WO1998014552A1 - Procede de production d'une composition detergente sans l'utilisation d'une tour - Google Patents

Procede de production d'une composition detergente sans l'utilisation d'une tour Download PDF

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Publication number
WO1998014552A1
WO1998014552A1 PCT/US1997/009790 US9709790W WO9814552A1 WO 1998014552 A1 WO1998014552 A1 WO 1998014552A1 US 9709790 W US9709790 W US 9709790W WO 9814552 A1 WO9814552 A1 WO 9814552A1
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WIPO (PCT)
Prior art keywords
surfactant
detergent
mixer
process according
mixtures
Prior art date
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PCT/US1997/009790
Other languages
English (en)
Inventor
Wayne Edward Beimesch
Original Assignee
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 DE69726439T priority Critical patent/DE69726439T2/de
Priority to CA002268068A priority patent/CA2268068C/fr
Priority to AT97928872T priority patent/ATE255159T1/de
Priority to EP97928872A priority patent/EP0929649B1/fr
Priority to US09/269,856 priority patent/US6211138B1/en
Priority to BR9711865A priority patent/BR9711865A/pt
Priority to JP51649098A priority patent/JP3299982B2/ja
Priority to AU33031/97A priority patent/AU3303197A/en
Publication of WO1998014552A1 publication Critical patent/WO1998014552A1/fr

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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
    • 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
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • 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
    • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
    • C11D11/02—Preparation in the form of powder by spray drying
    • 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
    • C11D17/0039—Coated compositions or coated components in the compositions, (micro)capsules
    • 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
    • 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
    • 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
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02—Anionic compounds
    • C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
    • C11D1/146—Sulfuric acid esters
    • 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
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02—Anionic compounds
    • C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/22—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
    • 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
    • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02—Anionic compounds
    • C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/29—Sulfates of polyoxyalkylene ethers

Definitions

  • the present invention generally relates to a non-tower process for producing a particulate detergent composition. More particularly, the invention is directed to a continuous process during which detergent agglomerates are produced by feeding a surfactant and coating materials into a series of mixers. The process produces a free flowing, detergent composition whose density can be adjusted for wide range of consumer needs, and which can be commercially sold.
  • the first type of process involves spray- drying an aqueous detergent slurry in a spray-drying tower to produce highly porous detergent granules (e.g., tower process for low density detergent compositions).
  • the various detergent components are dry mixed after which they are agglomerated with a binder such as a nonionic or anionic surfactant, to produce high density detergent compositions (e.g., agglomeration process for high density detergent compositions).
  • the important factors which govern the density of the resulting detergent granules are the shape, porosity and particle size distribution of said granules, the density of the various starting materials, the shape of the various starting materials, and their respective chemical composition.
  • This apparatus comprises a substantially horizontal, roughened, rotatable table positioned within and at the base of a substantially vertical, smooth walled cylinder.
  • This process is essentially a batch process and is therefore less suitable for the large scale production of detergent powders.
  • non-tower process for continuously producing a detergent composition having high density delivered directly from starting detergent ingredients, and preferably the density can be achieved by adjusting the process condition. Also, there remains a need for such a process which is more efficient, flexible and economical to facilitate large-scale production of detergents (1) for flexibility in the ultimate density of the final composition, and (2) for flexibility in terms of incorporating several different kinds of detergent ingredients, especially detergent ingredients in the form of liquid, into the process.
  • Laid Open No.WO96/04359 (Unilever).
  • Laid-open No.WO93/23,523 (Henkel) describes the process comprising pre-agglomeration by a low speed mixer and further agglomeration step by high speed mixer for obtaining high density detergent composition with less than 25 wt% of the granules having a diameter over 2 mm.
  • the U.S. Patent No. 4,427,417 (Korex) describes continuous process for agglomeration which reduces caking and oversized agglomerates.
  • the present invention meets the aforementioned needs in the art by providing a process which produces a high density granular detergent composition.
  • the present invention also meets the aforementioned needs in the art by providing a process which produces a granular detergent composition for flexibility in the ultimate density of the final composition from agglomeration (e.g., non-tower) process.
  • the process does not use the conventional spray drying towers currently which is limited in producing high surfactant loading compositions.
  • the process of the present invention is more efficient, economical and flexible with regard to the variety of detergent compositions which can be produced in the process.
  • the process is more amenable to environmental concerns in that it does not use spray drying towers which typically emit particulates and volatile organic compounds into the atmosphere.
  • agglomerates refers to particles formed by agglomerating raw materials with binder such as surfactants and or inorganic solutions / organic solvents and polymer solutions.
  • binder such as surfactants and or inorganic solutions / organic solvents and polymer solutions.
  • a process for preparing a granular detergent composition having a density at least about 600 g/1 is provided.
  • the process comprises the steps of:
  • the granular detergent compositions having a high density of at least about 600g/l produced by any one of the process embodiments described herein. Accordingly, it is an object of the invention to provide a process for continuously producing a detergent composition which has flexibility with respect to density of the final products by controlling energy input, residence time condition, and tip speed condition in the mixers. It is also an object of the invention to provide a process which is more efficient, flexible and economical to facilitate large-scale production.
  • the present invention is directed to a process which produces free flowing, granular detergent agglomerates having a density of at least about 600 g/1.
  • the process produces granular detergent agglomerates from an aqueous and/or non-aqueous surfactant which is then coated with fine powder having a diameter from 0.1 to 500 microns, in order to obtain low density granules.
  • aqueous and/or non- aqueous surfactant(s) which is/are in the form of powder, paste and/or liquid, and fine powder having a diameter from 0.1 to 500 microns, preferably from about 1 to about 100 microns are fed into a mixer, so as to make agglomerates.
  • surface of the surfactant which is coated by the fine powder is wet by finely atomized liquid so as to add more fine powder on the surface of the agglomerates.
  • an internal recycle stream of powder having a diameter of about 0.1 to about 300 microns generated in the fluidizing apparatus can be fed into the mixer in addition to the fine powder.
  • the amount of such internal recycle stream of powder can be 0 to about 60 wt% of final product.
  • the surfactant for the first step can be initially fed into a mixer or pre-mixer (e.g. a conventional screw extruder or other similar mixer) prior to the above, after which the mixed detergent materials are fed into the first step mixer as described herein for agglomeration.
  • a mixer or pre-mixer e.g. a conventional screw extruder or other similar mixer
  • the mean residence time of the mixer is in range from about 0.2 to about 5 seconds and tip speed of the mixer of the mixer is in range from about 10 m/s to about 30 m/s
  • the energy per unit mass of the mixer (energy condition) of the mixer is in range from about 0.15 kj/kg to about 5 kj/kg
  • the mean residence time of the mixer is in range from about 0.2 to about 5 seconds and tip speed of the mixer is in range from about 10 m/s to about 30 m/s
  • the energy per unit mass of the mixer (energy condition) is in range from about 0.15 kj/kg to about 5 kj/kg
  • the most preferably, the mean residence time of the mixer is in range from about 0.2 to about 5 seconds
  • tip speed of the mixer is in range from about 15 m/s to about 26 m/s
  • the energy per unit mass of the mixer (energy condition) is from about 0.2 kj/kg to about 3 kj/kg.
  • the examples of the mixer can be any types of
  • the agglomerates from the first step are fed into a fluidized apparatus, such as fluidized bed, in order to enhance granulation for producing free flowing high density granules.
  • the second step can proceed in one or more than one fluidized apparatus (e.g., combining different kinds of fluidized apparatus such as fluid bed dryer and fluid bed cooler).
  • the resultant product from the second step is fluidized thoroughly so that the granules from the second step have a round shape.
  • about 0 to about 10% , more preferably about 2-5% of powder detergent materials of the kind used in the first step and/or other detergent ingredients can be added to the second step.
  • condition of a fluidized apparatus can be; Mean residence time : from about 1 to about 10 minutes Depth of unfluidized bed : from about 100 to about 300 mm Droplet spray size : not more than about 50 micron Spray height: from about 175 to about 250 mm
  • Fluidizing velocity from about 0.2 to about 1.4 m/s Bed temperature : from about 12 to about 100 °C, more preferably; Mean residence time : from about 2 to about 6 minutes Depth of unfluidized bed : from about 100 to about 250 mm Droplet spray size : less than about 50 micron Spray height: from about 175 to about 200 mm Fluidizing velocity : from about 0.3 to about 1.0 m/s Bed temperature : from about 12 to about 80 °C. If two different kinds of fluidized apparatus would be used, mean residence time of the third step in total can be from about 2 to about 20 minutes, more preferably, from about 2 to 12 minutes.
  • a coating agent to improve flowability and/or minimize over agglomeration of the detergent composition can be added in one or more of the following locations of the instant process: (1) the coating agent can be added directly after fluid bed cooler or fluid bed dryer; (2) the coating agent may be added between fluid bed dryer and fluid bed cooler; and/or (3) the coating agent may be added directly to the fluid bed dryer.
  • 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 for detergent during use, but also serves to control agglomeration by preventing or minimizing over agglomeration. 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 total amount of the surfactants in products made by the present invention, which are included in the following detergent materials, finely atomized liquid and adjunct detergent ingredients is generally from about 5% to about
  • the surfactants which are included in the above can be from any part of the process of the present invention., e.g., from either one of the first step and/or the second step of the present invention.
  • the amount of the surfactant of the present process can be from about 5% to about 60%, more preferably from about 12% to about 40%, more preferably, from about 15 to about 35%, in total amount of the final product obtained by the process of the present invention.
  • the surfactant of the present process which is used as the above mentioned starting detergent materials in the first step, is in the form of powdered, pasted or liquid raw materials.
  • the surfactant itself is preferably selected from anionic, nonionic, zwittehonic, 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 3,929,678, 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 present invention include the conventional C11-C18 alkyl benzene sulfonates ("LAS"), primary, branched-chain and random C10-C20 a ' k y' sulfates (“AS”), the C10-C18 secondary (2,3) alkyl sulfates of the formula CH3(CH2) x (CHOSO3 " M + ) CH3 and CH3 (CH2)y(CHOSO3 ' M + ) CH2CH3 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 C10- 18 alk y' a'koxy sulfates ("AE X S"; especially EO 1-7 ethoxy sulfates).
  • LAS C11-C18 alkyl benzene s
  • Useful anionic surfactants also include water-soluble salts of 2-acyloxy- alkane-1-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 sulfonates containing from about 12 to 24 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 .
  • exemplary surfactants useful in the paste of the invention include C10-C18 a'kyl alkoxy carboxylates (especially the EO 1-5 ethoxycarboxylates), the glycerol ethers, the C ⁇
  • the conventional nonionic and amphoteric surfactants such as the C-12-C18 alkyl ethoxylates ("AE") including the so-called narrow peaked alkyl ethoxylates and C6-C12 alkyl phenol alkoxylates (especially ethoxylates and mixed ethoxy/propoxy), C-JQ-CI S amine oxides, and the like, can also be included in the overall compositions.
  • AE C-12-C18 alkyl ethoxylates
  • C6-C12 alkyl phenol alkoxylates especially ethoxylates and mixed ethoxy/propoxy
  • C-JQ-CI S amine oxides and the like
  • 8 N-alkyl polyhydroxy fatty acid amides can also be used. Typical examples include the C-12-C18 N-methylglucamides. See WO 9,206,154.
  • sugar- derived surfactants include the N-alkoxy polyhydroxy fatty acid amides, such as C10-C 8 N-(3-methoxypropyl) glucamide.
  • the N-propyl through N-hexyl C12- C18 glucamides can be used for low sudsing.
  • C10-C20 conventional soaps may also be used. If high sudsing is desired, the branched-chain C ⁇ ⁇ o-C-
  • Cationic surfactants can also be used as a detergent surfactant herein and suitable quaternary ammonium surfactants are selected from mono C6-C16. preferably C6-C10 N-alkyl or alkenyl ammonium surfactants wherein remaining N positions are substituted by methyl, hydroxyethyl or hydroxypropyl groups.
  • Ampholytic surfactants can also be used as a detergent surfactant herein, which include aliphatic derivatives of heterocyclic secondary and tertiary amines; zwitterionic surfactants which include derivatives of aliphatic quaternary ammonium, phosphonium and sulfonium compounds; water-soluble salts of esters of alpha-sulfonated fatty acids; alkyl ether sulfates; water-soluble salts of olefin sulfonates; beta-alkyloxy alkane sulfonates; betaines having the formula R(Rl)2N + R 2 COO ** , wherein R is a C6-C18 hydrocarbyl group, preferably a C10- C16 alkyl group or C10-CI6 acylamido alkyl group, each R 1 is typically C1-C3 alkyl, preferably methyl and R2 is a C1-C5 hydrocarbyl group, preferably a C
  • betaines examples include coconut acylamidopropyldimethyl betaine; hexadecyl dimethyl betaine; C12-I4 acylamidopropylbetaine; C8-14 acylamidohexyldiethyl betaine; 4[C1 -16 acylmethylamidodiethylammonio]-1-carboxybutane; C16-I8 acylamidodimethylbetaine; C12-I6 acylamidopentanediethylbetaine; and [C12-16 acylmethylamidodimethylbetaine.
  • Preferred betaines are C12-I8 dimethyl-ammonio hexanoate and the C10-I8 acylamidopropane (or ethane) dimethyl (or diethyl) betaines; and the sultaines having the formula (R(R 1 )2N + R2SO3 _ wherein R is a C6-C18 hydrocarbyl group, preferably a C10- C16 alkyl group, more preferably a C12-C13 alkyl group, each R 1 is typically C-
  • Suitable sultaines include C12-C14 dimethylammonio-2-hydroxypropyl sulfonate, C12- C14 amido propyl ammonio-2-hydroxypropyl sultaine, C12-C14 dihydroxyethylammonio propane sulfonate, and C-J6-18 dimethylammonio hexane sulfonate, with C 12-14 amido propyl ammonio-2-hydroxypropyl sultaine being preferred. Fine Powder
  • the amount of the fine powder of the present process, which is used in the first step, can be from about 94% to 30%, preferably from 86% to 54%, in total amount of starting material for the first step .
  • the starting fine powder of the present process preferably selected from the group consisting of ground soda ash, powdered sodium tripolyphosphate (STPP), hydrated tripolyphosphate, ground sodium sulphates, aluminosilicates, crystalline layered silicates, nithlotriacetates (NTA), phosphates, precipitated silicates, polymers, carbonates, citrates, powdered surfactants (such as powdered alkane sulfonic acids) and internal recycle stream of powder occurring from the process of the present invention, wherein the average diameter of the powder is from 0.1 to 500 microns, preferably from 1 to 300 microns, more preferably from 5 to 100 microns.
  • 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. In that regard, 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 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 [(AIO 2 ) z .(SiO 2 )y]xH2 ⁇ 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 [(AIO 2 )i2.(Si0 2 )i2]xH2 ⁇ 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.
  • 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 CaCO3 hardness/gram, calculated on an anhydrous basis, and which is preferably in a range from about 300 to 352 mg equivalent of CaCO3 hardness/gram.
  • 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 amount of the finely atomized liquid of the present process can be from about 1 % to about 10% (active basis), preferably from 2% to about 6% (active basis) in total amount of the final product obtained by the process of the present invention.
  • the finely atomized liquid of the present process can be selected from the group consisting of liquid silicate, anionic or cationic surfactants which are in liquid form, aqueous or non-aqueous polymer solutions, water and mixtures thereof.
  • Other optional examples for the finely atomized liquid of the present invention can be sodium carboxy methyl cellulose solution, polyethylene glycol (PEG), and solutions of dimethylene triamine pentamethyl phosphonic acid (DETMP),
  • anionic surfactant solutions which can be used as the finely atomized liquid in the present inventions are about 88 - 97% active HLAS, about 30 - 50% active NaLAS, about 28% active AE3S solution, about 40-50% active liquid silicate, and so on.
  • Cationic surfactants can also be used as finely atomized liquid herein and suitable quaternary ammonium surfactants are selected from mono C6-C16, preferably C6-C10 N-alkyl or alkenyl ammonium surfactants wherein remaining N positions are substituted by methyl, hydroxyethyl or hydroxypropyl groups.
  • aqueous or non-aqueous polymer solutions which can be used as the finely atomized liquid in the present inventions are modified polyamines which comprise a polyamine backbone corresponding to the formula: having a modified polyamine formula V( n+ ⁇ nW m Y n Z or a polyamine backbone corresponding to the formula:
  • polyamine backbone prior to modification having a modified polyamine formula V( n _k+i)W m Y n Y'kZ, wherein k is less than or equal to n, said polyamine backbone prior to modification has a molecular weight greater than about 200 daltons, wherein
  • V units are terminal units having the formula:
  • W units are backbone units having the formula:
  • Y units are branching units having the formula:
  • Z units are terminal units having the formula: X "
  • backbone linking R units are selected from the group consisting of C2- C ⁇
  • R1 is C2- C6 alkylene and mixtures thereof
  • R 2 is hydrogen, -(R 1 O) x B, and mixtures thereof
  • R 3 is C---C18 alkyl, C7-C12 arylalkyi, C7-C12 al yl substituted aryl, C ⁇ - C12 aryl, and mixtures thereof
  • R 4 is C-j-C-
  • R5 is C1-C-12 alkylene, C3-C12 hydroxyalkylene, C4-C12 dihydroxy-alkylene, C8-C12 dialkylarylene, -C(O)-, -C(O)NHR6NHC(O)-, -R1(0
  • polyethyleneimines a polyethyleneimine having a molecular weight of 1800 which is further modified by ethoxylation to a degree of approximately 7 ethyleneoxy residues per nitrogen (PEI 1800, E7). It is preferable for the above polymer solution to be pre-complex with anionic surfactant such as NaLAS.
  • anionic surfactant such as NaLAS.
  • polymeric polycarboxylate dispersants which can be prepared by polymerizing or copolymerizing suitable unsaturated monomers, preferably in their acid form.
  • Unsaturated monomeric acids that can be polymerized to form suitable polymeric polycarboxylates include acrylic acid, maleic acid (or maleic anhydride), fumaric acid, itaconic acid, aconitic acid, mesaconic acid, citraconic acid and methylenemalonic acid.
  • the presence in the polymeric polycarboxylates herein of monomeric segments, containing no carboxylate radicals such as vinylmethyl ether, styrene, ethylene, etc. is suitable provided that such segments do not constitute more than about 40% by weight of the polymer.
  • Homo-polymeric polycarboxylates which have molecular weights above
  • Particularly suitable homo- polymeric polycarboxylates can be derived from acrylic acid.
  • acrylic acid- based polymers which are useful herein are the water-soluble salts of polymerized acrylic acid.
  • the average molecular weight of such polymers in the acid form preferably ranges from above 4,000 to 10,000, preferably from above 4,000 to 7,000, and most preferably from above 4,000 to 5,000.
  • Water-soluble salts of such acrylic acid polymers can include, for example, the alkali metal, ammonium and substituted ammonium salts.
  • Co-polymeric polycarboxylates such as a Acrylic/maleic-based copolymers may also be used.
  • Such materials include the water-soluble salts of copolymers of acrylic acid and maleic acid.
  • the average molecular weight of such copolymers in the acid form preferably ranges from about 2,000 to 100,000, more preferably from about 5,000 to 75,000, most preferably from about 7,000 to 65,000.
  • the ratio of acrylate to maleate segments in such copolymers will generally range from about 30:1 to about 1 :1 , more preferably from about 10:1 to 2:1.
  • Water-soluble salts of such acrylic acid/maieic acid copolymers can include, for example, the alkali metal, ammonium and substituted ammonium salts. It is preferable for the above polymer solution to be pre-complexed with anionic surfactant such as LAS .
  • the starting 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 suppressors, antitarnish 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, C- * rj-l8 f attv 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. Such crystalline layered sodium silicates are discussed in Corkill et al, U.S. Patent No. 4,605,509, previously incorporated herein by reference.
  • 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 S ⁇ 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 condition an ester of glyoxyiic 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.
  • the process can comprise the step of spraying an additional binder in one or more than one of the first, second and/or the third mixers for the present invention.
  • 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, liquid silicates, 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.
  • Another optional step of the instant process entails finishing the resulting detergent agglomerates by a variety of processes including spraying and/or admixing other conventional detergent ingredients.
  • 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.
  • surfactant paste structuring process e.g., hardening an aqueous anionic surfactant paste by incorporating a paste-hardening material by using an extruder, prior to the process of the present invention.
  • surfactant paste structuring process e.g., hardening an aqueous anionic surfactant paste by incorporating a paste-hardening material by using an extruder.
  • the details of the surfactant paste structuring process are disclosed co-application No. PCT/US96/15960 (filed October 4, 1996) .
  • Step 1 120 - 160 kg/hr of HLAS (an acid precursor of C ⁇ ⁇
  • the surfactant is fed at about 50 to 60 °C, and the powders are fed at room temperature.
  • HLAS an acid precursor of C-
  • HLAS an acid precursor of C-
  • Step 2 The agglomerates from the Schugi mixer are fed to a fluid bed drying apparatus for drying, rounding and growth of agglomerates. 20 - 80 kg/hr of liquid silicate (43% solids, 2.0 R) can be also added in the fluid bed drying apparatus at 35°C.
  • the condition of the fluid bed drying apparatus is as follows:
  • Spray height 175 - 250 mm (above distributor plate)
  • Bed temperature 40 - 70 °C
  • the resultant from the step 2 has a density of about 600g/l, and can be optionally subjected to the optional process of cooling, sizing and/or grinding.
  • Step 1 120 - 160 kg/hr of HLAS (an acid precursor of C «
  • the condition of the Schugi mixer is as follows:
  • Step 2 The agglomerates from the Schugi mixer are fed to a fluid bed drying apparatus for drying, rounding and growth of agglomerates. 20 - 80 kg/hr of liquid silicate (43% solids, 2.0 R) can be also added in the fluid bed drying apparatus at 35°C. The condition of the fluid bed drying apparatus is as follows: Mean residence time : 2- 4 minutes
  • Spray height 175 - 250 mm (above distributor plate)
  • Fluidizing velocity 0.4 - 0.8 m/s
  • Bed temperature 40 - 70 °C
  • Step 3 The resultant from the fluid bed drying apparatus is fed to a fluid bed cooling apparatus. 5 - 10 kg/hr of liquid silicate (43% solids, 2.0 R) is added to the apparatus.
  • the condition of the fluid bed cooling apparatus is as follows: Mean residence time : 2- 4 minutes
  • the resultant from the step 3 has a density of about 600 g/l, and can be optionally subjected to the optional process of sizing an/or grinding.

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  • Engineering & Computer Science (AREA)
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Abstract

Cette invention se rapporte à un procédé n'utilisant pas de tour et servant à préparer en continu une composition détergente granulaire ayant une densité d'au moins 600 g/l environ. Ce procédé consiste: (a) à disperser un tensioactif et à revêtir ce tensioactif d'une fine poudre ayant un diamètre compris entre 0,1 et 500 microns, tout en mouillant le tensioactif revêtu de cette fine poudre avec un liquide finement atomisé dans un mélangeur, et (b) à réduire ces agglomérats en granulés dans un ou plusieurs appareils de fluidisation.
PCT/US1997/009790 1996-10-04 1997-06-05 Procede de production d'une composition detergente sans l'utilisation d'une tour WO1998014552A1 (fr)

Priority Applications (8)

Application Number Priority Date Filing Date Title
DE69726439T DE69726439T2 (de) 1996-10-04 1997-06-05 Verfahren zur herstellung von einer waschmittelzusammensetzung nach ohne-turm-verfahren
CA002268068A CA2268068C (fr) 1996-10-04 1997-06-05 Procede de production d'une composition detergente sans l'utilisation d'une tour
AT97928872T ATE255159T1 (de) 1996-10-04 1997-06-05 Verfahren zur herstellung von einer waschmittelzusammensetzung nach ohne-turm- verfahren
EP97928872A EP0929649B1 (fr) 1996-10-04 1997-06-05 Procede de production d'une composition detergente sans l'utilisation d'une tour
US09/269,856 US6211138B1 (en) 1996-10-04 1997-06-05 Process for making a detergent composition by non-tower process
BR9711865A BR9711865A (pt) 1996-10-04 1997-06-05 Processo para fabricar uma composi-Æo detergente por um processo sem utiliza-Æo de torre
JP51649098A JP3299982B2 (ja) 1996-10-04 1997-06-05 非タワープロセスによる洗剤組成物の製造方法
AU33031/97A AU3303197A (en) 1996-10-04 1997-06-05 Process for making a detergent composition by non-tower process

Applications Claiming Priority (2)

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PCT/US1996/015881 WO1998014549A1 (fr) 1996-10-04 1996-10-04 Procede de production d'une composition de detergent de faible densite par un processus sans colonne
ALPCT/US96/15881 1996-10-04

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WO1998014552A1 true WO1998014552A1 (fr) 1998-04-09

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PCT/US1997/009795 WO1998014557A1 (fr) 1996-01-05 1997-06-05 Procede de production d'une composition detergente sans l'utilisation d'une tour
PCT/US1997/009789 WO1998014551A1 (fr) 1996-10-04 1997-06-05 Procede de production d'une composition detergente sans l'utilisation d'une tour
PCT/US1997/009791 WO1998014553A1 (fr) 1996-10-04 1997-06-05 Procede de production d'une composition detergente sans l'utilisation d'une tour
PCT/US1997/009793 WO1998014555A1 (fr) 1996-01-05 1997-06-05 Procede de production d'une composition detergente sans l'utilisation d'une tour
PCT/US1997/009792 WO1998014554A1 (fr) 1996-10-04 1997-06-05 Procede de production d'une composition detergente sans l'utilisation d'une tour
PCT/US1997/009790 WO1998014552A1 (fr) 1996-10-04 1997-06-05 Procede de production d'une composition detergente sans l'utilisation d'une tour
PCT/US1997/009796 WO1998014558A1 (fr) 1996-10-04 1997-06-05 Procede de production d'une composition detergente sans l'utilisation d'une tour
PCT/US1997/009794 WO1998014556A1 (fr) 1996-10-04 1997-06-05 Procede de production d'une composition detergente sans l'utilisation d'une tour

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PCT/US1997/009795 WO1998014557A1 (fr) 1996-01-05 1997-06-05 Procede de production d'une composition detergente sans l'utilisation d'une tour
PCT/US1997/009789 WO1998014551A1 (fr) 1996-10-04 1997-06-05 Procede de production d'une composition detergente sans l'utilisation d'une tour
PCT/US1997/009791 WO1998014553A1 (fr) 1996-10-04 1997-06-05 Procede de production d'une composition detergente sans l'utilisation d'une tour
PCT/US1997/009793 WO1998014555A1 (fr) 1996-01-05 1997-06-05 Procede de production d'une composition detergente sans l'utilisation d'une tour
PCT/US1997/009792 WO1998014554A1 (fr) 1996-10-04 1997-06-05 Procede de production d'une composition detergente sans l'utilisation d'une tour

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PCT/US1997/009794 WO1998014556A1 (fr) 1996-10-04 1997-06-05 Procede de production d'une composition detergente sans l'utilisation d'une tour

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US6056905A (en) * 1997-06-16 2000-05-02 Lever Brothers Company Division Of Conopco, Inc. Production of detergent granulates
US6077820A (en) * 1995-12-20 2000-06-20 Lever Brothers Company Division Of Conopco, Inc. Process for preparing a granular detergent
US6133223A (en) * 1997-06-27 2000-10-17 Lever Brothers Company, Division Of Conopco, Inc. Production of detergent granulates
US6258773B1 (en) 1997-07-14 2001-07-10 The Procter & Gamble Company Process for making a low density detergent composition by controlling agglomeration via particle size
US6274544B1 (en) 1997-06-16 2001-08-14 Lever Brothers Company, Division Of Conopco, Inc. Production of detergent granulates
US6355606B1 (en) 1997-07-14 2002-03-12 The Procter & Gamble Company Process for making a low density detergent composition by controlled agglomeration in a fluid bed dryer
US6423679B1 (en) 1997-07-15 2002-07-23 The Procter & Gamble Company Process for making high-active detergent agglomerates by multi-stage surfactant paste injection
US6440342B1 (en) 1998-07-08 2002-08-27 The Procter & Gamble Company Process for making a low density detergent composition by controlling nozzle height in a fluid bed dryer
US6455490B1 (en) 1999-06-10 2002-09-24 Unilever Home & Personal Care Usa Division Of Conopco, In.C Granular detergent component containing zeolite map and laundry detergent compositions
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
US6555514B1 (en) 1998-10-26 2003-04-29 The Procter & Gamble Company Processes for making granular detergent composition having improved appearance and solubility
US11655436B2 (en) 2018-01-26 2023-05-23 Ecolab Usa Inc. Solidifying liquid amine oxide, betaine, and/or sultaine surfactants with a binder and optional carrier

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WO1996031510A1 (fr) * 1995-04-03 1996-10-10 Novartis Ag Derives de pyrazole et leurs procedes de preparation
US6794354B1 (en) * 1998-09-18 2004-09-21 The Procter & Gamble Company Continuous process for making detergent composition
GB9825558D0 (en) * 1998-11-20 1999-01-13 Unilever Plc Granular detergent components and particulate detergent compositions containing them
US6894018B1 (en) 1999-06-21 2005-05-17 The Procter & Gamble Company Process for making granular detergent in a fluidized bed granulator having recycling of improperly sized particles
GB0009877D0 (en) † 2000-04-20 2000-06-07 Unilever Plc Granular detergent component and process for its preparation
EP2123742A1 (fr) 2008-05-14 2009-11-25 The Procter and Gamble Company Compositions de détergent solide pour lessive comprenant du sel de silicate à faible densité
WO2011061045A1 (fr) 2009-11-20 2011-05-26 Unilever Nv Granulé de détergent et son procédé de fabrication
EP3140386B1 (fr) 2014-04-10 2024-02-28 The Procter & Gamble Company Granulés de détergent composites et compositions de lavage du linge comprenant ces derniers
CN111655828A (zh) 2018-01-26 2020-09-11 埃科莱布美国股份有限公司 用载体固化液体氧化胺、甜菜碱和/或磺基甜菜碱表面活性剂
CA3167784A1 (fr) 2018-01-26 2019-08-01 Ecolab Usa Inc. Tensioactifs anioniques liquides solidifiants

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Publication number Priority date Publication date Assignee Title
US6077820A (en) * 1995-12-20 2000-06-20 Lever Brothers Company Division Of Conopco, Inc. Process for preparing a granular detergent
US6056905A (en) * 1997-06-16 2000-05-02 Lever Brothers Company Division Of Conopco, Inc. Production of detergent granulates
US6274544B1 (en) 1997-06-16 2001-08-14 Lever Brothers Company, Division Of Conopco, Inc. Production of detergent granulates
US6429184B1 (en) 1997-06-16 2002-08-06 Lever & Brothers Company, Division Of Conopco, Inc. Production of detergent granulates
US6133223A (en) * 1997-06-27 2000-10-17 Lever Brothers Company, Division Of Conopco, Inc. Production of detergent granulates
US6258773B1 (en) 1997-07-14 2001-07-10 The Procter & Gamble Company Process for making a low density detergent composition by controlling agglomeration via particle size
US6355606B1 (en) 1997-07-14 2002-03-12 The Procter & Gamble Company Process for making a low density detergent composition by controlled agglomeration in a fluid bed dryer
US6423679B1 (en) 1997-07-15 2002-07-23 The Procter & Gamble Company Process for making high-active detergent agglomerates by multi-stage surfactant paste injection
US6440342B1 (en) 1998-07-08 2002-08-27 The Procter & Gamble Company Process for making a low density detergent composition by controlling nozzle height in a fluid bed dryer
US6492319B1 (en) 1998-08-20 2002-12-10 The Procter & Gamble Company High density detergent-making process involving a moderate speed mixer/densifier
US6555514B1 (en) 1998-10-26 2003-04-29 The Procter & Gamble Company Processes for making granular detergent composition having improved appearance and solubility
US6784151B2 (en) * 1998-10-26 2004-08-31 The Procter & Gamble Company Processes for making granular detergent composition having improved appearance and solubility
US6455490B1 (en) 1999-06-10 2002-09-24 Unilever Home & Personal Care Usa Division Of Conopco, In.C Granular detergent component containing zeolite map and laundry detergent compositions
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
US11655436B2 (en) 2018-01-26 2023-05-23 Ecolab Usa Inc. Solidifying liquid amine oxide, betaine, and/or sultaine surfactants with a binder and optional carrier
US11976255B2 (en) 2018-01-26 2024-05-07 Ecolab Usa Inc. Solidifying liquid amine oxide, betaine, and/or sultaine surfactants with a binder and optional carrier

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CA2268068A1 (fr) 1998-04-09
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CN1156561C (zh) 2004-07-07
AU3378597A (en) 1998-04-24
AR010508A1 (es) 2000-06-28
CN1239991A (zh) 1999-12-29
JP3345022B2 (ja) 2002-11-18
WO1998014557A1 (fr) 1998-04-09
CN1156560C (zh) 2004-07-07
CA2267424A1 (fr) 1998-04-09
AU3568397A (en) 1998-04-24
CA2268055C (fr) 2004-02-03
EP0929655A1 (fr) 1999-07-21
JP2000503719A (ja) 2000-03-28
JP3299985B2 (ja) 2002-07-08
MX219076B (en) 2004-02-10
EP0929650A1 (fr) 1999-07-21
CA2268068C (fr) 2003-06-03
ATE238409T1 (de) 2003-05-15
CN1156563C (zh) 2004-07-07
JP3299986B2 (ja) 2002-07-08
JP3305327B2 (ja) 2002-07-22
CA2268062A1 (fr) 1998-04-09
CA2268055A1 (fr) 1998-04-09
ES2201305T3 (es) 2004-03-16
BR9712490A (pt) 1999-10-19
ES2178778T3 (es) 2003-01-01
AR010729A1 (es) 2000-07-12
CN1239992A (zh) 1999-12-29
AU3478597A (en) 1998-04-24
EP0929653A1 (fr) 1999-07-21
EP0929651B1 (fr) 2003-11-26
CN1239508A (zh) 1999-12-22
CN1239993A (zh) 1999-12-29
WO1998014554A1 (fr) 1998-04-09
BR9712492A (pt) 1999-10-19
BR9713246A (pt) 1999-11-03
DE69721287D1 (de) 2003-05-28
EP0929649A1 (fr) 1999-07-21
JP2000503717A (ja) 2000-03-28
CN1156562C (zh) 2004-07-07
DE69723986D1 (de) 2003-09-11
DE69726439T2 (de) 2004-09-09
JP3299984B2 (ja) 2002-07-08
DE69715224D1 (de) 2002-10-10
WO1998014553A1 (fr) 1998-04-09
CA2268052C (fr) 2003-12-30
AU3478397A (en) 1998-04-24
JP2000503718A (ja) 2000-03-28
EP0929648B1 (fr) 2002-09-04
JP2000503715A (ja) 2000-03-28
EP0929649B1 (fr) 2003-11-26
WO1998014556A1 (fr) 1998-04-09
CN1239995A (zh) 1999-12-29
CA2267424C (fr) 2004-01-06
JP2000504062A (ja) 2000-04-04
DE69726440D1 (de) 2004-01-08
EP0929648A1 (fr) 1999-07-21
EP0929652A1 (fr) 1999-07-21
JP2000507632A (ja) 2000-06-20
AU3303197A (en) 1998-04-24
CA2268060A1 (fr) 1998-04-09

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