-04-09 1991-10-16 Unilever N.V. Compositions détergentes granulaires à haute densité apparente et leur procédé de préparation
US5133924A (en) * 1988-11-02 1992-07-28 Lever Brothers Company Process for preparing a high bulk density granular detergent composition
US5160657A (en) * 1989-03-17 1992-11-03 Lever Brothers Company, Division Of Conopo, Inc. 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

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5133924A (en) * 1988-11-02 1992-07-28 Lever Brothers Company Process for preparing a high bulk density granular detergent composition
US5160657A (en) * 1989-03-17 1992-11-03 Lever Brothers Company, Division Of Conopo, Inc. Detergent compositions and process for preparing them
EP0451894A1 (fr) * 1990-04-09 1991-10-16 Unilever N.V. Compositions détergentes granulaires à haute densité apparente et leur procédé de préparation
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

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000011131A1 (fr) * 1998-08-20 2000-03-02 The Procter & Gamble Company Procede de fabrication de detergent haute densite comportant un melangeur/densificateur a vitesse moderee
US6492319B1 (en) 1998-08-20 2002-12-10 The Procter & Gamble Company High density detergent-making process involving a moderate speed mixer/densifier
JP2003503548A (ja) * 1999-06-21 2003-01-28 ザ、プロクター、エンド、ギャンブル、カンパニー 顆粒洗剤組成物の製造方法
JP4786092B2 (ja) * 1999-06-21 2011-10-05 ザ プロクター アンド ギャンブル カンパニー 顆粒洗剤組成物の製造方法

Also Published As

Publication number Publication date
CA2263748C (fr) 2002-09-24
CA2263748A1 (fr) 1998-02-19
ATE223962T1 (de) 2002-09-15
EP0918843A1 (fr) 1999-06-02
CN1120230C (zh) 2003-09-03
BR9713167A (pt) 2000-02-01
DE69715428D1 (de) 2002-10-17
AR009078A1 (es) 2000-03-08
ES2179357T3 (es) 2003-01-16
DE69715428T2 (de) 2003-08-07
JP3696889B2 (ja) 2005-09-21
CN1232494A (zh) 1999-10-20
JP2000500816A (ja) 2000-01-25
EP0918843B1 (fr) 2002-09-11

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