JP2000507632A - Method for producing low-density detergent composition by non-tower method - Google Patents

Abstract

  (57) [Summary] Provided is a non-tower method for producing a granular detergent composition having a density of about 300 g / l to 600 g / l. The process comprises the steps of (a) (i) dispersing an aqueous or non-aqueous surfactant and (ii) interfacing with a fine powder having a diameter of 0.1 to 500 microns in a mixer operating under specific conditions. Coating the activator to obtain irregularly shaped granules and excess fines; and (b) in a mixer operating under specified conditions, the irregularly shaped granules and excess fines obtained from step (a). Spraying fine liquid onto the fine powder to bind the excess fine powder onto the irregularly shaped granules.

Description

DETAILED DESCRIPTION OF THE INVENTION                 Method for producing low-density detergent composition by non-tower method Field of the invention   The present invention generally relates to a non-tower method for producing a low density detergent composition. I do. More specifically, the present invention provides a series of mixers with surfactants and coating materials. The present invention relates to a continuous production method for producing detergent aggregates by supplying. This manufacturing method More freedom to adjust density to a wide range of consumer needs and sell commercially A flowable detergent composition is produced.                             Background of the Invention   In recent years, the detergent industry has been using “compact”, and thus low- Interest in agents is very high. Facilitates the production of these so-called low usage detergents. Detergents having a high bulk density, for example a density of 600 g / l or higher Many attempts have been made to produce. Low consumption detergents protect resources, Demand is currently high because it can be sold in small packages and is more convenient for consumers. No. However, it is not clear how modern detergent products need to be "compact". I'm not. In fact, many consumers, especially in developing countries, They prefer to use them in large quantities for washing. Agglomeration of the latest detergent compositions One of the common features of existing manufacturing methods, i.e., non-tower manufacturing, is that The apparent density of the granules produced by the process is generally at least 600 g / l . Therefore, the agglomeration technology (for example, non-tower manufacturing method) to manufacture the latest detergent composition In this regard, flexibility in the final density of the final composition, particularly low density (for example, when the density range From about 300 g / l to about 600 g / l).   In general, there are mainly three methods for producing detergent granules or powders. In the first production method, the aqueous detergent slurry is spray-dried in a spray-drying tower (For example, a tower-type production method for a low-density detergent composition). Second production In the method, the aqueous detergent slurry was spray-dried in a spray-drying tower as a first step, and the resultant was obtained. The granules are agglomerated with a binder, such as a nonionic or anionic surfactant, and Thereafter, various detergent components are dried and mixed to produce detergent granules (for example, coagulation in a tower production method). A high-density detergent composition is obtained by adding a mass production method). In the third manufacturing method, various detergent components After dry mixing the components, binders such as nonionic or anionic surfactants To produce a high-density detergent composition (for example, to obtain a high-density detergent composition). Agglomeration manufacturing method). The above three types of production methods support the density of the resulting detergent granules. Important factors to distribute are the shape, porosity and particle size distribution of the granules, and various parameters. The density of the starting materials, the shapes of the various starting materials, and their respective chemical compositions is there.   In this field, to develop manufacturing methods to increase the density of detergent granules or powders Many attempts have been made. In particular, the fineness of spray-dried granules Attention is being paid to densification. For example, in one attempt, batch production Spray-dried or granulated containing sodium phosphite and sodium sulfate Marumerizer detergent powder^RInside it is densified and spherical. This device is substantially At the bottom in a cylinder with vertical and smooth walls, a substantially horizontal, rough surface A rotatable table is arranged. However, this production method is practically batch production It is a process and therefore not very suitable for large-scale production of detergent powders. Than More recently, a series of “post-tower” or spray-dried detergent granules to increase the density Attempts have been made to provide a continuous manufacturing method. Typically, such a manufacturing method involves granulation A first device for pulverizing or pulverizing the powder and the density of the powdered granules Requires a second device to increase by agglomeration. These manufacturing methods are called "post-tower" Or by processing or densifying the spray-dried granules to increase the desired density , But without a subsequent coating step, the activity level of the Limited ability to raise Furthermore, "post-tower" processing or densification is economical Unfavorable in terms of performance (high capital cost) and operational complexity. Besides, the above All manufacturing methods are primarily directed to the processing of densified or spray-dried granules. ing. Currently, in the manufacture of detergent granules, the relative amounts of substances subjected to the spray drying process and And types are limited. For example, increasing the amount of surfactant in the resulting detergent composition Difficult to make, that is, to produce a detergent composition in a more efficient manner . Therefore, detergent compositions can be produced without the limitations imposed by conventional spray drying techniques. A possible manufacturing method is desired.   Therefore, in this industry, there are many disclosures of production methods involving aggregation of detergent compositions. example If the zeolite and / or layered silicate is mixed in a mixer, Attempts have been made to aggregate detergent builders by forming aggregates that I have. One such attempt is that detergent agglomerates can be produced using these production methods. These methods suggest that pastes, liquids and dry matter The starting detergent material in its solid form is effective for low density, brittle, free flowing detergent agglomerates. There is no mechanism that can effectively aggregate.   Therefore, in this field, the low-density detergent composition is continuously produced directly from the starting detergent component. Agglomeration produced, preferably whose density is achieved by adjusting the process conditions There is a need for a (non-tower) manufacturing method. Also, at the ultimate density of the final composition A more efficient and versatile way to produce detergents on a large scale for greater flexibility There is also a need for economical manufacturing methods.                             Background art   The following documents relate to densification of spray-dried granules. Appel et al, United States No. 5,133,924 (Lever), Bortolotti et al., US Pat. 657 (Lever), Johnson et al., British Patent No. 1,517,713 (Unilever), And Curtis, European Patent Application 451,894.   The following documents relate to the production of detergents by coagulation. Charles et al., Rice No. 4,992,079 (FMC Corporation), Beujean et al., Published WO 93 / No. 23,523 (Henkel), Beerse et al., US Pat. No. 5,108,646 (Procter  & Gamble), Capeci et al., U.S. Patent No. 5,366,652 (Procter & Gamble), Aouad et al., U.S. Patent No. 5,451,354 (Procter & Gamble), Hollingsworth Et al., European Patent Application No. 351,937 (Unilever), and Swatling et al., US Japanese Patent No. 5,205,958.   For example, in the specification of WO 93 / 23,523, pre-agglomeration is performed using a low-speed mixer. The granules having a diameter of more than 2 mm A process for producing a high-density detergent composition having less than% by weight is disclosed. This disclosure includes By adjusting the amount of liquid binder added to the second mixer, the final agglomerate Also, a production method capable of adjusting the density of is described. From this disclosure, what has led to density reduction It is not clear if they will contribute. Production as described in published WO 93 / 23,523 It will be apparent to those skilled in the art that the method differs from the invention disclosed herein.   U.S. Pat. No. 4,992,079 discloses non-ionic bleed resistance. An agglomeration method for low density non-phosphate detergents with increased water content is disclosed. First step In this case, the detergent components are agglomerated with a non-aqueous liquid surfactant. Second coagulation work following the first process In this process, particles containing a surfactant are dispersed in an inert gas medium, With a spray stream of aqueous sodium silicate or separately of water and concentrated sodium silicate To form a flocculant detergent. What contributes to low density from this disclosure It is not clear what to do. Further, this disclosure includes aqueous surfactants and phosphates. Contained detergent is not included. U.S. Pat. No. 4,992,079 The method of preparation differs from the invention disclosed herein, as will be apparent to those skilled in the art.Summary of the Invention   The present invention provides a method for producing a low-density granular detergent composition, The above-mentioned demand in the field is met. The present invention relates to coagulation (for example, non-tower type) ) Condyles for ultimate density flexibility of the final composition obtained from the manufacturing method By providing a method for producing a granular detergent composition, the above-mentioned demand can be met. is there. The proposed method of the invention provides a method of adjusting the shape of the granules, The density of the granules can be adjusted. That is, the method of the present invention has a low density. Granular detergent composition (e.g., having a density of about 300 g / l to about 600 g / l, Regular shaped granules) can be produced. This production method currently uses large amounts of surfactants. It does not use a conventional spray-drying tower whose use is limited to the production of the composition to be included. Sa Furthermore, the method of the present invention relates to various detergent compositions that can be produced by this method. Efficient, economical and flexible. Moreover, the method generally involves the use of particles Because it does not use a spray drying tower that releases particulate matter and volatile organic compounds to the atmosphere. , More favorable for environmental issues.   As used herein, the term "agglomerate" refers to the use of a raw material as a binder, such as And / or by coagulation with inorganic / organic and polymer solutions. Means the particles formed. As used herein, the term “irregular shaped granules” Formed by flocculating detergent substances, fatty acids and finely sprayed liquids Granules having an irregular shape at low density. Hundred used here All fractions are expressed as "% by weight" unless otherwise indicated.   According to one aspect of the invention, having a low density, preferably between about 300 g / l and 600 g / l The present invention provides a method for producing a granular detergent composition. The method comprises the steps of (a) (i) aqueous or non-aqueous Dispersing the aqueous surfactant, and (ii) under the following conditions: [Average residence time : About 5 to about 30 seconds, tip speed: about 5 to about 10 m / s, energy condition: about 0. 15 to about 4.20 kj / kg] in a mixer operating at 0.1 to 500 Coating the surfactant with a fine powder having a diameter of Ron to obtain granules, and then ( b) under the following conditions: [Average residence time: about 0.2 to about 5 seconds, tip speed : About 10 to about 23 m / s, energy condition: about 0.15 to about 2.9 kj / kg] In a mixer, add the finely divided liquid to the granules and excess fine powder obtained from step (a). To bind excess fine powder onto the irregularly shaped granules.   Low density, preferred, prepared by any of the manufacturing embodiments described herein. Also provided is a granular detergent composition having from about 300 g / l to about 600 g / l.   Therefore, an object of the present invention is to provide energy input, residence time conditions, Flexibility in terms of final product density by adjusting chip and chip speed The present invention provides a method for continuously producing a detergent composition. Low and high use A more efficient, versatile, and economical manufacturing method that can produce large quantities of detergent Provision is also an object of the present invention. Those skilled in the art will appreciate the details of the preferred embodiments described below. These and other aspects of the invention will be apparent from a reading of the detailed description and the appended claims. The purpose, features and advantages of will become apparent.                             BRIEF DESCRIPTION OF THE FIGURES   FIG. 1 shows the low density (about 475 g / l to 530 g / l) after the first step of the production method of the present invention. 3 is a photograph showing an irregularly shaped aggregate having the following.   FIG. 2 shows the low density (about 475 g / l- 5 is a photograph showing irregularly shaped aggregates having a weight of 500 g / l).   FIG. 3 shows the first and second steps and the drying and cooling steps of the production method of the present invention. Photo showing irregularly shaped aggregates with low density (about 450 g / l to 475 g / l) It is.   FIG. 4 shows the round shape after the aggregation step to obtain a high density (approximately 700-800 g / l). 4 is a photograph showing a state aggregate.Detailed Description of the Preferred Embodiment   The present invention relates to a method for producing at least about 300 g / l, preferably about 300 g / l to 600 g / l. The present invention relates to a method for producing a free-flowing granular detergent aggregate having a low density. . The method comprises adding an aqueous or non-aqueous surfactant to a diameter of 0.1 to 500 microns. To produce a high-density granular detergent aggregate by coating with a fine powder having the same.                                 Manufacturing method First step   In the first step of the manufacturing process, one or more of them are in powder, paste or liquid form. More aqueous or non-aqueous surfactants, and 0.1-500 microns, preferably Alternatively, a fine powder having a diameter of about 1 to about 100 microns is fed to the mixer. (Definition of surfactant and fine powder is described in detail below.)   In another embodiment of the present invention, which is described in more detail below, the surfactant may be added prior to aggregation. The first is a mixer or premixer (such as a conventional screw extruder or other (Similar mixer), and then mix the detergent material here in terms of flocculation. Into the first stage mixer described.   Generally, to achieve low densities (about 300 g / l to about 600 g / l), preferably The average residence time in the mixer is from about 5 to about 30 seconds and the tip speed of the mixer Is about 5 m / s to about 10 m / s, and the energy per unit substance in the mixer is about 0 m / s. . 15 kj / kg to about 4.20 kj / kg, more preferably the average residence time in the mixer The time is about 10 to about 15 seconds, and the tip speed of the mixer is about 6 m / s to about 8 m / s. Yes, the energy per unit material in the mixer is about 0.15 kj / kg to about 2.5 k j / kg, most preferably the average residence time in the mixer is from about 10 to about 15 seconds And the tip speed of the mixer is about 6.5 m / s to about 7.5 m / s. Is about 0.15 kj / kg to about 1.30 kj / kg.   In the example of the mixer for the first step, the mixer can maintain the conditions of the first step described above. Can be any type of mixer known to those skilled in the art. One case Is a Loedige CB mixer manufactured by Loedige (Germany). As a result of the first step, Granules with fine powder on the surface are obtained (FIG. 1).Second step   In the second step of the production process, the product obtained in the first step (granules and excess fine powder) ) To a second mixer and then spraying the particulate liquid onto the granules in the mixer You. About 0-10%, to bind the excess fines on the granules obtained from the first step, More preferably about 2-5% of a powder detergent component of the type used in the first step and And / or other detergent components can be added to the second step.   Generally, to achieve low densities (about 300 g / l to about 600 g / l), preferably The average residence time of the mixer for the second step is from about 0.2 to about 5 seconds; The tip speed of the mixer for the second step is about 10 m / s to about 23 m / s, and the mixer for the second step The energy per unit substance (energy condition) is about 0.15 kj / kg To about 2.9 kj / kg, more preferably the average residence time of the mixer is about 0.5 ~ 2 seconds, the tip speed of the mixer is about 13m / s ~ 20m / s, The energy per unit material of the sir is about 0.15 kj / kg to about 1.9 kj / kg, Most preferably, the average residence time in the mixer is from about 0.5 to about 2 seconds. The tip speed of the mixer is about 15 m / s to about 17.5 m / s, and the The energy of the fray is about 0.15 kj / kg to about 1.0 kj / kg.   In the example of the mixer for the second step, the mixer can maintain the conditions of the first step described above. Can be any type of mixer known to those skilled in the art. One case Is a Flexomic Model manufactured by Schugi (Netherlands). As a result of the first step, A detergent composition is obtained (FIG. 2).   Due to the process of the present invention, a general flocculation process known to those skilled in the art Excess recycling from the second step compared to the amount of fine powder due to The amount of fines drops surprisingly. Excessive fines create excessive circulating flow , Which hinders the process, which is economically undesirable.   According to the present invention, the recycled fine powder coming out of the second step is the fine powder used in the first step. They generally make up about 10% to 40% of the total body mass.Starting detergent substance   Surfactants for the present invention, contained in the following detergent substances, particulate liquids and The total amount of the auxiliary detergent components is based on the total amount of the final product obtained by the production method of the present invention. Generally about 5% to about 60%, more preferably about 12% to about 40%, more preferably Is about 15% to about 35%. The surfactant to be included in the above is the production method of the present invention. Of the present invention from any part of the first step or the second step, for example. It may be from both steps.Detergent surfactant (aqueous / non-aqueous)   The amount of the aqueous or non-aqueous surfactant of the present production method is obtained by the production method of the present invention. From about 5% to about 60%, more preferably from about 12% to about 40% of the total amount of the final product More preferably, from about 15% to about 35%.   The aqueous or non-aqueous process of the present process used as a starting detergent material in the first step above. The aqueous surfactant is in the form of a powder or pasted raw material.   The surfactant itself is preferably an anionic, nonionic, zwitterionic or amphoteric. And cationic surfactants and their compatible mixtures. You. Detergent surfactants useful herein are both U.S. Pat. No. 3,664,961, Norris, promulgated May 23, 1972, and U.S. Pat. No. 3,929,678, Laughlin et al., Dec. 30, 1975. Promulgation. Both useful cationic surfactants are listed here. U.S. Pat. No. 4,222,905, Cockrell, 1980. September Promulgated on the 16th, and U.S. Pat. No. 4,239,659, Murphy, 1980. The surfactants described on Dec. 16, 2016 are also included. In surfactant In the above, anionic and nonionic are preferred, and anionic is most preferred.   Non-limiting examples of preferred anionic surfactants useful in the present invention include: C₁₁~ C₁₈Alkylbenzene sulfonate ("LAS"), primary, branched and And irregular chain C_Ten~ C₂₀Alkyl sulfate ("AS"), formula           CH_Three(CH_Two)_x(CHOSO_Three ^-M⁺) CH_Threeand           CH_Three(CH_Two)_y(CHOSO_Three ^-M⁺) CH_TwoCH_Three Wherein x and (y + 1) are at least about 7, preferably at least about 9, Where M is the C of the cation that confers water solubility, especially sodium_Ten~ C₁₈Second Grade (2,3) alkyl sulfates, unsaturated sulfates such as oleyl sal Fate, and C_Ten~ C₁₈Alkyl alkoxy sulfate ("AE_xS ", In particular, EO 1-7 ethoxy sulfate).   Useful anionic surfactants include those having about 2 to 9 carbon atoms in the acyl group, 2-acyloxy-alkane-1-sulfone having from about 9 to about 23 carbon atoms in the moiety Water soluble salts of olefin sulfonates having about 12 to 24 carbon atoms, And an alkyl group having about 1 to 3 carbon atoms and an alkane moiety having about 8 to about 20 carbon atoms. Beta-alkyloxyalkanesulfonates are also included.   Optionally, other representative surfactants useful in the paste of the present invention include: C_Ten~ C₁₈Alkyl alkoxy carboxylate (especially EO 1-5 ethoxyca Ruboxylate), C_10-18Glycerol ether, C_Ten~ C₁₈Alkyl polyg Lycosides and corresponding sulfated polyglycosides, and C₁₂~ C₁₈Alphas There are rufonated fatty acid esters. Normal nonionic and amphoteric if necessary Surfactants such as C containing so-called narrow peak alkyl ethoxylates₁₂~ C₁₈ Alkyl ethoxylates ("AE") and C₆~ C₁₂Alkyl phenol Alkoxylates (especially ethoxylates and mixed ethoxy / propoxy), C_Ten ~ C₁₈Amine oxides, and others, can also be included in the overall composition. C_Ten~ C₁₈N-alkyl polyhydroxy fatty acid amides can also be used. As a representative example C₁₂~ C₁₈There is N-methylglucamide. WO 9,206,154 See the book. Surfactants derived from other sugars include N-alkoxypolyhydroxy Fatty acid amides such as C_Ten~ C₁₈N- (3-methoxypropyl) glucamide, is there. N-propyl to N-hexyl C₁₂~ C₁₈Glucamide can be used for low foaming You. C_Ten~ C₂₀Normal soap can also be used. Branching when high foaming is desired Chain C_Ten~ C₁₆Soap can be used. For anionic and nonionic surfactants Mixtures are particularly useful. Other common useful surfactants are listed in standard textbooks Have been.   Cationic surfactants can also be used as detergent surfactants and are suitable quaternary. Ammonium surfactant is Mono C₆~ C₁₆, Preferably C₆~ C_Ten, N-Al Or alkenyl ammonium surfactants, with the remaining Is substituted by a methyl, hydroxyethyl or hydroxypropyl group Have been.   Amphoteric surfactants can also be used as detergent surfactants, including heterocyclic Aliphatic derivatives of secondary and tertiary amines, aliphatic quaternary ammonium, phospholipids Zwitterionic surfactants containing derivatives of chromium and sulfonium compounds; Water-soluble salts of esters of far-sulfonated fatty acids, alkyl ether sulfates , Water-soluble salts of olefin sulfonates, beta-alkyloxyalkane sulfo Nate, formula R (R¹)_TwoN⁺R^TwoCOO^-(Where R is C₆~ C₁₈Hydrocarbyl group, good Preferably C_Ten~ C₁₆Alkyl group or C_Ten~ C₁₆An acylamidoalkyl group, Each R¹Is typically C₁~ C_ThreeAlkyl, preferably methyl,^TwoIs C₁ ~ C_FiveA hydrocarbyl group, preferably C₁~ C_ThreeAlkylene group, more Preferably C₁~ C_Two(Which is an alkylene group). Suitable solid Examples of cocoins include coconut acylamidopropyl dimethyl betaine, hexa Decyl dimethyl betaine, C_12-14Acylamidopropyl betaine, C_8-14Reed Luamidohexyl diethyl betaine, 4 [C_14-16Acylmethylamide diethyl Ammonio] -1-carboxybutane, C_16-18Acylamide dimethyl betaine , C_12-16Acylamidopentanediethylbetaine, and [C_12-16Acylmethi There is luamide dimethyl betaine. Preferred betaines are C_12-18Dimethyl ammo Niohexanoate and C_10-18Acylamide propane (or ethane) dye Chill (or diethyl) betaine, and the formula (R (R¹)_TwoN⁺R^TwoSO_Three ^-(Where R is C₆~ C₁₈Hydrocarbyl group, preferably Is C_Ten~ C₁₆An alkyl group, more preferably C₁₂~ C₁₃An alkyl group, each R¹ Is generally C₁~ C_ThreeAlkyl, preferably methyl,^TwoIs C₁~ C₆Hid Locarbyl group, preferably C₁~ C_ThreeAlkylene or preferably hydroxyal A saltine having a kylene group. An example of a suitable saltine is , C₁₂~ C₁₄Dimethylammonio-2-hydroxypropylsulfonate, C₁₂ ~ C₁₄Amidopropylammonio-2-hydroxypropylsaltine, C₁₂~ C₁₄Dihydroxyethylammoniopropanesulfonate, and C₁₆~ C₁₈The There is methylammoniohexanesulfonate, but C_12-14Amidopropylan Monio-2-hydroxypropyl saltine is preferred.Fine powder   The amount of fine powder used in the first step of the present production method is about the total amount of the starting materials in the first step. It is 94% to 30%, preferably 86% to 54%. Fine powder of this production method is More preferably, ground soda ash, powdered sodium tripolyphosphate (STP P), hydrated tripolyphosphate, ground sodium sulfate, aluminosilicate, Crystalline layered silicate, nitrilotriacetate (NTA), phosphate, precipitated silica Acid salts, polymers, carbonates, citrates, powdered surfactants (eg powdered alkanes) Sulfonic acid) and the fine powder for recycling that results from the production method of the present invention. The average diameter of the powder is between 0.1 and 500 microns, preferably between 1 and 300 microns , More preferably 5 to 100 microns. Hydrated as fine powder of the present invention When STPP is used, STPP hydrated to a level of 50% or more is preferred. This The aluminosilicate ion exchange material used as a detergent builder is Preferably, it has both a lucium ion exchange capacity and a high exchange rate. theory Is not limited to such high calcium ion exchange rates and Capacity correlates with several methods derived from the production of aluminosilicate ion exchange materials Depends on the factor. In that regard, the aluminosilicate a On-exchange materials are preferably disclosed by Corkill et al., The disclosure of which is hereby incorporated by reference. Manufactured according to U.S. Pat. No. 4,605,509 (Procter & Gamble).   The potassium and hydrogen forms of this aluminosilicate are given by the sodium form Aluminosilicate ion-exchange materials, because they do not exhibit an exchange rate as high as The "sodium" form is preferred. In addition, aluminosilicate ion exchange materials are In an overdried form to facilitate the production of the brittle detergent agglomerates described here Is preferred. The aluminosilicate ion exchange material used here is a detergent builder It is preferred to have a particle diameter that optimizes potency as a particle. Use here The term "particle diameter" refers to conventional analytical techniques, such as microscopy and scanning electron microscopy. Of a specific aluminosilicate ion exchange material, as measured by a mirror (SEM) Represents the average particle diameter. Preferred particle size diameter of aluminosilicate is about 0.1 micron About 10 microns, more preferably about 0.5 microns to about 9 microns. . Most preferably, the particle diameter is from about 1 micron to about 8 microns.   Preferably, the aluminosilicate ion exchange material has the formula:           Na_z[(AlO_Two)_z・ (SiO_Two)_y] XH_TwoO Where z and y are integers of at least 6, and the molar ratio of z to y is about 1 And x is from about 10 to about 264. More preferably, aluminosilicate The salt has the formula:           Na₁₂[(AlO_Two)₁₂・ (SiO_Two)₁₂] XH_TwoO Where x is from about 20 to about 30, preferably about 27. These preferred New aluminosilicates include, for example, zeolite A, zeolite B and zeolite It is commercially available under the number X. Alternatively, natural or suitable for use herein Synthetic aluminosilicate ion exchange materials, the disclosure of which is hereby incorporated by reference. As described in U.S. Pat. No. 3,985,669 to Krummel et al. Can be manufactured.   The aluminosilicate used here further has an ion exchange capacity measured in an anhydrous state. Calculated to have at least about 200 mg equivalents of CaCO_ThreeIt is characterized by hardness / gram And preferably about 300-352 mg equivalent of CaCO_ThreeHardness / gram. Sa In addition, the aluminosilicate ion-exchange materials have a high rate of calcium ion exchange. At least about 2 grains Ca⁺⁺/ Gallon / min / -gram / gallon, more preferred Or about 2 grains Ca⁺⁺/ Gallon / min / -gram / gallon to about 6 grains Ca⁺⁺ / Gallon / min / -gram / gallon.Particulate liquid   The amount of the particulate liquid used in the second step of the present production method depends on the production method of the present invention. About 1% to about 10% (active basis), preferably 2%, of the total amount of the final product obtained ~ 6% (active basis). The particulate liquid used in this production method is liquid silicate , Anionic or cationic surfactants in liquid form, aqueous or non-aqueous polymers It can be selected from the group consisting of solutions, water and mixtures thereof. Of the present invention Other examples of particulate liquids include sodium carboxymethyl cellulose solution. Liquid, polyethylene glycol (PEG), and dimethylenetriamine pentame Chill There is a solution of phosphonic acid (DETMP).   Of an anionic surfactant solution that can be used as a particulate liquid in the present invention. Preferred examples are about 88-97% active HLAS, about 30-50% active NaLAS, About 28% active AE3S solution, about 40-50% active liquid silicate, and others is there.   Solutions of cationic surfactants can also be used here as other liquid compositions and suitable The quaternary ammonium surfactant is mono C₆~ C₁₆, Preferably C₆~ C_Ten, N -Selected from alkyl or alkenyl ammonium surfactants, , The remaining N positions are by methyl, hydroxyethyl or hydroxypropyl groups Has been replaced.   An aqueous or non-aqueous polymer solution that can be used as a particulate liquid in the present invention A preferred example is the formula A modified polyamine comprising a polyamine skeleton corresponding to Equation V_{(n + 1)}W_mY_nHas Z, or A modified polyamine comprising a polyamine skeleton corresponding to Equation V_{(n-k + 1)}W_mY_nY '_kZ, where k is n or less, and the polyamine The backbone, prior to denaturation, has a molecular weight of greater than about 200 daltons; i) V unit is the formula Is a terminal unit having ii) W unit is the formula Is a skeleton unit having iii) Y unit is the formula A branched chain unit having iv) Z is the formulaIs a terminal unit having The R unit connecting the skeleton is C_Two~ C₁₂Alkylene, C_Four~ C₁₂Alkenylene, C_Three ~ C₁₂Hydroxyalkylene, C_Four~ C₁₂Dihydroxy-alkylene, C₈~ C₁₂ Dialkylarylene,-(R¹O)_xR¹−, − (R¹O)_XR^Five(OR¹)_X−, − (CH_TwoCH (OR^Two) CH_TwoO)_Z(R¹O)_yR¹(OCH_TwoCH (OR^Two) CH_Two)_w-, -C (O) (R^Four)_rC (O)-, -CH_TwoCH (OR^Two) CH_TwoSelected from the group consisting of-and mixtures thereof. , R¹Is C_Two~ C₆Alkylene and mixtures thereof;^TwoIs hydrogen, − (R¹O)_xB, and mixtures thereof;^ThreeIs C₁~ C₁₈Alkyl, C₇ ~ C₁₂Arylalkyl, C₇~ C₁₂Alkyl-substituted aryl, C₆~ C₁₂A Reels, and mixtures thereof, wherein R^FourIs C₁~ C₁₂Alkylene, C_Four~ C₁₂ Alkenylene, C₈~ C₁₂Arylalkylene, C₆~ C_TenArylene and its A mixture of these,^FiveIs C₁~ C₁₂Alkylene, C_Three~ C₁₂Hydroxyalkyl Ren, C_Four~ C₁₂Dihydroxy-alkylene, C₈~ C₁₂Dialkylarylene, -C (O)-, -C (O) NHR⁶NHC (O)-, -R¹(OR¹)-, -C (O) (R^Four)_rC (O)-, -CH_TwoCH (OH) CH_Two−, -CH_TwoCH (OH) CH_TwoO (R¹O)_yR¹OCH_TwoCH (OH) CH_Two−, And And mixtures thereof, R⁶Is C_Two~ C₁₂Alkylene or C₆~ C₁₂Arile And the E unit is hydrogen, C₁~ C_{twenty two}Alkyl, C_Three~ C_{twenty two}Alkenyl, C₇~ C_{twenty two}Arylalkyl, C_Two~ C_{twenty two}Hydroxyalkyl, − (CH_Two)_pCO_TwoM,-(CH_Two)_qSO_ThreeM, -CH (CH_TwoCO_TwoM) CO_TwoM,-(CH_Two)_pPO_ThreeM, − (R¹O)_XB, -C (O) R^Three, And their mixtures, oxides B is hydrogen, C₁~ C₆Alkyl,-(CH_Two)_qSO_ThreeM, − (CH_Two)_pCO_TwoM,-(CH_Two)_q(CHSO_ThreeM) CH_TwoSO_ThreeM, − (CH_Two)_q(CHSO_TwoM) CH_TwoSO_ThreeM,-(CH_Two)_pPO_ThreeM, -PO_ThreeM, and mixtures thereof, where M is hydrogen or charge balance. A water-soluble cation in an amount sufficient to add; X is a water-soluble anion; m has a value of 4 to about 400, n has a value of 0 to about 200, and p has a value of 1 to 6. Q has a value of 0-6, r has a value of 0 or 1, w is a value of 0 or 1 X has a value of 1 to 100, y has a value of 0 to 100, and z has a value of 0 or It has a value of 1. One example of the most preferred polyethyleneimine has a molecular weight of 1800 And about 7 ethyleneoxy residues per nitrogen by ethoxylation. Polyethyleneimine (PEI 1800, E7) modified to a degree of groups . The above polymer solution is prepared by pre-complexing with an anionic surfactant such as NaLAS. Preferably, it is formed.   An aqueous or non-aqueous polymer solution that can be used as a particulate liquid in the present invention Another preferred example is the polymerization of suitable unsaturated monomers, preferably in their acid form. Or dispersion of a polymeric polycarboxylic acid ester which can be produced by copolymerization Things. Unsaturation that can form suitable polymeric polycarboxylic esters by polymerization Acrylic acid, maleic acid (or maleic anhydride) is used as the acid which is a sum monomer. , Fumaric acid, itaconic acid, aconitic acid, mesaconic acid, citraconic acid and methyl There is lemmalonic acid. In the polymer polycarboxylic acid ester, vinyl methyl ether Ter, styrene, ethylene, and other carboxy-free monomer moieties are present Preferably, however, such portions should not exceed about 40% by weight.   Homopolymer polycarboxylic acid having a molecular weight exceeding 4000 as described below. Ter is preferred. A particularly suitable homopolymeric polycarboxylic acid ester is acrylic acid Can be derived from Such acrylic acid polymers useful herein are heavy polymers. It is a water-soluble salt of acrylic acid combined. The average molecular weight of such a polymer in the acid form is Preferably from 4,000 to 10,000, preferably from 4,000 to 7,000, most preferably Is also preferably 4,000 to 5,000. Water of such acrylic acid polymer Soluble salts include, for example, alkali metals, ammonium and substituted ammonium. Salts may be included.   Copolymer polyesters such as acrylic acid / maleic acid copolymers Can also be used. Such materials include copolymers of acrylic acid and maleic acid. There are water-soluble salts. The average molecular weight of such copolymers in the acid form is preferably about 2, 000-100,000, more preferably about 5,000-75,000, most preferably More preferably, it is about 7,000 to 65,000. Act on such copolymers The ratio of the lylate moiety to the maleate moiety is generally about 30: 1. To about 1: 1, more preferably from about 10: 1 to 2: 1. Such acrylic acid / Water-soluble salts of the maleic acid copolymer include, for example, alkali metals, ammonium and Substituted ammonium salts can be included. The polymer solution described above is the LAS It is preferable to form a preliminary complex with such an anionic surfactant.Supplementary detergent ingredients   The starting detergent material in the present process may include additional detergent components, and And / or any additional components may be added to the detergent composition during subsequent steps of the process. It can be incorporated into the composition. These auxiliary ingredients include other detergent builders -, Bleach, bleach activator, foam accelerator or foam inhibitor, anti-fogging agent and corrosion Inhibitor, soil suspending agent, soil release agent, bactericide, pH adjuster, non-builder alkalinity Sources, chelating agents, smectite clay, enzymes, enzyme stabilizers and fragrances You. U.S. Pat. No. 3,936,537, 1976, incorporated herein by reference. Promulgated to Baskerville, Jr. et al.   Other builders generally include various water-soluble, phosphoric, polyphosphoric, phosphonic acids , Polyphosphonic acid, carbonic acid, boric acid, polyhydroxysulfonic acid, polyacetic acid, cal Alkali metals, ammonium and substituted ammonic acids of boric acid and polycarboxylic acids Can be selected from the group consisting of: Alkali metal salts mentioned above, especially sodium salts Is preferred. For use here, phosphates, carbonates, C_10-18Fatty acids, poly Carboxylates, and mixtures thereof, are preferred. Sodium tripolyphosphate, Pi Tetrasodium lophosphate, citrate, mono- and di-succinate tartrate, and And mixtures thereof (see below) are more preferred.   Compared to amorphous sodium silicate, crystalline layered sodium silicate And magnesium ion exchange capacity is clearly large. In addition, layered sodium silicate Thorium prefers magnesium ions to calcium ions because of This is a necessary feature to ensure that virtually all "hardness" is removed from the material. However , These crystalline layered sodium silicates are compatible with amorphous silicates and other builders. -More expensive than Therefore, to produce economically useful laundry detergents, The proportion of crystalline layered sodium silicate used must be carefully determined.   Crystalline layered sodium silicate suitable for use herein preferably comprises the following formula: Have.           NaMSi_xO_{2x + 1}・ YH_TwoO Wherein M is sodium or hydrogen, x is from about 1.9 to about 4, y is from about 0 to about 20. More preferably, the crystalline layered sodium silicate has the following formula: Having.           NaMSi_TwoO_Five・ YH_TwoO Wherein M is sodium or hydrogen and y is from about 0 to about 20. This These and other crystalline layered sodium silicates are already incorporated herein by reference. Corkill et al., In U.S. Pat. No. 4,605,509.   Specific examples of the inorganic phosphate builder include tripolyphosphoric acid, pyrophosphoric acid, and a polymerization degree of about Polymer metaphosphoric acid which is 6-21, and sodium and potassium orthophosphoric acid Um salt. An example of a polyphosphonate builder is the ethylene diphosphonic acid nato Lithium and potassium salts, nato of ethane 1-hydroxy-1,1-diphosphonic acid Lithium and potassium salts, and sodium ethane, 1,1,2-triphosphonic acid And potassium salts. All other phosphorus builder compounds are referenced here U.S. Pat. Nos. 3,159,581, 3,213,030, 3rd , 422,021, 3,422,137, 3,400,176 and No. 3,400,148.   Examples of non-phosphorous inorganic builders are tetraborate decahydrate, and SiO 2_TwoAnd al The weight ratio of potassium metal oxide is about 0.5 to about 4.0, preferably about 1.0 to about 2.4. Is a silicate. Here, useful water-soluble non-phosphorus organic builders , Various polyacetic acids, carboxylic acids, polycarboxylic acids and polyhydroxy sulfones There are alkali metal, ammonium and substituted ammonium salts of acids. Polyacetate And examples of polycarboxylate builders are ethylenediaminetetraacetic acid, nitrile Rotriacetic acid, oxysuccinic acid, melitic acid, benzene polycarboxylic acid and que Sodium, potassium, lithium, ammonium and substituted ammonium acids Salt.   The polymeric polycarboxylate builder is a rice brewer whose disclosure is incorporated herein by reference. No. 3,308,067, Diehl, promulgated March 7, 1967. It is listed. Such substances include aliphatic carboxylic acids such as maleic acid, Conic, mesaconic, fumaric, aconitic, citraconic and methylene There are water-soluble salts of homopolymers and copolymers of lonic acid. Some of these substances Is useful as a water-soluble anionic polymer described below, but is a non-soap anionic polymer. Only when sufficiently mixed with the ON-based surfactant.   Other polycarboxylates suitable for use herein are both incorporated herein by reference. U.S. Pat. No. 4,144,226, issued Mar. 13, 1979 to Crut. issued to Chfield et al., and US Pat. No. 4,246,495, 1979 Polyacetal carboxyl, promulgated to Crutchfield et al. On March 27 Acid salt. These polyacetal carboxylates can be used as glyoxylic acid esters. Can be prepared by placing the polymer under polymerization conditions together with a polymerization initiator. Next The resulting polyacetal carboxylic acid ester to a chemically stable end group. To rapidly depolymerize polyacetal carboxylate in alkaline solution And converted to the corresponding salt and added to the detergent composition. Especially preferred Polycarboxylate builders are disclosed in U.S. Pat. No. 4,663,071, described in Bush et al., Issued May 5, 1987. A combination comprising a combination of monosuccinate tartrate and disuccinate tartrate Tercarboxylate builder.   Bleaching agents and activators are described in U.S. Pat. No. 2,934, issued to Chung et al., Nov. 1, 1983, and U.S. Pat. No. 4,483,781, Hartman, promulgated on November 20, 1984. Have been. Chelating agents are also incorporated by reference in US Pat. No. 71, Bush et al., Column 17, line 54 to column 18, line 68. You. Foaming improvers are also components used as needed, and both are referred to here. U.S. Patent No. 3,933,672, Bart on January 20, 1976. oletta, and 4,136,045, Jan. 23, 1979 Promulgated in Gault et al.   Smectite clay suitable for use here is a rice smectite included here by reference. No. 4,762,645, Tucker et al., Promulgated August 9, 1988, Column 6, line 3 to column 7, line 24. Additions suitable for use here Additional detergent builders are available from Baskerville's patents, both of which are incorporated herein by reference. Detail, column 13, line 54 to column 16, line 16, and U.S. Pat. No. 71, Bush et al., Issued May 5, 1987.   For comparison with the present invention, a series of mixers operating under different conditions from the present invention FIG. 4 shows a photograph of the high-density aggregate (average density of about 700 to 800 g / l) obtained by the above method. You. Referring to FIG. 4, Loedige CB mixer (operating at CB-30, 550 RPM), then Schugi Flexomic mixer (operated at 2800 RPM) and finally Loedige KM mixer (K M-600, running at 100 RPM on a regular plow) was used for the agglomeration. Aggregate shown in FIG. The substances used to obtain are the same as in Example 2 described in detail in "Examples".                         Manufacturing processes performed as needed   Required for reducing the water content in the aggregate obtained from the second step Is a drying step. This is well known to those skilled in the art. This can be achieved by various types of devices. Fluid bed equipment is preferred. In the description below, it is called a dryer.   Another optional step of the process involves the detergent coming out of the fluid bed dryer. The agglomerates are further conditioned by additional cooling in a cooling device. Preferred equipment Is a fluidized bed. Another optional step improves the flowability of the detergent composition And / or to minimize excessive agglomeration, one or more of the following Add coating at more locations. That is, (1) the coating agent is a fluidized bed cooling device Or (2) the coating can be added to the fluidized bed dryer and (3) Coatings, which can be added between moving bed cooling devices, are well known in the art. Between the fluidized bed dryer and the medium speed mixer for agglomeration, commonly known to the trader. And / or (4) coatings may be applied in this field and in fluid bed drying. Directly into a medium speed mixer for agglomeration, generally known to those skilled in the art of dryers. Can be added. The coating is preferably aluminosilicate, silicate, carbonate Selected from the group consisting of salts, and mixtures thereof. Coating agent is used during cleaning Of the resulting detergent composition, which is preferred by consumers because it can be easily scooped Not only does it enhance free-flowing properties, but especially when added directly to a medium speed mixer, Preventing or minimizing clumping also helps control aggregation. As is well known to those skilled in the art, over-agglomeration can lead to flow properties and The appearance can be greatly impaired.   Optionally, the method may comprise one or both of the first and second mixers of the present invention. Or additional fluid bed dryer and / or fluid bed cooler A step of fogging may be included. The binder may be a "binding" or a Added to enhance cohesion by providing a "sticky" agent. The binder is Water, anionic surfactants, nonionic surfactants, liquid silicates, polyethylene Glycol, polyvinylpyrrolidone polyacrylate, citric acid and the like Is preferably selected from the group consisting of: The binders listed here Other suitable binders, including those disclosed herein by reference, Beerse et al., No. 5,108,646 (Procter & Gamble Co.). You.   Other optional steps that may be considered in this method include screening There is a step of screening for detergent aggregates that are too large in the cleaning device. This device An example of a conventional screen selected to obtain the desired particle size of the final detergent product However, the present invention is not limited to this. other If necessary, the agglomerate is further dried using the above-mentioned apparatus. To control the detergent agglomerates.   Another optional step in this process involves spraying other conventional detergent ingredients. Finishing the resulting detergent agglomerates by various treatments, including and / or mixing There is a process. For example, the finishing process involves the addition of fragrance, brightener and And spraying the enzyme to a more complete detergent composition. Such technology and The ingredients are well known in the art.   The method for producing a granular detergent composition by the production method of the present invention and, if necessary, A representative example of a series of mixers for the same process is shown below. A. (1) Aggregation with Loedige CB Model-(2) Then with Schugi Flexomic Model-- (3) Sizing in a Mogensens sizing machine to remove particles larger than 4.5 mm -(4) Drying in fluidized bed dryer-(5) Cooling in fluidized bed cooler-(6 ) Sizing in a Mogensen sizing machine to remove particles larger than 1.2 mm-(7 ) Grinding to reduce excess size agglomerates coming from the sizer-and (8) Pulverized agglomerate is fluidized bed dryer or fluidized bed cooler or Loedige CB mixer Return to B. (1) Aggregation with Loedige CB Model-(2) Then with Loedige KM Model-(3) Furthermore, with the Schugi Flexomic Model-(4) to remove particles larger than 4.5 mm In a Mogensens sizing apparatus for cultivation-(5) Drying in a fluidized bed dryer-(6) Cooling in a fluidized bed cooler-(7) Mo to remove particles larger than 1.2 mm Sizing in gensen sizer-(8) Reduce excess size agglomerates coming from sizer Milling to reduce-and (9) fluidizing the milled agglomerates in a fluid bed drier or Return to floor cooler or Loedige CB mixer.   Another essential step in the process involves a highly active paste structuring step. For example, before the production method of the present invention, using an extruder to compound the paste-cured substance This cures the anionic surfactant paste. Highly active paste structure Details of the conversion process are described in Related Application No. 1 filed on the same day as the present invention. JA162F specification (Submitted October 4, 1996).   The following examples are provided for a better understanding of the present invention, but these examples are for illustration only. It does not limit the scope.                                   An example Example 1 (irregular shaped aggregate after the first step of the present invention)   Loedige CB mixer (CB-30), followed by fluid bed dryer (FBD), fluid bed cooler An example for producing an agglomerate using sizing (FBC) followed by sizing and grinding. Shown below.   Aqueous coconut fatty alcohol sulfate with pin tool of CB-30 mixer 259 kg / hr of surfactant paste (71.5% active ingredient) 217 kg / hr of average particle size 40-75 microns, finely ground soda ash (average particle size 5 169 kg / hr, finely ground sulfate (average particle size 5-30 micron) Ron) 103 kg / hr, and 288 kg / hr of fine powder for recycle use. interface The activator paste is supplied at about 40-55 ° C and the powder is supplied at room temperature. CB-30 Miki The conditions of the sir are as follows.     Average residence time: 14-20 seconds     Chip speed: 6.5-7.0m / s     Energy conditions: 0.15 to 1.0 kj / kg   After the coagulation, the bed temperature of the FBD is maintained at 40 to 60 ° C., Maintain at 0 ° C.   The resulting granules have a density of 475-530 g / l (FIG. 1). After CB-30 mixer The amount of fine powder is 30 to 50% against the target of 25%.Example 2 (irregular shaped aggregate after first and second steps of the invention)   Loedige CB mixer (CB-30), then Schugi Flexomic mixer, then fluid bed Using a dryer (FBD), fluidized bed cooler (FBC), then sizing and grinding An example for producing agglomerates by means of (after agglomeration with Loedige CB mixer) Except for the addition of coagulation with a Schugi Flexomic mixer, Same as Example 1).   The aggregate obtained from the CB-30 mixer is fed to a Schugi Flexomic mixer. HLA S30 kg / hr is atomized and sprayed into a Schugi Flexomic mixer. Schugi mixer The conditions of the following are as follows.     Average residence time: 0.5-2 seconds     Tip speed: 15-18m / s     Energy conditions: 0.15 to 1.0 kj / kg   The granules obtained after the Schugi mixer have a density of 475-500 g / l (FIG. 2). , Granules obtained after sizing and grinding have a density of 450-475 g / l (FIG. 3) . The amount of fine powder obtained from the Schugi Flexomic mixer is 22-30%.Example 3 (irregular shaped aggregate obtained by the production method of the present invention)   Loedige CB mixer (CB-30), then Schugi Flexomic mixer, then fluid bed Refrigerator (FBC) for producing agglomerates using sizing and grinding An example is shown below. Non-aqueous linear alkylbenzene by pin tool of CB-30 mixer Sulfonic acid (94-96% active ingredient) 220 kg / hr, powder STPP (average particle size) 300kg / hr, finely ground soda ash (average particle size 5-30) Micron) 230kg / hr, finely ground sulfate (average particle size 5-30 microns) 100 kg / hr, zeolite 90 kg / hr and recycle fine powder 100 kg / hr Sprinkle. The surfactant is supplied at about 40-55 ° C and the powder is supplied at room temperature. CB-3 0 The conditions of the mixer are as follows.     Average residence time: 10-18 seconds     Chip speed: 6-13m / s     Energy conditions: 0.15 to 3.5 kj / kg   The aggregate obtained from the CB-30 mixer is fed to a Schugl Flexomic mixer. HLA S30kg / hr is atomized and sprayed into a Schugi Flexomic mixer, carbonate 20kg / h Add r to Schugi mixer. The conditions of the Schugi mixer are as follows.     Average residence time: 0.5-2 seconds     Tip speed: 15-18m / s     Energy conditions: 0.15 to 1.0 kj / kg   Granules obtained after Schugi mixer and after sizing and grinding have a density of 500-5 It is 50 g / l.Example 4 (irregular shaped aggregate obtained by the production method of the present invention)   Loedige CB mixer (CB-30), then Loedige KM mixer (KM-600) and Schug i Flexomic mixer, followed by fluidized bed cooler (FBC), then sizing and grinding An example for producing an agglomerate using is shown below.   Non-aqueous linear alkyl benzene sulfonate by pin tool of CB-30 mixer (94 to 96% active ingredient) 220 kg / hr was added to powder STPP (average particle size 40 to 7). 5 micron) 300 kg / hr, finely ground soda ash (average particle size 5 to 30 micron) 2 30 kg / hr, finely ground sulfate (average particle size 5 to 30 microns) 100 kg / hr, It is dispersed together with 90 kg / hr of zeolite and 100 kg / hr of fine powder for circulation. interface The activator is provided at about 40-55 ° C and the powder is provided at room temperature. Article of CB-30 mixer The matter is as follows.     Average residence time: 10-18 seconds     Chip speed: 6-13m / s     Energy conditions: 0.15 to 3.5 kj / kg   Agglomerate obtained from the CB-30 mixer is put into a KM mixer holding about 40-60 kg. It is. The plow RPM is 100 and the chopper RPM is 1300 (three chips on the mixer). There is a chopper). The aggregate obtained from the KM mixer has a density of 750 to 80 It is 0 g / l.   The aggregate obtained from the KM mixer is supplied to a Schugi Flexomic (FX-160) mixer. You. HLAS 30 kg / hr is atomized, sprayed into a Schugi Flexomic mixer, and carbonated. Add 20 kg / hr of salt to the Schugi mixer. The conditions of the Schugi mixer are as follows is there.     Average residence time: 0.5-2 seconds     Tip speed: 15-18m / s     Energy conditions: 0.15 to 1.0 kj / kg   Granules obtained after Schugi mixer and after sizing and grinding have a density of about 600 g / l.   While the present invention has been described in detail, it will be apparent to those skilled in the art that Various modifications are possible without departing from the invention, and the invention is described in the written description. The content is not limited.

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Claims (1)

[Claims]   1. Granules having a density of about 300 g / l to 600 g / l, comprising the steps of: Non-tower method for producing a detergent composition. (A) (i) disperse an aqueous or non-aqueous surfactant, and (ii) operate under the following conditions: Surfactant in a fine powder having a diameter of 0.1 to 500 microns in a mixer Step of obtaining granules by coating [Average residence time: about 5 to about 30 seconds,   Chip speed: about 5 to about 10 m / s,   Energy conditions: about 0.15 to about 4.2 kj / kg] and (B) in a mixer operating under the following conditions, the granules obtained from step (a) and The fine liquid is sprayed on the excess fine powder, and the excess fine powder is formed on irregularly shaped granules. The process of combining. [Average residence time: about 0.2 to about 5 seconds,   Tip speed: about 10 to about 23 m / s,   Energy conditions: about 0.15 to about 2.9 kj / kg]   2. The surfactant may be an anionic surfactant, a nonionic surfactant, or a cation surfactant. Choose from ionic surfactants, zwitterionics, amphoteric, and mixtures thereof. The method of claim 1, wherein the method is selected.   3. The surfactant is an alkyl benzene sulfonate or an alkyl alkoxide. Cisulfate, alkyl ethoxylate, alkyl sulfate, coconut Selected from the group consisting of fatty alcohol sulfates and mixtures thereof, The method of claim 1.   4. Aqueous or non-aqueous polymer solution in step (a) (i) with said surfactant 2. The method of claim 1, wherein the method is distributed.   5. The fine powder is soda ash, powdered sodium tripolyphosphate, Lipolyphosphate, sodium sulfate, aluminosilicate, crystalline layered silicate, Silicate, precipitated silicate, polymer, carbonate, citrate, nitrilotriacetate (NTA), powdered surfactant, recycled fine powder obtained from step (b) The method of claim 1, wherein the method is selected from the group consisting of: and mixtures thereof.   6. Fine liquids include liquid silicates, anionic surfactants, and cationic From surfactants, aqueous polymer solutions, non-aqueous polymer solutions, water and mixtures thereof The method of claim 1, wherein the method is selected from the group consisting of:   7. The average residence time of the detergent agglomerates in the mixer of step (a) is from about 10 seconds to about For 15 seconds, the tip speed of the detergent aggregates in the mixer of step (a) is from about 6 m / s to about 8 m / s, and the energy condition of the mixer of step (a) ranges from about 0.15 kj / kg to 2. The method of claim 1, wherein said method is about 2.5 kj / kg.   8. The average residence time of the detergent agglomerates in the mixer of step (b) is from about 0.5 seconds to For about 2 seconds, the tip speed of the detergent aggregates in the mixer of step (b) is from about 13 m / s to about 13 m / s. 20 m / s, and the energy range of the mixer in step (b) is about 0.15 kj / 6. The method of claim 5, wherein the weight is from about kg to about 1.9 kj / kg.   9. Recycled fine powder obtained from step (b) in the total amount of fine powder of step (a) 2. The method of claim 1, wherein the total body mass is from about 10% to about 40%.   10. The fine powder is STPP hydrated to a level of at least 50%, The method of claim 1.   11. The total amount of the surfactant for the production method of claim 1 is The method of claim 1, wherein the amount is from about 5% to about 60% of the total amount of the resulting composition.   12. A granular detergent composition produced by the method according to claim 1.