JP2000504062A - 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 and coating the surfactant with a fine powder (a first aggregate is formed); (b) mixing on the first aggregate in the mixer Spraying a finely-sprayed liquid onto the mixture (a second aggregate is formed); and (c) granulating a third aggregate with one or more flow devices. The process may further include step (b ') between step (b) and step (c), i.e., thoroughly mixing the second 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 a method for producing detergent aggregates comprising It relates to a continuous process produced by feeding quality into a series of mixers. The process requires that the density be adapted 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. The ability to incorporate certain types of detergent components, especially those in liquid form, into the process More efficient and flexible to facilitate large-scale production of detergents And the need for such an economical process remains.   The following references relate to densification of spray-dried granules: Appel et al. U.S. Pat. No. 5,133,924 (Lever); Bortolotti et al., U.S. Pat. No. 60,657 (Lever) and British Patent No. 1,517,713 to Johnson et al. lever) and Curtis, European Patent Application 451,894.   The following references relate to the production of detergents by flocculation: 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. (Korex U.S. Patent No. 5,108,646 to Beerse et al. (Procter & Gamble), Capeci. U.S. Patent No. 5,366,652 (Procter &Gamble); Hollingsworth et al. European Patent Application 351,937 (Unilever); Swatling et al., US Pat. No. 05,958, published by Dhalewadikar et al., WO 96/04359 (Unilever) Thin book.   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. Describes a continuous process for agglomeration, which reduces excessive agglomerates I have.   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, Meet the needs in the industry. 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 Is (i) an average residence time of about 2 to about 50 seconds, and (ii) a chip of about 4 to about 25 m / s. Speed and energy conditions of (iii) about 0.15 to about 7 kj / kg; Object is formed);   (B) Spray the finely sprayed liquid on the first aggregate using a mixer (under the conditions of the mixer). Is (i) an average residence time of about 0.2 to about 5 seconds, and (ii) a time of about 10 to about 30 m / s. And (iii) an energy condition of about 0.15 to about 5 kj / kg, Aggregates are formed); and   (C) granulating the second aggregate with one or more fluidizers (each condition of the fluidizers (I) average residence time of about 1 to about 10 minutes; (ii) 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) spray height of about 175 to about 250 mm, (v) about 0.2 to about 1.4 m / s and a (vi) 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 Is (i) an average residence time of about 2 to about 50 seconds, and (ii) a chip of about 4 to about 25 m / s. Speed and energy conditions of (iii) about 0.15 to about 7 kj / kg; Object is formed);   (B) Spray the finely sprayed liquid on the first aggregate using a mixer (under the conditions of the mixer). Is (i) an average residence time of about 0.2 to about 5 seconds, and (ii) a time of about 10 to about 30 m / s. And (iii) an energy condition of about 0.15 to about 5 kj / kg, Aggregates are formed);   (B ') Mix the second aggregate sufficiently with a mixer (mixer conditions include (I) an average residence time of about 0.5 to about 15 minutes and (ii) about 0.15 to about 7 kj / k. g energy conditions, a third aggregate is formed); and   (C) granulating the third aggregate with one or more fluidizing devices (each condition of the fluidizing device is (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) spray height of about 175 to about 250 mm, (v) about 0.2 to about 1.4 m / s and a (vi) 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.                             BRIEF DESCRIPTION OF THE FIGURES   FIG. 1 shows the production of a granular detergent composition having a density of at least 600 g / l. First, the coagulation process by the first mixer, then the second mixer, and then the flow device FIG. 3 is a process diagram of a process according to one embodiment of the present invention, including:   FIG. 2 shows the production of a granular detergent composition having a density of at least 600 g / l. First, then the second mixer, then the third mixer, and finally the flow device FIG. 3 is a flowchart of a process according to an embodiment of the present invention, including an agglomeration process according to the present invention.   FIG. 3 shows a first mixer, a second mixer, and a second mixer for producing a granular detergent composition. Various mixers selected from the group consisting of three mixers, flow devices and combinations thereof. It is a process drawing of the process which can perform the collection process.                         Specific description of preferred embodiments   The present invention produces a free-flowing granular detergent aggregate having a density of at least 600 g / l. On how to do it. In that method, to obtain low density granules, aqueous and / or Is from 0.1 to 500 micron after producing granule detergent aggregate from non-aqueous surfactant Coated with a fine powder having a diameter ofprocess   Aspects of the present invention, namely the following first step, second step (i) and third step FIG. 1 showing a flow chart illustrating an example of a process comprising The first embodiment, the following second steps (i) and (ii) and the third step See FIG. 2 for a flowchart illustrating the process consisting of steps. It is.First step [Step (a)]   In the first step of the process, the surfactant 11, namely powder, paste and One or more aqueous and / or non-aqueous surfactants in liquid form; Fine particles having a diameter of 0.1 to 500 microns, preferably about 1 to about 100 microns Powder 12 is fed into a first mixer 13 to form an agglomerate (surfactant Definitions of agents and fine powders are described in detail below). In some cases, From about 0.1 to about 300 microliters coming out of the flow device 27 described at step 3. The internal recycle stream of powder 30 having a diameter of 0.5 mm Sir can be supplied. The amount of such an internal recycle stream of powder 30 is 0 to about 60 wt% of end product 29.   In another embodiment of the present invention, surfactant 11 is first added to the mixer before the above. Or premixer (eg, a conventional screw extruder or other similar mixer) The detergent material fed into and subsequently mixed with the detergent material herein Feed into the first step mixer as described herein.   Generally speaking, preferably, the average residence time of the first mixer is from about 2 to about 50 seconds. And the tip speed of the first mixer is in the range of about 4 to about 25 m / s. Yes, the energy per unit mass (energy condition) of the first mixer is About 0.15 to about 7 kj / kg, more preferably the average residence time of the first mixer. Is in the range of about 5 to about 30 seconds and the tip speed of the first mixer is about 6 to about 18 m / s, the energy per unit mass of the first mixer (energy Condition) is in the range of about 0.3 to about 4 kj / kg, most preferably the first mixer The average residence time of the first mixer is in the range of about 5 to about 20 seconds, and the tip speed of the first mixer is Energy in the range of about 8 to about 18 m / s, per unit mass of the first mixer (Energy conditions) are in the range of about 0.3 to about 4 kj / kg.   An example of a mixer in the first step is that the mixer relates to the first step. Any type of mixer known to those skilled in the art as long as the above conditions can be maintained It may be. As an example, Lodig manufactured by the Lodge company (Germany) There is an eCB mixer. As a result of the first step, product 16 (on the surface of the aggregates) (A first aggregate having fine powder) is obtained.Second step [Step (b) / Step (b ')]   In one preferred embodiment, only two types of alternatives, namely the second step (i) Or the second step (i) followed by the second step (ii).   Second step (i) [step (b)]: The obtained product 16, ie, the first aggregate Is supplied to a second mixer 17, after which the fine spray liquid 18 is mixed with the first Sprayed over the collection. In some cases, excess fine powder formed in the first step Is added to the second step. Excess fine powder is added to the second step (i) Spraying the fine spray liquid binds the excess fine powder on the surface of the agglomerate if Useful for Used in the first step and / or other detergent ingredients About 0 to 10%, more preferably about 2 to 5% of the powder detergent components 7 can be added.   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 . Between 15 and 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 energy (energy condition) is about 0.2 to about 3 kj / kg.   An example of a second mixer 17 is the mixer described in the above section relating to the second step (i). Any type of mixer known to those skilled in the art, as long as the You may. As an example, Flexomic manufactured by the Schugi company (Nelherlands)  There is a Model. As a result of the second step, a product 20 is obtained. Then get Product 20 (second aggregate) is subjected to the second step (ii) or the third step You.   Second step (ii) [Step (b ')]: The product obtained in the second step (i) The product 20 (second aggregate) is supplied to the third mixer 21. That is, the second mixer The resulting product is mixed in a third mixer 21 for spheroidization and growth of aggregates. And is often sheared. Optionally, first and / or second steps (I) about 0-1 of the powder detergent component of the type used for the other detergent component; 0%, more preferably about 2-5% can be added to the second step (i) . Preferably, the chopper that can be connected to the third mixer is Can be used to crush the collection. Therefore, the third mixer 2 with chopper Process containing 1 is useful for reducing the amount of excessive aggregates as a final product And such a process is one preferred embodiment of the present invention.   Generally speaking, preferably, the average residence time of the third mixer is from about 0.5 to about 1 Within 5 minutes, the energy per unit mass of the third mixer (energy Condition) is in the range of about 0.15 to about 7 kj / kg, and more preferably the third mixer. The average residence time of the third mixer is about 3 to about 6 minutes, and the energy per unit mass of the third mixer is The energy (energy condition) is in the range of about 0.15 to about 4 Kj / kg.   An example of the third mixer 21 is that the mixer is the same as that described in the second step (ii). Any type of mixer known to those skilled in the art, as long as the You may. As an example, Lodige KM manufactured by the Lodge company (Germany)  There is a Mixer. As a result of the second step (ii), product 24, a spherical granule, can get.Third step [Step (c)]   In the third step of the process, the product obtained in the second step, ie product 2 0 or product 24 to enhance granulation in producing free-flowing high-density granules At a fluidized device 27 such as a fluidized bed. Third step is one or two The above fluidization devices (eg, fluid bed dryers and fluid bed coolers, A combination of different types of flow devices). In the third step, The product obtained from the two steps is such that the granules from the third step have a spherical shape Fluidized enough. Optionally, for the first step and / or other detergent ingredients About 0 to about 10%, more preferably about 2 to 5% of the type of powder detergent material used , Can be added to the third step. Moreover, the first step, the second step About 0% of the liquid detergent material of the type used in the two-step and / or other detergent ingredients From about 20%, more preferably from about 2 to about 10%, by granulation and coating on the surface of the granules. Can be added to that step to enhance the logging.   Generally speaking, a density of at least 600 g / l, preferably 650 g / l or more To achieve, 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 of the third step is about It is 2 to about 20 minutes, more preferably about 2 to 12 minutes.   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 is the third mixer 21 and the fluidized bed May be added directly to the ear. The coating agent is preferably an aluminosilicate , Silicates, carbonates and mixtures thereof. Coatings are used by consumers in that they make it easier to extract detergent during use. Not only enhances the free-flowing properties of the detergent composition, but also prevents or minimizes excessive agglomeration. By reducing the number, it is also useful for controlling aggregation. Well-known by those skilled in the art As described above, excessive flocculation can make the flow and aesthetics of the final detergent product very undesirable. To make things better.   The process of the present invention has (1) flexibility in injecting at least two liquid components. CB mixer; (2) Flexible for injecting at least two liquid components Schugi mixer; (3) Flexible for injecting at least one liquid component KM mixer; (4) flexible in injecting at least two liquid components When performed with a fluidized (fluid) bed, the process involves seven different liquids. Ingredients can be incorporated into the process. Therefore, the process presented is in liquid form They are rather expensive and can be handled and / or stored more than solid materials. One skilled in the art of incorporating the sometimes cumbersome starting detergent material in the granulation process into the granulation process. Is beneficial to   One skilled in the art would use a divertor that could be connected / disconnected between each device. Thus, a series of equipment can be installed in the plant (eg, as shown in FIG. 3), thus Those skilled in the art will be able to meet the desired properties (eg, particle size, density, The proposed invention is engineered because the process variation can be selected It is also useful in terms of business requirements. Such variations include the process of the present invention. 3, the process (i) as shown in FIG. ) First second mixer 17- (line 26) -flow device 27- (line 28) -final Product 29, (ii) first mixer 13- (line 16) -second mixer 17- (la In 20) -third mixer 21- (line 24) -flow device 27- (line 28) Not only the final product 29, but also (iii) the first mixer 17- (line 16 ') Three mixer 21- (line 24) -flow device 27- (line 28) -final product 2 9, (iv) first mixer 13- (line 16 ')-third mixer 21- (line 23) -second mixer 17- (line 26) -flow device 27- (line 28) -Final product 29, and (v) first mixer 13-(line 16 ")-flow device 2 7- (line 28) -the end product 29 is also there.                               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, Any of the first, second and / or third steps of the present invention It depends.Detergent 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 C_ll -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-sulfo having from about 9 to about 23 carbon atoms in the moiety Water-soluble salts of carboxylic acids; water of olefin sulphonates having about 12 to 24 carbon atoms Soluble salt; about 1 to 3 carbon atoms in the alkyl group and about 8 to 20 carbon atoms in the alcohol moiety. There are also β-alkyloxyalkanesulfonates having a substituent.   Optionally, other exemplary surfactants useful in the pastes of the present invention include C_Ten -C₁₈Alkyl alkoxy carboxylate (particularly EO1-5 ethoxycarboxy) Silate), C_Ten-C₁₈Glycerol ether, C_Ten-C₁₈Alkyl polyglyco Cid and the corresponding sulfated polyglycoside, and C₁₂-C₁₈α-sul There are honated fatty acid esters. If desired, conventional nonionic and amphoteric Surfactants such as C, including so-called narrow peak alkyl ethoxylates₁₂ -C₁₈Alkyl ethoxylate ("AE"), C₆-C₁₂Alkylphenol Lucoxylates (especially ethoxylates and mixed ethoxy / propoxy), C_Ten -C₁₈Amine oxide and the like can also be included in the overall composition. C_Ten− C₁₈N-alkyl polyhydroxy fatty acid amides can also be used. A typical example is C₁₂ -C₁₈There is N-methylglucamide. See WO 9,206,154. Other sugar induction Surfactants include C_Ten-C₁₈Such as N- (3-methoxypropyl) glucamide There are N-alkoxy polyhydroxy fatty acid amides. N-propyl to N-hexy Le C₁₂-C₁₈Glucamide can be used for its low foaming properties. C_Ten-C₂₀Customary soap May be used. If high foaming properties are desired, the branched chain C_Ten-C₁₆Soap may also be used. Mixtures of anionic and nonionic surfactants are particularly useful. Other idiomatic Useful surfactants are 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-C₁₆Acylamide alkyl And each R¹Is typically C₁-C_ThreeAlkyl, preferably methyl, R^TwoIs C₁-C_FiveA hydrocarbyl group, preferably C₁-C_ThreeAlkylene group, more preferred Or C₁-C_Two(Which is an alkylene group) can also be used as the detergent surfactant. Suitable Examples of smart betaines include coconut acylamidopropyl dimethyl betaine, Sadecyl dimethyl betaine, C₁₂−₁₄Acylamidopropyl betaine, C₈−₁₄ Acylamidohexyldiethyl betaine, 4- [C₁₄−₁₆Acylmethylamide di Ethylammonio] -1-carboxybutane, C₁₆−₁₈Acylamide dimethylbe Tyne, C₁₂−₁₆Acylamidopentanediethylbetaine and C₁₂−₁₆Acyl There is methylamide dimethyl betaine. Preferred betaines are C₁₂−₁₈Dimethyl Ammoniohexanoate and C_Ten−₁₈Acylamide propane (or ethane ) Dimethyl (or diethyl) betaine; Formula R (R¹)_TwoN⁺R^TwoSO_Three ^-(R is C₆-C₁₈Hydrocarbyl Group, preferably C_Ten-C₁₆Alkyl group, more preferably C₁₂-C₁₃With an alkyl group Yes, each R¹Is typically C₁-C_ThreeAlkyl, preferably methyl, R^TwoIs C₁ -C₆A hydrocarbyl group, preferably C₁-C_ThreeAn alkylene group, or preferably A hydroxyalkylene group). Examples of suitable sultaines include C₁₂-C₁₄ Dimethylammonio-2-hydroxypropylsulfonate, C₁₂-C₁₄Amidopropylammonio-2-hydroxypropylsultaine, C₁₂ -C₁₄Dihydroxyethylammoniopropanesulfonate and C_16-18The There is methylammoniohexanesulfonate, C_12-14Amidopropyl ammo Nio-2-hydroxypropylsultaine 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 Considered to be a function of several correlation factors based on the method of producing 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. Used here The term “particle size” refers to conventional analytical techniques, such as microscopy and scanning electron 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 micron And more preferably from about 0.5 to about 9 microns. Most preferably, the particle size is about 1 to about 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. Be charged.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 Ruammonium surfactant (the remaining N-position is methyl, hydroxyethyl or hydride Substituted with a roxypropyl 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) the unit is a branched unit having the formula: 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-C₁₂Dialkylarylene,-(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-And their Selected from the group consisting of mixtures; R¹Is C_Two-C₆Alkylene and their mixtures R^TwoIs hydrogen,-(R¹O)_xB and mixtures thereof; R^ThreeIs C₁-C₁₈Alkyl, C₇-C₁₂Arylalkyl, C₇-C₁₂Alkyl substitution Aryl, C₆-C₁₂Aryl and mixtures thereof; R^FourIs C₁-C₁₂Al Kiren, C_Four-C₁₂Alkenylene, C₈-C₁₂Arylalkylene, C₆-C_TenA Rylene and mixtures thereof; R^FiveIs C₁-C₁₂Alkylene, C_Three-C₁₂Hid Roxyalkylene, C_Four-C₁₂Dihydroxyalkylene, C₈-C₁₂Dialkylur Rylene, -C (0)-, -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 Mixtures thereof; R⁶Is C_Two-C₁₂Alkylene or C₆-C₁₂Arylene E units are 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^ThreeSelected from the group consisting of An oxide; 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; M is hydrogen or charge balance Is a sufficient amount of a water-soluble cation; X is a water-soluble anion; m is from 4 to about 4 Has a value of 00; n has a value of 0 to about 200; p has a value of 1 to 6; q has a value of 0-6; r has a value of 0 or 1; w has a value of 0 or 1 X has a value between 1 and 100; y has a value between 0 and 100; Or a value of 1. One example of a most preferred polyethylene imine is Molecules further modified by ethoxylation to the extent of seven ethyleneoxy residues Polyethyleneimine having a quantity of 1800 (PEI 1800, E7). Pre-complexing with an anionic surfactant such as NaLAS is Preferred for the polymer solution.   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 from about 7000 to 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 , There are chelating agents, smectite clay, enzymes, enzyme stabilizers and fragrances. For reference Baskerville, Jr., issued February 3, 1976, incorporated herein by reference. See, e.g., 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 Eat, 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 ethylene diphosphonic acid, ethane 1-hydroxy- Sodium and potassium salts of 1,1-diphosphonic acid and ethane 1,1,2-to These are the sodium and potassium salts of phosphonic acid. Other phosphorus builder compounds U.S. Patent Nos. 3,159,581, 3,213,030, 3,422,0 No. 21, No. 3,422,137, No. 3,400,176 and No. 3,400 148, all of which are incorporated herein by reference. Be included.   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. Pat. Nos. 4,144,226 and 1979 issued to Crutchlield 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 US Patent No. 3,933, Bartoletta et al., 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. (Procier & Gamble Co.). And 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 .   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 (Issued 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   The following is a Lodige CB mixer (CB-30), and then a Schugi FX-160 mixer -And then using a Lodige KM mixer (KM-600) and finally further granulation This is an example for obtaining an aggregate having a high density using a fluidized bed apparatus.   [Step 1] Aqueous coconut fatty alcohol sulfate surfactant paste (C₁₂-C₁₈, 71.5% activity) from 250 to 270 kg / hr with powdered STPP (40 220kg / hr) ground soda ash (15 micron average) Particle size) 160-200kg / hr) Ground sodium sulfate (15 micron average particle size) CB with 80-120kg / hr and internal recycle stream of powder 200kg / hr Disperse with a -30 mixer pin tool. Surfactant paste is about 40 ~ Feed at 52 ° C and powder at room temperature. The conditions of the CB-30 mixer are as follows: It is a cage:   Average residence time: 10 to 18 seconds   Chip speed: 7.5 to 14 m / s   Energy condition: 0.5-4kj / kg   Mixer speed: 550-900 rpm   Jacket temperature: 30 ° C   [Step 2 (i)] Agglomerate from CB-30 mixer is transferred to Schugi FX-160 Supply to sir. HLAS (C₁₁−C₁₈Acid precursors of alkylbenzene sulfonates Body: 94-97% activity) 30 kg / hr is finely sprayed 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 2 (ii)] The aggregate from the Schugi mixer is further aggregated, Feed to KM-600 mixer for sphering and growth. Zeolite 30kg / hr Is also added to the KM mixer. Reduce the amount of excessive agglomerates by using the chopper of the KM mixer It may be used for cleaning. The conditions of the KM mixer are as follows:   Average residence time: 3-6 minutes   Energy conditions: 0.15 to 2 kj / kg   Mixer speed: 100-150 rpm   Jacket temperature: 30-40 ° C   [Step 3] 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. Fluidized bed The drying equipment conditions 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 granules obtained from step 3 have a density of about 700 g / l, It can optionally be subjected to any process of jing and / or grinding.Example 2   The following is a Lodige CB mixer (CB-30), and then a Schugi FX-160 mixer ー, then use a Lodige KM mixer (KM-600), and finally further granulation For obtaining an aggregate having high density using a fluidized bed apparatus.   [Step 1] HLAS (C at about 50 ° C.₁₁-C₁₈Alkylbenzenesulfone Acid precursor; 95% activity) 15-30 kg / hr and aqueous coconut fat alcohol Lusulfate surfactant paste (C₁₂-C₁₈, 71.5% activity) 250-2 70 kg / hr, 220 kg / hr powdered STPP (average particle size of 40-75 microns), Ground soda ash (15 micron average particle size) 160-200kg / hr, ground sodium sulfate 80 to 120 kg / hr (15 micron average particle size) and internal recycling of powder Dispersed with the pin tool of the CB-30 mixer together with the flow of 200 kg / hr. You. The surfactant paste is supplied at about 40-52 ° C and the powder is supplied at room temperature. The conditions of the CB-30 mixer are as follows:   Average residence time: 10 to 18 seconds   Chip speed: 7.5 to 14 m / s   Energy condition: 0.5-4kj / kg   Mixer speed: 550-900 rpm   Jacket temperature: 30 ° C   [Step 2 (i)] Agglomerate from the CB-30 mixer is transferred to Schugi FX-160 MIKI. Supply to sir. Neutralized AE_ThreeS liquid (28% active) 35kg / hr about 30 ~ Disperse as a fine spray in a Schugi mixer at 40 ° C. Soda ash 20-80kg / h Add r to 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 2 (ii)] Aggregate from the Schugi mixer is further aggregated. Feed to KM-600 mixer for sphering and growth. Crushed soda ash ( 60 kg / hr (average particle size of 15 microns) are also added to the 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: 30-40 ° C   [Step 3] 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. Fluidized bed The drying equipment conditions 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 product obtained from the fluidized bed dryer is supplied to a fluidized bed cooler. Article of fluidized bed cooling device The results are as follows:   Average residence time: 2-4 minutes   Non-fluidized bed depth: 200mm   Flow velocity: 0.4-0.8 m / s   Floor temperature: 12-60 ° C The granules obtained from step 3 have a density of about 700 g / l and are sized And / or may optionally be subjected to any process of grinding.Example 3   The following is a Lodige CB mixer (CB-30), and then a Schugi FX-160 mixer Using a fluidized bed apparatus for further coagulation It is an example for obtaining a thing.   [Step 1] Aqueous coconut fatty alcohol sulfate surfactant paste (C₁₂-C₁₈, 71.5% activity) from 250 to 270 kg / hr with powdered STPP (40 220 kg / hr, ground soda ash (average particle size of 15 microns) Particle size) 160-200kg / hr, ground sodium sulfate (15 micron average particle size) CB with 80-120kg / hr and internal recycle stream of powder 200kg / hr Disperse with a -30 mixer pin tool. Surfactant paste is about 40 ~ Feed at 52 ° C and powder at room temperature. The conditions of the CB-30 mixer are as follows: It is a cage:   Average residence time: 10 to 18 seconds   Chip speed: 7.5 to 14 m / s   Energy condition: 0.5-4kj / kg   Mixer speed: 550-900 rpm   Jacket temperature: 30 ° C   [Step 2 (i)] Agglomerate from the CB-30 mixer is transferred to Schugi FX-160 MIKI. Supply to sir. HLAS (C₁₁-C₁₈Acid precursors of alkylbenzene sulfonates 30-kg / hr at about 50-60 ° C into a Schugi mixer Disperse as a mist. 20-80 kg / hr of soda ash is added 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 granules obtained from step 3 have a density of about 600 g / l, It can optionally be subjected to any process of jing 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.

────────────────────────────────────────────────── ─── Continuation of front page    (81) Designated countries EP (AT, BE, CH, DE, DK, ES, FI, FR, GB, GR, IE, IT, L U, MC, NL, PT, SE), OA (BF, BJ, CF) , CG, CI, CM, GA, GN, ML, MR, NE, SN, TD, TG), AP (GH, KE, LS, MW, S D, SZ, UG), UA (AM, AZ, BY, KG, KZ , MD, RU, TJ, TM), AL, AM, AT, AU , AZ, BA, BB, BG, BR, BY, CA, CH, CN, CU, CZ, DE, DK, EE, ES, FI, G B, GE, GH, HU, IL, IS, JP, KE, KG , KP, KR, KZ, LC, LK, LR, LS, LT, LU, LV, MD, MG, MK, MN, MW, MX, N O, NZ, PL, PT, RO, RU, SD, SE, SG , SI, SK, TJ, TM, TR, TT, UA, UG, US, UZ, VN, YU (72) Inventors Manibanan, Kanda Sammy             5-11, 501, Mukoyo-cho, Higashinada-ku, Kobe, Hyogo Prefecture             ―2508

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 Conditions include (i) an average residence time of about 2 to about 50 seconds, and (ii) about 4 to about 25 m / s. Including tip speed and (iii) energy conditions of about 0.15 to about 7 kj / kg, Aggregates are formed);   (B) Spray the finely sprayed liquid on the first aggregate using a mixer (under the conditions of the mixer). Is (i) an average residence time of about 0.2 to about 5 seconds, and (ii) a time of about 10 to about 30 m / s. And (iii) an energy condition of about 0.15 to about 5 kj / kg, Aggregates are formed); and   (C) 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) spray height of about 175 to about 250 mm, (v) about 0.2 to about 1.4 m / s and a (vi) 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 Conditions include (i) an average residence time of about 2 to about 50 seconds, and (ii) about 4 to about 25 m / s. Including tip speed and (iii) energy conditions of about 0.15 to about 7 kj / kg, Aggregates are formed);   (B) Spray the finely sprayed liquid on the first aggregate using a mixer (under the conditions of the mixer). Is (i) an average residence time of about 0.2 to about 5 seconds, and (ii) a time of about 10 to about 30 m / s. And (iii) an energy condition of about 0.15 to about 5 kj / kg, Aggregates are formed);   (B ') Mix the second aggregate sufficiently with a mixer (mixer conditions include: (I) an average residence time of about 0.5 to about 15 minutes and (ii) about 0.15 to about 7 kj / k. g energy conditions and a third aggregate is formed); and   (C) granulating the third aggregate with one or more fluidizing devices (each condition of the fluidizing device is (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) spray height of about 175 to about 250 mm, (v) about 0.2 to about 1.4 m / s and a (vi) 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. Excess fine powder is formed in step (a) and excess fine powder is The process according to claim 1 or 2, wherein the process is added to (b).   6. 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.   7. 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:   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 The process according to claim 1 or 2, wherein the process is selected from the group consisting of:   9. 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.   10. Granule detergent composition made according to the process according to claim 1 or 2 object.