JP2000503715A - Method for producing detergent composition by non-tower process - Google Patents

Abstract

  (57) [Summary] A non-tower process is provided for continuously producing a granular detergent composition having a density of at least about 600 g / l. The process comprises: (a) dispersing the surfactant in a mixer, coating the surfactant with a fine powder having a diameter of 0.1-500 microns, and (b) agglomerating with one or more flow devices. Granulation. The process may further include step (a ') between step (a) and step (b), i.e., spraying the fine spray onto the first agglomerate with a mixer.

Description

DETAILED DESCRIPTION OF THE INVENTION                 Method for producing detergent composition by non-tower process                               Field of the invention   The present invention generally relates to a non-tower process for producing a particulate detergent composition. I do. More specifically, the present invention relates to detergent aggregates It relates to a continuous process produced by feeding quality into a series of mixers. The process requires that the density be tailored to a wide range of consumer needs and be marketed. To produce a free flowing detergent composition.                               Background of the Invention   In recent years, the detergent industry has been focusing on laundry detergents that are "compact" and require low usage. There is considerable interest within. Facilitate the production of these so-called low usage detergents Many attempts have been made to produce high bulk density detergents, e.g. I have been. Low usage detergents are currently in high demand because they conserve resources , Can be sold in small packages that are more convenient for consumers. However In fact, the degree to which current detergent products need to be “compact” remains to be determined. Up to. In fact, many consumers have their own laundry operations, especially in developing countries. And continue to favor higher usage levels.   Usually, there are two main types of processes in which detergent granules or powders are manufactured. . In the first type of process, sponges are used to produce highly porous detergent granules. Spray dry the aqueous detergent slurry in a laye drying tower (eg, low density detergent Composition tower process). In the second type of process, various detergent ingredients are dried. Once immiscible, they are nonionic to produce a high-density detergent composition Or aggregated with a binder such as an anionic surfactant (eg, a high density detergent set Product agglomeration process). The density of the resulting detergent granules in the above two processes Important factors influencing the shape, porosity and particle size distribution of the granules Starting material densities, various starting material shapes, and their respective chemical compositions.   Many attempts have been made in the industry to provide a process for increasing the density of detergent granules or powders. Has been done in Special attention must be paid to the fineness of the spray-dried granules by post-tower processing. It has been paid for densification. For example, one attempt is to use sodium tripolyphosphate and And a batch process for densification and spheroidization. This device is substantially vertical Substantially horizontal, located inside and at the base of the cylinder with straight and smooth walls Consists of a coarse turntable. However, this process is essentially a batch process As such, it is not well suited for large scale production of detergent powders. More recently, Other attempts are "post tower" or continuous to increase the density of spray-dried detergent granules Made to serve the process. Typically, in such a process, the granules are A first device for pulverizing or pulverizing and a second device for increasing the density of pulverized granules by agglomeration And require. These processes use “post tower” or spray-dried granules Can be processed or densified to achieve the desired increase in density, The ability to increase surfactant levels without a coating step is limited. In addition Therefore, processing or densification by “post tower” is economical (high capital cost) and And operation complexity is not desirable. In addition, all the above processes are sprayed It is mainly concerned with densifying or otherwise processing the rye granules. Current , The relative amounts and ties of substances subjected to the spray drying process in the production of detergent granules Is limited. For example, the resulting detergent composition may require high levels of surfactant. Although it was difficult to do so, its characteristics make the production of detergent more efficient. As a result, detergent compositions are limited by conventional spray drying techniques. It is desirable to have a process that can be produced without any problems.   To that end, the art is also rich in disclosing processes involving agglomeration of detergent compositions. In. For example, mixing zeolite and / or laminated silicate with a mixer Attempts have been made to agglomerate detergent builders by forming free flowing agglomerates Was. In such attempts, those processes can be used to produce detergent agglomerates. Starting wash in the form of pastes, liquids and dry substances Mechanism by which dispersant materials can be effectively aggregated into crisp, free-flowing detergent agglomerates For, they do not provide.   Therefore, the detergent composition is continuously produced to increase the density directly from the starting detergent components. Need to have an agglomerated (non-tower process) process And preferably the density can be achieved by adjusting the process conditions. Moreover, (1) flexibility in terms of final density of the final composition and (2) some differences. Flexibility in incorporating different types of detergent components (especially liquid components) into the process And more efficient, flexible and flexible to facilitate large-scale production of detergents. There remains a need for such a process that is economical and economical.   The following references relate to densifying spray-dried granules: Appel et al. U.S. Pat. No. 5,133,924 (Lever); Bortolotti et al., U.S. Pat. 0,657 (Lever); Johnson et al., British Patent 1,517,713 (Unilever). And Curtis European Patent Application 451,894.   The following references relate to producing detergents by coagulation: Beujean et al. WO 93 / 23,523 (Henkel); Lutz et al., U.S. Pat. No. 4,992,079. (FMC Corporation), US Patent No. 4,427,417 to Porasik et al. U.S. Patent No. 5,108,646 to Beerse et al. (Procter &Gamble); Capeci et al., US Patent No. 5,366,652 (Procter &Gamble); European Patent Application No. 351,937 to Hollingsworth et al. (Unilever); U.S. Pat. No. 5,205,958, published WO 96/0435 to Dhalewadikar et al. No. 9 (Unilever).   For example, WO 93 / 23,523 (Henkel) discloses a low speed mixer. Process with more pre-agglomeration and less than 25 wt% of granules with a diameter of 2 mm or more Note the separate flocculation step with a high-speed mixer to obtain a high-density detergent composition It is listed. U.S. Pat. No. 4,427,417 (Korex) discloses caking and Describes a continuous process for agglomeration that reduces You.   None of the current technologies have demonstrated all of the advantages and effects of the present invention.                               Summary of the Invention   The present invention provides a process for producing a high-density granular detergent composition, Meets the needs in the art. The present invention relates to agglomeration (eg, non-tower ) Process to provide a granular detergent composition with flexibility in terms of final density of the final composition Providing a production process also meets the needs in the industry. are doing. The process limits the production of compositions with high surfactant content. No limited conventional spray-dry tower is used. In addition, the process of the present invention Is more efficient, economical and efficient for the various detergent compositions that can be produced in the process. And flexible. Further, the process typically involves particles and volatile organic Environmentally friendly because it does not use a spray-dry tower that releases compounds into the atmosphere. Easy to deal with the problem.   As used herein, the term “aggregate” refers to a surfactant and / or Aggregating raw materials with binders such as organic solvent / organic solvent and polymer solution Related to the particles formed. As used herein, the term "granulation" is used for The agglomerates are sufficiently fluidized to produce fluid, spherically agglomerated agglomerates. About things. The term "average residence time" as used herein is defined below. About righteousness:         Average residence time (hr) = mass (kg) / throughput (kg / hr)   All percentages used in this specification are "unless otherwise stated" % By weight ". All ratios are by weight unless otherwise indicated. You. As used herein, “comprising” refers to any other term that does not affect the results. It means that steps and other ingredients can be added. The term "consists of "And" consisting essentially of. "   According to one aspect of the present invention, a granular detergent composition having a density of at least about 600 g / l A method for manufacturing an article is provided.   The method is:   (A) In a mixer, disperse the surfactant to form 0.1 to 500 microns The surfactant is coated with a fine powder having a diameter of Are (i) average residence time of about 0.5 to about 15 minutes and (ii) about 0.15 to about 7 kj. / kg energy conditions, aggregates are formed); and   (B) Agglomerate is granulated with one or more fluidizers (each condition of the fluidizer includes (i ) An average residence time of about 1 to about 10 minutes; Fluidized bed, (iii) droplet spray size of about 50 microns or less, (iv) about 175 to about A spray height of 250 mm, (v) a flow velocity of about 0.2 to about 1.4 m / s and (Vi) including a bed temperature of about 12 to about 100 ° C) Consists of steps.   The following method for producing a granular detergent composition having a density of at least about 600 g / l is also provided. Provided, the method is:   (A) In a mixer, disperse the surfactant to form 0.1 to 500 microns The surfactant is coated with a fine powder having a diameter of Are (i) average residence time of about 0.5 to about 15 minutes and (ii) about 0.15 to about 7 kj. / kg energy condition, the first aggregates are formed);   (A ′) Spraying the finely sprayed liquid on the first aggregate using a mixer (mixer conditions) (I) an average residence time of about 0.2 to about 5 seconds, and (ii) an average residence time of about 10 to about 30 m / s. A tip speed and (iii) an energy condition of about 0.15 to about 5 kj / kg; Aggregates are formed); and   (B) granulating the second aggregate with one or more fluidizers (each condition of the fluidizers (I) an average residence time of about 1 to about 10 minutes; (ii) a depth of about 100 to about 300 mm. A non-fluidized bed of (iii) a droplet spray size of about 50 microns or less, (iv) about 175 (V) a flow velocity of about 0.2 to about 1.4 m / s; And (vi) including a bed temperature of about 12 to about 100 ° C) Consists of steps.   At least one produced by any one of the process aspects described herein. Also provided is a granular detergent composition having a high density of about 600 g / l.   Therefore, it is an object of the present invention to provide a mixer with energy input, residence time conditions and Flexibility in terms of final product density by controlling chip and tip speed conditions. It is an object of the present invention to provide a method for continuously producing a detergent composition. Big To provide a more efficient, flexible and economical way to facilitate scale production Is also an object of the present invention. These and other objects, features and additional benefits of the present invention Points may be read in the following specific description of the preferred embodiments and the appended claims. And will be apparent to those skilled in the art.                         Specific description of preferred embodiments   The present invention produces a free-flowing granular detergent agglomerate having a density of at least about 600 g / l. On how to produce. In that method, an aqueous and / or water-based granulation Alternatively, after producing a granular detergent aggregate from a non-aqueous surfactant, 0.1-500 micron Coated with fine powder having a diameter of RON.process First step (i) [Step (a)]   In the first step (i) of the process, the powder, paste and / or liquid One or more aqueous and / or non-aqueous surfactants in form; Fine powder having a diameter of about 1 micron, preferably from about 1 to about 100 microns, Is fed into the first mixer to make (the definition of surfactant and fine powder is Described in detail below). Optionally, a fluidizing device (eg, fluidized bed dry From about 0.1 to about 300 microns emerging from the The internal recycle stream of powder having a diameter of Can be paid. The amount of such an internal recycle stream of powder is zero for the end product ~ 60 wt%.   Preferably, the chopper connectable to the first mixer is Can be used to crush the collection. Therefore, a second mixer with a chopper The accompanying process is useful to reduce the amount of excessive aggregates as end products Such a process is one preferred embodiment of the present invention.   In another embodiment of the present invention, the surfactant of the first step (i) is as described above. Before starting, first use a mixer or premixer (eg, a conventional screw extruder). Or other similar mixers) and subsequently mixed detergent material The feed is fed into the first mixer as described herein for the collection.   Generally speaking, preferably, the average residence time of the first mixer is from about 0.5 to about 1 Within 5 minutes, the energy per unit mass of the first mixer (energy Condition) is in the range of about 0.15 to about 7 kj / kg, and more preferably the first mixer The average residence time of the first mixer is about 3 to about 6 minutes, and the energy per unit mass of the first mixer is The energy (energy conditions) is in the range of about 0.15 to about 4 kj / kg.   An example of a first mixer is that the mixer maintains the above conditions for the first step. As far as possible, it can be any type of mixer known to the person skilled in the art. An example is the Lodge KM Mixer manufactured by the Lodge company (Germany) . An aggregate (first aggregate) is obtained as a result of the first step (i). First The collection is either (1) the second step, or (2) the first step (ii) followed by the second step. Attached to the top.First step (ii) [Step (a ')]   The product from the first step (i) (ie the first agglomerate) is passed to the second mixer Supplied. The first agglomerate is fed to the second mixer, after which the fine spray is transferred to the second mixer. Sprayed on the agglomerate with a sir. Optionally formed in the first step (i) The excess fine powder is added to the first step (ii). Excessive fine powder Spraying the microspray, if added to step (ii), Useful for binding excess fines. Used in the first step (i) About 0-10%, more preferably, of powdered detergent components and / or other detergent components About 2-5% may also be added to the second mixer.   Generally speaking, preferably, the average residence time of the second mixer is from about 0.2 to about 5 Second mixer tip speed in the range of about 10 to about 30 m / s. And the energy per unit mass of the second mixer (energy condition) is about 0 . Within the range of 15 to about 5 kj / kg, more preferably the average residence of the second mixer The time is in the range of about 0.2 to about 5 seconds and the tip speed of the second mixer is about 10 約 30 m / s, the energy per unit mass of the second mixer (d Energy conditions) are in the range of about 0.15 to about 5 kj / kg, most preferably The average residence time of the two mixers is in the range of about 0.2 to about 5 seconds, and the second mixer Chip speed is in the range of about 15 to about 26 m / s and the unit mass of the second mixer The energy per hit (energy condition) is about 0.2 to about 3 kj / kg.   An example of a second mixer is that the mixer satisfies the above conditions for the first step (ii). Any type of mixer known to those skilled in the art, as long as it can be maintained Good. As an example, Flexomic Mode manufactured by Schugi company (Netherlands) There is l. As a result of the first step (ii), a second aggregate is obtained.Second step [Step (b)]   In the second step, the first aggregate or first step from step (i) The second agglomerate from step (ii) increases granulation in producing free-flowing high-density granules. To enhance, it is fed into a fluidizing device such as a fluidized bed. The second step is one Or two or more fluidizing devices (such as fluidized bed dryers and fluidized bed coolers). (Combinations of different types of flow devices). In some cases, the first About 0 to about 1 powder detergent substance and / or other detergent ingredients of the type used in the step 0%, more preferably about 2-5%, may be added to the second step. And if The liquid detergent of the kind used in the first step (i) and the first step (ii) About 0% to about 20%, more preferably about 2% to about 10%, of substances and / or other detergent ingredients % Also add to that step to enhance granulation and granule surface coating be able to.   Generally speaking, a density of at least about 600 g / l, preferably at least 650 g / l. In achieving the degree, the conditions of the flow device are as follows:   Average residence time: about 1 to about 10 minutes   Non-fluidized bed depth: about 100 to about 300 mm   Droplet spray size: about 50 microns or less   Spray height: about 175 to about 250mm   Flow velocity: about 0.2 to about 1.4 m / s   Floor temperature: about 12 to about 100 ° C More preferably   Average residence time: about 2 to about 6 minutes   Non-fluidized bed depth: about 100 to about 250 mm   Droplet spray size: less than about 50 microns   Spray height: about 175 to about 200mm   Flow velocity: about 0.3 to about 1.0 m / s   Floor temperature: about 12 to about 80 ° C   If two different flow devices are used, the average residence time in the second step is the total It is about 2 to about 20 minutes, more preferably about 2 to 12 minutes on the body.   Coating that improves the flowability of the detergent composition and / or minimizes excessive agglomeration A printing agent can also be added at one or more of the following points in the process: (1) The coating agent can be added directly after the fluid bed cooler or the fluid bed dryer; (2) The coating agent may be added between the fluidized bed dryer and the fluidized bed cooler. And / or (3) the coating agent may be added directly to the fluid bed dryer. No. The coating agent is preferably aluminosilicate, silicate, carbon And mixtures thereof. Coating agent used Detergent compositions desired by consumers in that they facilitate the scooping of detergent during Agglomeration by preventing or minimizing excessive agglomeration as well as increasing free flow It is also useful for controlling As those skilled in the art are well aware, excessive aggregation is It makes the flow and aesthetics of the final detergent product very undesirable.                               Starting detergent substance   Made in the present invention, contained in the following detergent substances, microsprays and auxiliary detergent ingredients: The total amount of surfactant in the finished product, in percentage ranges, is usually about 5 to about 6 0%, more preferably about 12 to about 40%, more preferably about 15 to about 35%. You. The surfactant contained above may be used in any part of the process of the invention, for example, First step (i), first step (ii) and / or second step of the present invention Depending on one ofDetergent surfactant (aqueous / non-aqueous)   The amount of surfactant in the present process depends on the final product obtained by the process of the present invention. About 5 to about 60%, more preferably about 12 to about 40%, more preferably, of the total amount Is about 15 to about 35%.   The surfactant of the present process used as the starting detergent material in the first step is In the form of raw materials, as a powder, paste or liquid.   The surfactant itself is preferably anionic, nonionic, zwitterionic, amphoteric and And cationic classes and compatible mixtures thereof. Washing useful in the present invention Surfactants are disclosed in Norris U.S. Pat. No. 3,301, issued May 23, 1972. US Pat. No. 664,961 and Laughlin et al. Issued on Dec. 30, 1975 No. 3,929,678, both of which are referred to. Incorporated herein. Useful cationic surfactants include September 1980 Cockrell U.S. Pat. Nos. 4,222,905 and 198, issued on Dec. 16, 2016. U.S. Pat. No. 4,239,659 to Murphy, issued on Dec. 16, 2009. Some are described herein, both of which are incorporated herein by reference. Among surfactants, anionic and nonionic are preferable, and anionic is most preferable. Is also preferred.   Non-limiting examples of preferred anionic surfactants useful in the present invention include the conventional C₁₁ -C₁₈Alkyl benzene sulfonates ("LAS"), primary branched chains and runs Dam 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_ThreeC_Ten-C₁₈Second grade (2,3) Rukylsulfate (x and (y + 1) are at least about 7, preferably at least An integer of about 9 and M is a water-soluble cation, especially sodium), unsaturated monkey Fate, such as oleyl sulfate, C_Ten-C₁₈Alkyl alkoxy There is sulfate ("AExS"; especially EO1-7 ethoxy sulfate).   Useful anionic surfactants include about 2 to 9 carbon atoms in the acyl group and an alkane 2-acyloxyalkane-1-sulfones having, in part, from about 9 to about 23 carbon atoms Water soluble salts of acids; water soluble olefin sulfonates having about 12 to 24 carbon atoms Salt; about 1 to 3 carbon atoms in the alkyl group and about 8 to 20 carbon atoms in the alkane moiety There is also a β-alkyloxyalkanesulfonate having   Optionally, other exemplary surfactants useful in the pastes of the present invention include C_Ten -C₁₈Alkyl alkoxy carboxylate (especially EO1-5 ethoxycarboxy) Rate), C_Ten-C₁₈Glycerol ether, C_Ten-C₁₈Alkyl polyglycoside And the corresponding sulfated polyglycosides, and C₁₂-C₁₈α-sulfonation There are fatty acid esters. If desired, conventional nonionic and amphoteric surfactants Agents, such as C, including so-called narrow peak alkyl ethoxylates₁₂-C₁₈ Alkyl ethoxylate ("AE"), C₆-C₁₂Alkyl phenol alkoxy Rates (especially ethoxylates and mixed ethoxy / propoxy), C_Ten-C₁₈A Min oxide and the like can also be included in the overall composition. C_Ten-C₁₈N-A Ruby polyhydroxy fatty acid amides can also be used. A typical example is C₁₂-C₁₈N-Me There is tilgurucamide. See WO 9,206,154. For other sugar-derived surfactants Is C_Ten-C₁₈N-alkoxypolyesters such as N- (3-methoxypropyl) glucamide There are rehydroxy fatty acid amides. N-propyl to N-hexyl C₁₂-C₁₈Gurkha Mids can be used for low foaming properties. C_Ten-C₂₀Conventional soaps may also be used. High foaming If desired, the branched chain C_Ten-C₁₆Soap may also be used. Anionic and no Mixtures of nonionic surfactants are particularly useful. Other conventional and useful surfactants Is listed in the standard text.   Cationic surfactants can also be used as detergent surfactants and suitable quaternary The surfactant is Mono C₆-C₁₆, Preferably C₆-C_TenN-alkyl or Alkenyl ammonium surfactant (the remaining N-position is methyl, hydroxyethyl or Or substituted with a hydroxypropyl group). Heterocyclic secondary Surfactants including aliphatic derivatives of tertiary and tertiary amines; aliphatic quaternary ammonium Surfactants including derivatives of uranium, phosphonium and sulfonium compounds Agent; water-soluble salt of ester of α-sulfonated fatty acid; alkyl ether sulfate G; water-soluble salt of olefin sulfonate; β-alkyloxyalkane sulfone The formula R (R¹)_TwoN⁺R^TwoCOO^-(R is C₆-C₁₈Hydrocal A building group, preferably C_Ten-C₁₆Alkyl group or C_Ten-C₁₆Acylamidoalkyl And each R¹Is typically C₁-C_ThreeAlkyl, preferably methyl, R^Two Is C₁-C_FiveA hydrocarbyl group, preferably C₁-C_ThreeAlkylene group, more preferably C₁-C_Two(Which is an alkylene group) can also be used as the detergent surfactant. Appropriate Examples of tine include coconut acylamidopropyl dimethyl betaine, hexadecyl Ledimethyl betaine, C_12-14Acylamidopropyl betaine, C_8-14Asilua Midohexyl diethyl betaine, 4- [C_14-16Acylmethylamide diethylan Monio] -1-carboxybutane, C_16-18Acylamide dimethyl betaine, C_{12- 16} Acylamidopentanediethylbetaine and C_12-16Acylmethylamide di There is methyl betaine. Preferred betaines are C_12-18Dimethyl ammonium hex Sanoate and C_10-18Acylamidopropane (or ethane) dimethyl (or Or diethyl) betaine; Formula R (R¹)_TwoN⁺R^TwoSO_Three-Having sultain (R is C₆-C₁₈Hydrocarbyl group , Preferably C_Ten-C₁₆Alkyl group, more preferably C₁₂-C₁₃An alkyl group , Each R¹Is typically C₁-C_ThreeAlkyl, preferably methyl, R^TwoIs C₁-C₆ A hydrocarbyl group, preferably C₁-C_ThreeAlkylene group, or preferably hydro A xylene alkylene group). Examples of suitable sultaines include C₁₂-C₁₄Jime Tilammonio-2-hydroxypropylsulfonate, C₁₂-C₁₄Amidopropylammonio-2-hydroxypropylsultaine, C₁₂- C₁₄Dihydroxyethylammoniopropanesulfonate and C_16-18Dimethi Luammoniohexane sulfonate, C_12-14Amidopropylammonio- 2-Hydroxypropyl sultaine is preferred.Fine powder   The amount of fine powder of the process used in the first step is About 94-30%, preferably 86-54% of the total amount of starting materials. This process The starting fine powder is ground soda ash, powdered sodium tripolyphosphate (STP P), hydrated tripolyphosphate, ground sodium sulfate, aluminosili Kate, crystal laminated silicate, nitrilotriacetate (NTA), phosphate , Precipitated silicate, polymer, carbonate, citrate, powdered surfactant ( (Eg, powdered alkanesulfonic acid) and of the powder resulting from the process of the present invention. And the average diameter of the powder is 0.1 to 500 mm. Cron, preferably 1-300 microns, more preferably 5-100 microns is there. When hydrated STPP is used as the fine powder of the present invention, a level of 50% or more is required. STPP hydrated to a minimum is preferred. Used in the present invention as a detergent builder The aluminosilicate ion exchange material preferably has a high calcium ion exchange It has both capacity and high exchange rate. Without being bound by theory, High calcium ion exchange rate and capacity are aluminosilicate ion exchange materials Is considered to be a function of several correlation factors based on the way You. In that regard, the aluminosilicate ion exchange material used in the present invention is Produced according to US Patent No. 4,605,509 to Corkill et al. (Procter & Gamble) Preferably, the disclosure is incorporated herein by reference.   Preferably, the aluminosilicate ion exchange material is in "sodium" form. The reason is that the potassium and hydrogen forms of the aluminosilicate R It does not exhibit a high exchange rate and capacity as offered. In addition, aluminos The liquefied ion exchange material has a crisp detergent agglomeration as described herein. Preferably, it is in an overdried form to facilitate production of the product. Departure The aluminosilicate ion exchange material used in the light It is preferred to have a particle size that optimizes their effectiveness. As used here The term "particle size" refers to conventional analytical techniques such as microscopy and scanning electron microscopy. Of a given aluminosilicate ion-exchange material as measured by a microscope (SEM) Represents the average particle size. The preferred particle size of the aluminosilicate is from about 0.1 to about 10 microns And more preferably from about 0.5 to about 9 microns. Most preferably, the particle size is about 1 ~ 8 microns.   Preferably, the aluminosilicate ion exchange material has the following formula:             Na_z[(AlO_Two)_z(SiO_Two)_y] XH_TwoO Wherein z and y are at least integers of 6 and 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 is Has the notation:             Na₁₂[(AlO_Two)₁₂(SiO_Two)₁₂] XH_TwoO In the above formula, x is about 20 to about 30, preferably about 27. These preferred al Minosilicates include, for example, zeolite A) zeolite B and zeolite X. It is commercially available under the name On the other hand, natural or synthetic alumino suitable for use in the present invention Silicate ion exchange materials are described in U.S. Pat. No. 3,985,669 to Krummel et al. May be made as described herein, the disclosure of which is incorporated herein by reference. It is.   The aluminosilicates used in the present invention are calculated on an anhydrous basis and at least About 200mg of CaCO_ThreeHardness / g, preferably about 300 to 352 m g of CaCO_ThreeFurther characterized by an ion exchange capacity in the range of hardness / g It is. In addition, the aluminosilicate ion exchange material has at least about 2 grains. Ca⁺⁺/ Gal / min / -g / gal, more preferably from about 2 to about 6 grains Ca⁺⁺ / Gallon / min / -g / gallon further characterized by a calcium ion exchange rate in the range Attached.Fine spray liquid   The amount of microspray in this process depends on the total end product obtained by the process of the present invention. Of the amount, from about 1 to about 10% (active basis), preferably 2 to about 6% (active basis) ). The fine spray liquid of this process is liquid silicate, anion in liquid form Or cationic surfactants, aqueous or non-aqueous polymer solutions, water and it It can be selected from the group consisting of a mixture of these. Other optional examples of the fine spray liquid of the present invention include nato Lium carboxymethyl cellulose solution, polyethylene glycol (PEG) And dimethylenetriaminepentamethylphosphonic acid (DETMP).   Preferred examples of the anionic surfactant solution that can be used as the fine spray liquid in the present invention are: About 88-97% active HLAS, about 30-50% active NaLAS, about 28% active AE3S solution, about 40-50% active liquid silicate, and the like.   Cationic surfactants can also be used as the microspray liquid and suitable quaternary ammonium Surfactant is Mono C₆-C₁₆, Preferably C₆-C_TenN-alkyl or alkenyl Ammonium surfactant (the remaining N-position is methyl, hydroxyethyl or hydro Substituted with a xypropyl group).   Preferred aqueous or non-aqueous polymer solutions that can be used as microsprays in the present invention Examples are polyamine backbones corresponding to the formula: And modified polyamine formula V_{(n + 1)}W_mY_nZ or Applicable polyamine main chain: And modified polyamine formula V_{(n-k + 1)}W_mY_nY '_kZ (k is less than or equal to n) Modified polyamine, wherein the polyamine backbone before modification is about $ 200. Having a molecular weight of at least i) V units are terminal units having the formula: ii) W units are backbone units having the formula: iii) Y units are branching units having the formula:                                                                and iv) Z units are terminal units having the formula: In the above formula, the main chain linking R unit is C_Two-C₁₂Alkylene, C_Four-C₁₂Alkenylene, C_Three- C₁₂Hydroxyalkylene, C_Four-C₁₂Dihydroxyalkylene, C₈-C₁₂Gials Kill Allylene,-(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_Two-Consisting of and their mixture Selected from the group; R¹Is C_Two-C₆Alkylene and mixtures thereof; R^TwoIs Hydrogen,-(R¹O)_xB and mixtures thereof; R^ThreeIs C₁-C₁₈Alkyl, C₇- C₁₂Arylalkyl, C₇-C₁₂Alkyl-substituted aryl, C₆-C₁₂Aryl and And mixtures thereof; R^FourIs C₁-C₁₂Alkylene, C_Four-C₁₂Alkenylene, C₈ -C₁₂Arylalkylene, C₆-C_TenArylene and mixtures thereof; R^FiveIs C₁-C₁₂Alkylene, C_Three-C₁₂Hydroxyalkylene, C_Four-C₁₂Dihydroxya Lucylene, 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-Oh. And mixtures thereof; R⁶Is C_Two-C₁₂Alkylene or C₆-C₁₂In Arylene Yes; E units are hydrogen, C₁-C_{twenty two}Alkyl, C_Three-C_{twenty two}Alkenyl, C₇-C_{twenty two}Ally Rualkyl, C_Two-C_{twenty two}Hydroxyalkyl,-(CH_Two)_pCO_TwoM,-(CH_Two)_q SO_ThreeM, -CH (CH_TwoCO_TwoM) CO_TwoM,-(CH_Two)_pPO_ThreeM,-(R¹O)_xB , -C (O) R^ThreeAnd oxides thereof; B is selected from the group consisting of 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 M is hydrogen or a sufficient amount of water to satisfy the charge balance. X is a water-soluble anion; m has a value from 4 to about 400 N has a value of 0 to about 200; p has a value of 1 to 6; q has a value of 0 to 6 Has a value of 0 or 1; w has a value of 0 or 1; x has a value of 1 Y has a value of 0-100; z has a value of 0 or 1 I do. One example of the most preferred polyethyleneimine is about 7 ethylene per nitrogen Has a molecular weight of 1800, further modified by ethoxylation to the extent of oxy residues Polyethyleneimine (PEI 1800, E7). Like NaLAS Pre-complexing with an anionic surfactant is important for the polymer solution. Is preferred.   Other preferred aqueous or non-aqueous polymer solutions that can be used as microsprays in the present invention A preferred example is to polymerize or copolymerize a suitable unsaturated monomer, preferably in the acid form. And a polymer polycarboxylate dispersant which can be produced by Polymerize Unsaturated monomeric acids capable of forming suitable polymeric polycarboxylates Include acrylic acid, maleic acid (or maleic anhydride), fumaric acid, itacone There are acids, aconitic acid, mesaconic acid, citraconic acid and methylenemalonic acid. Carboxylate groups such as vinyl methyl ether, styrene, ethylene, etc. The presence of monomer segments not present in the polymer polycarboxylate Is suitable, provided that such segments comprise more than about 40% by weight of the polymer. must not.   Homopolymer polycarbo having a molecular weight of 4000 or more as described below Xylates are preferred. Particularly suitable homopolymer polycarboxylates are acrylic It can be derived from luic acid. Such acrylic acid bases useful in the present invention Limers are water-soluble salts of polymerized acrylic acid. Of such polymers in acid form The average molecular weight is preferably 4000 to 10,000, preferably 4000 to 70. 00, most preferably 4000 to 5000. Such acrylic acid polymer Water-soluble salts of, for example, alkali metals, ammonium and substituted ammonium There is salt.   Copolymer polycarboxy, such as acrylic acid / maleic acid based copolymer Rates may also be used. Such materials include acrylic acid and maleic acid There are water-soluble salts of limers. The average molecular weight of such copolymers in the acid form is favorable. Preferably about 2000 to 100,000, more preferably about 5000 to 750,000 0, most preferably about 7000-65,000. In such copolymers The acrylate / maleate segment ratio in is typically about 30: 1 to about 1 : 1, more preferably about 10: 1 to 2: 1. Such acrylic acid / male Water-soluble salts of the formic acid copolymers include, for example, alkali metals, ammonium and There are exchanged ammonium salts. Pre-complexed with anionic surfactants such as LAS It is preferable for the polymer solution to be kept.Auxiliary detergent ingredients   The starting detergent material of the process may include additional detergent components and / or Or some additional ingredients in the detergent composition during later steps in the process can do. These supplements include other cleaning builders, bleach, Activators, foam enhancers or suppressors, fade inhibitors, and corrosion Inhibitor, soil suspending agent, soil release agent, bactericide, pH adjuster, non-builder alkali source , Chelating agents, smectite clay, enzymes, enzyme stabilizers and fragrances. Reference Baskerville, published February 3, 1976, incorporated herein by reference. Jr. See U.S. Patent No. 3,936,537.   Other builders usually use various water-soluble alkali metals, ammonium or substituted Ammonium phosphate, polyphosphate, phosphonate, polyphosphonate , Carbonate, borate, polyhydroxysulfonate, polyacetate, It can be selected from carboxylate and polycarboxylate. Alkali metal Particularly preferred are sodium and the above-mentioned salts. Preferred for use in the present invention are phosphines , Carbonate, C_10-18Fatty acids, polycarboxylates and their Mixed. More preferred are sodium tripolyphosphate, tetranato Lium pyrophosphate, citrate, tartrate mono and dissuccine And mixtures thereof (see below).   Compared to amorphous sodium silicate, crystalline laminated sodium silicate 4 shows the calcium and magnesium ion exchange capacity clearly increased. in addition, Stacked sodium silicate prefers magnesium ions over calcium ions This is necessary to ensure that virtually all "hardness" is removed from the wash water. It is a feature. However, these crystalline sodium silicates are amorphous silicon silicates. Like and usually more expensive than other builders. Therefore, economically possible washing In order to provide a rinse, the percentage of crystalline sodium silicate used should be considered. It must be determined with due consideration. Such a crystal-laminated sodium silicate U.S. Patent No. 4,605 to Corkill et al., Which is already incorporated herein by reference. , 509.   Specific examples of inorganic phosphate builders include sodium and potassium tripolyphosphates. Sulfate, pyrophosphate, polymer metaphos with a degree of polymerization of about 6 to 21 Fate, and orthophosphate. Examples of polyphosphonate builders are , Sodium and potassium salts of ethylenediphosphonic acid, ethane 1-hydroxy- Sodium and potassium salts of 1,1-diphosphonic acid and ethane 1,1,2-tri Sodium and potassium salts of phosphonic acids. Other phosphorus builder compounds are rice National Patent Nos. 3,159,581, 3,213,030, 3,422,02 No. 1, No. 3,422,137, No. 3,400,176 and No. 3,400, No. 148, all of which are incorporated herein by reference. I will.   Examples of non-phosphorus inorganic builders are tetraborate decahydrate and about 0.5 to about 4.0. , Preferably from about 1.0 to about 2.4 SiO_TwoHas a weight ratio of alkali metal oxide to Silicate. Various water-soluble non-phosphorus organic builders useful in the present invention include: Alkali metal, ammonium and substituted ammonium polyacetate, carbox There are sylate, polycarboxylate and polyhydroxysulfonate. Po Examples of riacetate and polycarboxylate builders are ethylenediamine Acetic acid, nitrilotriacetic acid, oxydisuccinic acid, melitic acid, benzenepolycarboxylic acid Sodium, potassium, lithium, ammonium and substitution of acids and citric acid It is an ammonium salt.   The Polymer Polycarboxylate Builder was issued on March 7, 1967 No. 3,308,067 to Diehl, the disclosure of which is hereby incorporated by reference. Is incorporated herein by reference. Such substances include aliphatic carboxylic acids For example, maleic acid, itaconic acid, mesaconic acid, fumaric acid, aconitic acid, cyto There are water-soluble salts of homo- and copolymers of laconic and methylene malonic acids. This Some of these substances are useful as water-soluble anionic polymers as described below, However, only in the case of a complete mixture with a non-soap anionic surfactant.   Other polycarboxylates suitable for use in the present invention are described on March 13, 1979. U.S. Patent Nos. 4,144,226 and 1979 issued to Crutchfield et al. U.S. Pat. No. 4,246,495 issued to Crutchfield et al. Polyacetal carboxylate described in the description, both of which are reference And incorporated herein by reference. These polyacetal carboxylates are By combining the ester of glyoxylic acid and the polymerization initiator under polymerization conditions Can be manufactured. Then, the obtained polyacetal carboxylate ester is Stable polyacetal carboxylate against rapid depolymerization in alkaline solution To a chemically stable end group, converted to the corresponding salt, Added to the detergent composition. A particularly preferred polycarboxylate builder is 19 U.S. Pat. No. 4,663,071 issued to Bush et al. On May 5, 1987. Tartrate monosuccinate and tartrate disuccinate as described in An ether carboxylate builder composition comprising a combination of Incorporated herein by reference.   Bleaches and activators are available from Chung, issued November 1, 1983. U.S. Pat. No. 4,412,934 and issued Nov. 20, 1984. No. 4,483,781 to Hartman, which is incorporated herein by reference. Both are incorporated herein by reference. Chelating agents are also provided for reference No. 4,663,071 to Bush et al., No. 17, incorporated by reference. It is described in column 54 line to column 18 line 68. The foam control agent is also an optional ingredient Bartole et al., US Patent No. 3,933, issued January 20, 1976. No. 672 and Gault et al., No. 4,136, issued Jan. 23, 1979. No. 045, both of which are incorporated herein by reference. .   Smectite clays suitable for use in the present invention are incorporated herein by reference. U.S. Pat. No. 4,762,6, issued Sep. 9, 1988 to Tucker et al. No. 45, column 6, line 3 to column 7, line 24. Used in the present invention Additional wash builders suitable for use are described in Baskerville Patent Specification, column 13, line 54- Column 16, line 16, and Bush et al., U.S. Pat. No. 4, issued May 5, 1987. No. 663,071 and both are incorporated herein by reference. Be included.Optional process steps   Optionally, the process may involve a first, second and / or third Spraying the additional binder with one or more of the xers. You may. Binders are provided by providing a "binding" or "sticking" agent for the detergent components. Is added for the purpose of increasing cohesion. The binder is preferably water, an anionic Surfactant, nonionic surfactant, liquid silicate, polyethylene glycol, Polyvinyl pyrrolidone polyacrylate, citric acid and mixtures thereof Group. Other suitable binder materials, including those listed herein Are described in U.S. Pat. No. 5,108,646 to Beerse et al. (Procter & Gamble Co.). , The disclosure of which is incorporated herein by reference.   Another optional step considered by this process is to remove excess detergent agglomerates. Screening with a cleaning device, which is desired in the final detergent product It is not limited to a conventional screen selected according to the particle size, but includes It can take various forms. Other optional steps include the already described equipment Conditioning of detergent agglomerates by adding agglomerates to additional drying of .   Another optional step in the process is to spray other conventional detergent ingredients Detergent aggregation obtained by various processes including and / or mixing Finish things. For example, the finishing step provides a more complete detergent composition For this purpose, fragrances, brighteners and enzymes are sprayed on the final agglomerates. Such techniques Techniques and ingredients are well known in the art.   Another optional step in the process is a surfactant paste building professional Process, for example, using an extruder prior to the process of the present invention to remove the paste hardened material. By mixing, the aqueous anionic surfactant paste is hardened. Surface activity The details of the agent paste construction process are described in co-pending PCT / US96 / 15960 (1 (Filed October 4, 996).   For a better understanding of the present invention, the following examples are referenced, By way of illustration only, and not limitation of the claims.                                     An example Example 1   Below is a Lodige KM mixer (KM-600) and then a Schugi FX-160 mixer This is an example for obtaining an aggregate having high density using a fluidized bed apparatus.   [Step 1] HLAS (C₁₁-C₁₈Alkyl benzene sulf 120-260 kg / hr of acid precursor of phonate; 95% active) was added to powdered STPP (4 220 kg / hr, average particle size of 0-75 microns, ground soda ash (15 microns Equivalent particle size) 160 ~ 20Okg / hr) Ground sodium sulfate (15 micron average particle size) 80 ~ 120 kg / hr and 200 kg / hr of internal recycle stream of powder, KM-60 Disperse using a mixer 0 and / or chopper. K for serrated ski It can be used as a mixing element in an M mixer. KM mixer chop Pars may be used to reduce the amount of excessive aggregates. The conditions of the KM mixer are It is as follows:   Average residence time: 3-6 minutes   Energy conditions: 0.15 to 2 kj / kg   Mixer speed: 100-150 rpm   Jacket temperature: 30-50 ° C   [Step 2] Aggregate from KM-600 mixer is transferred to Schugi FX-160 mixer Supply. HLAS (C₁₁-C₁₈Acid precursors of alkylbenzenesulfonates; 9 4-97% activity) Fine spray of 10-20 kg / hr to Schugi mixer at about 50-60 ° C Disperse as a liquid. Soda ash (average particle size of about 10-20 microns) 20-80 Add kg / hr to the Schugi mixer. The conditions of the Schugi mixer are as follows :   Average residence time: 0.2-5 seconds   Chip speed: 16-26m / s   Energy conditions: 0.15 to 2 kj / kg   Mixer speed: 2000-3200 rpm   [Step 3] Aggregate from Schugi mixer is dried, spheroidized and Feed to fluid bed dryer for growth. Liquid silicate (solid content 43%, 2. 0R) 20-80 kg / hr can also be added to the fluid bed dryer at 35 ° C. flow The conditions of the floor dryer are as follows:   Average residence time: 2-4 minutes   Non-fluidized bed depth: 200mm   Droplet spray size: less than 50 microns   Spray height: 175-250mm (on distributor plate)   Flow velocity: 0.4-0.8 m / s   Floor temperature: 40-70 ° C The one obtained from step 3 has a density of about 700 g / l, It can optionally be subjected to any process of jing and / or grinding.Example 2   Below is a Lodige KM mixer (KM-600), followed by a Schugi FX-160 mixer This is an example for obtaining an aggregate having high density using a fluidized bed apparatus.   [Step 1] HLAS (C₁₁-C₁₈Alkyl benzene sulf 15-30 kg / hr of acid precursor of phonate; 95% active 220 kg / hr, average particle size of 75 microns, ground soda ash (average particle size of 15 microns) Diameter) 160-200kg / hr, ground sodium sulfate (15 micron average particle size) 8 KM-6 with 0-120 kg / hr and 200 kg / hr of internal recycle stream of powder Disperse with a 00 mixer chopper and / or skim. Serrated The key can be used as a mixing element in a KM mixer. KM mixer A chopper may be used to reduce the amount of excessive agglomerates. KM mixer The conditions are as follows:   Average residence time: 3-6 minutes   Energy conditions: 0.15 to 2 kj / kg   Mixer speed: 100-150 rpm   Jacket temperature: 30-50 ° C   [Step 2] Aggregate from KM-600 mixer is transferred to Schugi FX-160 mixer Supply. Neutralized AE_ThreeS liquid (25-28% active) 10-25 kg / hr Disperse as a fine spray in a Schugi mixer at 30-40 ° C. Soda ash 20-8 Add 0 kg / hr to the Schugi mixer. Schugi mixer conditions are as follows: RU:   Average residence time: 0.2-5 seconds   Chip speed: 16-26m / s   Energy conditions: 0.15 to 2 kj / kg   Mixer speed: 2000-3200 rpm   [Step 3] Aggregate from Schugi mixer is dried, spheroidized and Feed to fluid bed dryer for growth. Liquid silicate (solid content 43%, 2. 0R) 20-80 kg / hr can also be added to the fluid bed dryer at 35 ° C. The conditions of the fluidized bed dryer are as follows:   Average residence time: 2-4 minutes   Non-fluidized bed depth: 200mm   Droplet spray size: less than 50 microns   Spray height: 175-250mm (on distributor plate)   Flow velocity: 0.4-0.8 m / s   Floor temperature: 40-70 ° C The one obtained from step 3 has a density of about 700 g / l, It can optionally be subjected to any process of jing and / or grinding.Example 3   Below is a Lodige KM mixer (KM-600), then flow for further granulation This is an example for obtaining an aggregate having a high density using a moving bed apparatus.   [Step 1] Aqueous coconut fatty alcohol sulfate surfactant paste (C₁₂-C₁₈, 71.5% activity) 250-270 kg / hr, HLAS (C₁₁-C₁₈A Acid precursor of alkylbenzenesulfonate; 94-97% activity) 40-80 kg / hr Powdered STPP (average particle size of 40 to 75 microns) 220 kg / hr, ground soda Ash (15 micron average particle size) 160-200 kg / hr, ground sodium sulfate (1 80-120 kg / hr (5 micron average particle size) and internal recycle stream 20 of powder Feed together with 0 kg / hr to KM-600 mixer. Surfactant paste is about Feed at 40-52 ° C, powder at room temperature. KM mixer chopper, It may be used to reduce the amount of excessive aggregates. The conditions of the KM mixer are as follows It is a cage:   Average residence time: 3-6 minutes   Energy conditions: 0.15 to 2 kj / kg   Mixer speed: 100-150 rpm   Jacket temperature: 30-50 ° C   [Step 2] The aggregate from the KM mixer is dried, spheroidized and formed. Feed to fluid bed dryer for length. Liquid silicate (solid content 43%, 2.0 R) 20-80 kg / hr can also be added to the fluid bed dryer at 35 ° C. The conditions of the fluidized bed dryer are as follows:   Average residence time: 2-4 minutes   Non-fluidized bed depth: 200mm   Droplet spray size: less than 50 microns   Spray height: 175-250mm (on distributor plate)   Flow velocity: 0.4-0.8 m / s   Floor temperature: 40-70 ° C The one obtained from step 3 has a density of at least 700 g / l, Can optionally be subjected to any process of sizing and / or grinding .   Although the present invention has been described in detail, various modifications may depart from the scope of the invention. Without limiting the invention to those described in the specification. That will be apparent to those skilled in the art.

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Claims (1)

[Claims]   1. (A) In a mixer, a surfactant is dispersed to form a mixture of 0.1 to 500 Coat the surfactant with a fine powder having the diameter of a clone (mixer The conditions include (i) an average residence time of about 0.5 to about 15 minutes and (ii) about 0.15 to about 15 minutes. Containing energy conditions of about 7 kj / kg, aggregates are formed); and   (B) Agglomerate is granulated with one or more fluidizers (each condition of the fluidizer includes (i ) An average residence time of about 1 to about 10 minutes; Fluidized bed, (iii) droplet spray size of about 50 microns or less, (iv) about 175-175 A spray height of about 250 mm, (v) a flow velocity of about 0.2 to about 1.4 m / s and (Vi) including a bed temperature of about 12 to about 100 ° C) A granular detergent composition having a density of at least about 600 g / l comprising Non-tower process for building.   2. (A) In a mixer, a surfactant is dispersed to form a mixture of 0.1 to 500 Coat the surfactant with a fine powder having the diameter of a clone (mixer The conditions include (i) an average residence time of about 0.5 to about 15 minutes and (ii) about 0.15 to Containing an energy condition of about 7 kj / kg, a first aggregate is formed);   (A ′) Spraying the finely sprayed liquid on the first aggregate using a mixer (mixer conditions) (I) an average residence time of about 0.2 to about 5 seconds, and (ii) an average residence time of about 10 to about 30 m / s. A tip speed and (iii) an energy condition of about 0.15 to about 5 kj / kg; Aggregates are formed); and   (B) granulating the second aggregate with one or more fluidizers (each condition of the fluidizers (I) an average residence time of about 1 to about 10 minutes; (ii) a depth of about 100 to about 300 mm. Non-fluidized bed, (iii) droplet spray size of about 50 microns or less, (iv) about 175 (V) a flow velocity of about 0.2 to about 1.4 m / s; And (vi) including a bed temperature of about 12 to about 100 ° C) A granular detergent composition having a density of at least about 600 g / l comprising Non-tower process for building.   3. Surfactant is anionic surfactant, nonionic surfactant, cation Selected from the group consisting of amphoteric surfactants, zwitterionic, amphoteric and mixtures thereof, The process according to claim 1.   4. When the surfactant is an alkylbenzene sulfonate or an alkyl alkoxysa Rulfate, alkyl ethoxylate, alkyl sulfate, coconut fatty acid Claims selected from the group consisting of rucol sulfate and mixtures thereof. 3. The process according to 1 or 2.   5. The aqueous or non-aqueous polymer solution is separated with the surfactant in step (a). The process of claim 1 or 2, wherein the process is dispersed.   6. The fine powder is soda ash, powdered sodium tripolyphosphate, trihydrated Polyphosphate, sodium sulfate, aluminosilicate, crystal laminate Silicate, phosphate, precipitated silicate, polymer, carbonate, citrate , Nitrilotriacetate, powdered surfactants and mixtures thereof The process according to claim 1, wherein the process is selected from:   7. An internal recycle stream of powder from the fluidizer is added to step (a) The process according to claim 1, wherein the process is performed.   8. The fine spray liquid is liquid silicate, anionic surfactant, cationic interface From activators, aqueous polymer solutions, non-aqueous polymer solutions, water and mixtures thereof 3. The process of claim 2, wherein the process is selected from the group consisting of:   9. Excess fine powder is formed in step (a) and the excess fine powder is 3. The process according to claim 2, which is added to a ').   10. Granule detergent composition made according to the process according to claim 1 or 2 object.