JP2000503721A - 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 the first aggregate in the mixer Thoroughly mixing (a second agglomerate is formed); and (c) granulating the second agglomerate with one or more flow devices. The process may further include step (b ') between step (b) and step (c), i.e., spraying the fine spray onto 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 surfactants and coatings. 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 densification of spray-dried granules: Appel et al. U.S. Pat. No. 5,133,924 (Lever); Bortolotti et al., U.S. Pat. 0,657 (Lever) and British Patent No. 1,517,713 to Johnson et al. (Unilever ) 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 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, 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) Mix the first aggregate sufficiently with a mixer (mixer conditions include (i ) An average residence time of about 0.5 to about 15 minutes and (ii) an average residence time of about 0.15 to about 7 kj / kg. Energy conditions, a second aggregate is 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). 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) Mix the first aggregate sufficiently with a mixer (mixer conditions include (i ) An average residence time of about 0.5 to about 15 minutes and (ii) an average residence time of about 0.15 to about 7 kj / kg. Energy conditions, a second aggregate is formed);   (B ′) Spraying the finely sprayed liquid onto the second 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. Including tip speed and (iii) energy conditions of about 0.15 to about 5 kj / kg; Aggregates are 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.                         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 of                                 process   (1) Aspects of the present invention, namely the following first step, second step (i) and FIG. 1 which shows a flowchart illustrating a three-step process; And (2) aspects of the present invention, namely the following first step, second step (i) and ( Diagram showing a flowchart illustrating a process consisting of ii) and the third step 2 is referenced.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 the final 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 of the first mixer (energy condition) is about 0.1 5 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 Average residence time is in the range of about 5 to about 20 seconds and the tip speed of the first mixer Is in the range of about 8 to about 18 m / s, and the energy per unit mass of the first mixer is (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. For example, Lodige manufactured by Lodige company (Germany) There is a CB 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 (first aggregate) It is supplied to the second mixer 17. That is, the obtained product 16 is passed through the second mixer 17. Mix well for spheroidization and growth of aggregates and shear well. In some cases, Powder detergent components of the type used in the first step and / or other detergent components 18 About 0 to 10%, more preferably about 2 to 5% of Can be. Preferably, a chopper connectable to a second mixer is desirable Can be used to grind large aggregates. Therefore, the second with chopper The process involving the mixer 17 reduces the amount of excessive agglomerates as a final product Such a process is one preferred embodiment of the present invention.   Generally speaking, preferably, the average residence time of the second mixer is from about 0.5 to about 1 Within 5 minutes, the energy per unit mass of the second mixer (energy Condition) is in the range of about 0.15 to about 7 kj / kg, and more preferably the second mixer The average residence time of the second mixer is in the range of about 3 to about 6 minutes, and is Rip energy is in the range of about 0.15 to about 4 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, Lodige KM manufactured by the Lodge company (Germany) There is a Mixer. As a result of the second step (i), the spherical product 20 (second aggregate ) Is obtained. Then, the obtained product 20 is subjected to the second step (ii) or the third step described below. It is attached to a step.Second step (ii) [Step (b ')]: Obtained product 20 (second aggregate) Is supplied to the third mixer 21, after which the fine spray liquid 22 is mixed by the mixer 21 Sprayed over the collection. Optionally, the first and / or second steps The excess fine powder formed in step (i) is added to the second step (ii). Excess Spraying a fine spray if fine powder is added to the second step (ii) Is useful for binding excess fines on the surface of the agglomerate. First step Powder detergent of the kind used in the second step (i) and / or other detergent components About 0-10%, more preferably about 2-5% of the ingredients are added to the mixer 21 Can be.   Generally speaking, preferably, the average residence time of the third mixer is from about 0.2 to about 5 And the tip speed of the third mixer is in the range of about 10 to about 30 m / s. And the energy per unit mass of the third mixer (energy condition) is about 0 . Between 15 and about 5 kj / kg, more preferably the average residence of the third mixer. The time is in the range of about 0.2 to about 5 seconds, and the tip speed of the third mixer is about 10 And the energy per unit mass of the third mixer is about 30 m / s. 0.15 to about 5 kj / kg, and most preferably the average residence time of the third mixer. The residence time is in the range of about 0.2 to about 5 seconds, and the tip speed of the third mixer is about 1 Energy per unit mass of the third mixer (e.g. Energy conditions) are in the range of about 0.2 to about 3 kj / kg.   An example of a mixer 21 is that the mixer satisfies the above conditions for the second 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 second step, product 24, ie, having excess fines on top Agglomerates are obtained. Next, the obtained product 24 (third aggregate) is Attached to theThird step [Step (c)]   In the third step of the process, the product 20 (second aggregate) obtained or Product 24 (third agglomerate) is granulated to produce a free-flowing, dense granule Is fed into a fluidizing device 27, such as a fluidized bed. The third step is One or more fluidization devices (eg, fluidized bed dryers and fluidized bed coolers) Combinations of different types of flow devices). Third step In the product obtained from the second step, the granules from the third step have a spherical shape. Fluidized enough to have. Optionally, first step, second step Flour of the type used in (i), second step (ii) and / or other detergent ingredients About 0 to about 10%, more preferably about 2 to 5% of the detergent material is added to the third step. Can be obtained. And optionally, the first step and / or other detergents From about 0 to about 20%, more preferably from about 2 to about 20% of the liquid detergent material of the type used in the ingredients. Approximately 10% take that step to enhance granulation and granule surface coating Can be added.   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 one liquid component KM mixer; (3) flexible in injecting at least two liquid components Schugi 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 Are rather expensive, and are easier to handle and / or store 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. Allows the installation of a series of equipment in the plant, so that those skilled in the art Variation of the process to meet properties (eg, particle size, density, recipe design) The proposed invention is also useful in terms of industrial requirements as it allows you to choose . Such variations include the process of the present invention, ie, (i) the first mixer -Second mixer-flow device, (ii) first mixer-second mixer-third mixer -(Iii) first mixer-third mixer-flow device as well as the flow device, (iv) First mixer-third mixer-second mixer-flow device, and (v) first mixer There is also a sir-flow device.                               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 C₁₁ -C₁₈Alkyl benzene sulfonates ("LAS"), primary branched chains and runs Dam C_Ten-C₂₀Alkyl sulfate ("AS"), Formula CH₃(CH₂)_x(CHOSO₃ ⁻M⁺) CH₃and CH₃(CH₂)_y(CHOSO₃ ⁻M⁺) CH₂CH₃C_Ten-C₁₈Second grade (2 , 3) alkyl sulfates (x and (y + 1) are at least about 7, preferably An integer of at least about 9 and M is a water-soluble cation, especially sodium), Saturated sulfates, such as oleyl sulfate, C_Ten-C₁₈Alkyl alcohol There is cis 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 A soluble salt; about 1 to 3 carbon atoms in the alkyl group and about 8 to 20 carbon atoms in the alkane moiety. There are also β-alkyloxyalkanesulfonates which have an offspring.   Optionally, other exemplary surfactants useful in the pastes of the present invention include C_Ten -C₁₈Alkyl alkoxy carboxylate (especially 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-C₁₈Like N- (3-methoxypropyl) glucamide There are N-alkoxy polyhydroxy fatty acid amides. N-propyl to N-hex 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)₂N⁺R²COO⁻(R is C₆C₁₈Hid Locarbyl group, preferably C_Ten-C₁₆Alkyl group or C_Ten-C₁₆Acylamide An alkyl group, each R¹Is typically C₁-C₃Alkyl, preferably methyl Is^,R²Is C₁-C₅A hydrocarbyl group, preferably C₁-C₃Alkylene Group, more preferably C₁-C₂Alkylene group) also as a detergent surfactant Can be used. An example of a suitable betaine is coconut acylamidopropyldimethyl Betaine, hexadecyl dimethyl betaine, C_12-14Acylamidopropyl solid Inn, C_8-14Acylamidohexyl diethyl betaine, 4- [C_14-16Asilmer Cylamidodiethylammonio] -1-carboxybutane, C_16-18Acylami Dodimethyl betaine, C_12-16Acylamidopentanediethylbetaine and C_{1 2-16} There is acylmethylamide dimethyl betaine. Preferred betaines are C_{12-1 8} Dimethylammoniohexanoate and C_10-18Acylamide propane (also Is ethane) dimethyl (or diethyl) betaine; Formula R (R¹)₂N⁺R²SO₃ ⁻(R is C₆-C₁₈Hydroca Ruby group, preferably C_Ten-C₁₆Alkyl group, more preferably C₁₂-C₁₃Archi And each R¹Is typically C₁-C₃Alkyl, preferably methyl , R²Is C₁-C₆A hydrocarbyl group, preferably C₁-C₃Alkylene group Or preferably a hydroxyalkylene group). Examples of suitable sultaines Has C₁₂-C₁₄Dimethylammonio-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 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 This is because they do not show a high exchange rate and capacity so that they can be used. In addition, Alumino The silicate ion exchange material may be a crisp detergent coagulant as described herein. Preferably, it is in an overdried form to facilitate the production of the agglomerate. Book The aluminosilicate ion exchange material used in the invention is a detergent builder. Re 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[(AlO₂)_z(SiO₂)_y] XH₂O 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[(AlO₂)₁₂(SiO₂)₁₂] XH₂O 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 CaCO₃Hardness / g, preferably about 300 to 352 m g of CaCO₃Further characterized by an ion exchange capacity in the range of hardness / g You. In addition, the aluminosilicate ion exchange material has at least about 2 grains C a⁺⁺/ Gallon / min / -g / gallon, more preferably 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 alk Nyl ammonium surfactant (the remaining N-position is methyl, hydroxyethyl or Substituted with a droxypropyl 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) The modified polyamine having a polyamine main chain before modification of about 200 domains. 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 C₂-C₁₂Alkylene, C₄-C₁₂Alkenylene, C₃-C₁₂Hydroxyalkylene, C₄-C₁₂Dihydroxyalkylene, C₈-C₁₂Dialkylarylene,-(R¹O)_xR¹- -(R¹O)_xR⁵(OR¹)_x-,-(CH₂CH (OR²) CH₂O)_z (R¹O)_yR¹(OCH₂CH (OR²) CH₂)_w- -C (O) (R⁴)_rC (O)-, -CH₂CH (OR²) CH₂-And it R is selected from the group consisting of:¹Is C₂-C₆Alkylene and them R is a mixture of²Is hydrogen,-(R¹O)_xB and mixtures thereof; R³Is C₁-C₁₈Alkyl, C₇-C₁₂Arylalkyl, C₇-C₁₂Alkyl Substituted aryl, C₆-C₁₂Aryl and mixtures thereof; R⁴Is C₁- C₁₂Alkylene, C₄-C₁₂Alkenylene, C₈-C₁₂Arylalkylene, C₆-C_TenArylene and mixtures thereof; R⁵Is C₁-C₁₂Alkylene, C₃-C₁₂Hydroxyalkylene, C₄-C₁₂Dihydroxyalkylene, C₈- C₁₂Dialkylarylene, -C (O)-, -C (O) NHR⁶NHC (O)-, -R¹(OR¹)-, -C (O) (R⁴)_rC (O)-, -CH₂CH (OH) CH₂, -CH₂CH (OH) CH₂O (R¹O)_yR¹OCH₂CH (OH) CH₂- And mixtures thereof; R⁶Is C₂-C₁₂Alkylene or C₆-C₁₂Ants E units are hydrogen, C₁-C_{twenty two}Alkyl, C₃-C_{twenty two}Alkenyl, C₇-C_{twenty two}Arylalkyl, C₂-C_{twenty two}Hydroxyalkyl, -(CH₂)_pCO₂M,-(CH₂)_qSO₃M, -CH (CH₂CO₂M) CO₂M,-(CH₂)_pPO₃M, -(R¹O)_xB, -C (O) R³Selected from the group consisting of Oxide; B is hydrogen, C₁-C₆Alkyl,-(CH₂)_qSO₃M, -(CH₂)_pCO₂M,-(CH₂)_q(CHSO₃M) CH₂SO₃M, -(CH₂)_q(CHSO₂M) CH₂SO₃M,-(CH₂)_pPO₃M, -PO₃M and mixtures thereof; M is hydrogen or charge balance Is a sufficient amount of a water-soluble cation; X is a water-soluble anion; Has a value of about 400; n has a value of 0 to about 200; p has a value of 1 to 6 Q has a value of 0-6; r has a value of 0 or 1; w has a value of 0 or 1 Has a value; x has a value of 1 to 100; y has a value of 0 to 100; It has a value of 0 or 1. One example of the most preferred polyethylene imine is nitrogen Further modified by ethoxylation to a degree of about 7 ethyleneoxy residues, Polyethyleneimine having a molecular weight of 1800 (PEI 1800, E7) . Pre-complexing with an anionic surfactant such as NaLAS, Preferred for the above 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 include, for example, alkali metals, ammonium and substituted ammonium. There are um salts.   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. See U.S. Pat. No. 3,936,537 to Jr. et al.   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 E , Carbonate, C_10-18Fatty acids, polycarboxylates and their mixtures It is. More preferred are sodium tripolyphosphate, tetranatri Umpyrophosphate, citrate, tartrate mono and disuccinate , 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- Sodium and potassium salts of triphosphonic acid. Other phosphorus builder compounds Are U.S. Patent Nos. 3,159,581, 3,213,030, 3,422. Nos. 021, 3,422,137, 3,400,176 and 3,40 No. 0,148, all of which are incorporated herein by reference. Be impregnated.   Examples of non-phosphorus inorganic builders are tetraborate decahydrate and about 0.5 to about 4.0. , Preferably 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 Lucali metal, ammonium and substituted ammonium polyacetate, carboxy Rates, polycarboxylates and polyhydroxysulfonates. Poly Examples of acetate and polycarboxylate builders are ethylenediaminetetravinegar Acid, nitrilotriacetic acid, oxydisuccinic acid, melitic acid, benzenepolycarboxylic acid And citric acid sodium, potassium, lithium, ammonium and substituted It is a 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. Particularly preferred polycarboxylate builders are No. 4,663,071 issued to Bush et al. On May 5, 1987. Tartrate monosuccinate and tartrate disuccine described in the detailed description An ether carboxylate builder composition comprising a combination of The indications are 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 Bartoletta et al., U.S. 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 Beerse et al., US Pat. No. 5,108,646 (Procter & 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 (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 Lodige CB mixer (CB-30), then Lodige KM mixer (KM-600), then use a fluidized bed apparatus for further granulation This is an example for obtaining an agglomerate.   [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 pin tool on a -30 mixer. 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 further aggregated. Feed to KM-600 mixer for collection, spheronization and growth. HLAS (C₁₁ -C₁₈Acid precursors of alkylbenzenesulfonates; 94-97% active) 15- 30 kg / hr and ground soda ash (15 micron average particle size) 0-60 kg / hr Add to M mixer. KM mixer chopper, reduce the amount of excessive aggregates May be used for 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   Below is Lodige CB mixer (CB-30), then Lodige KM mixer (KM-600), and then using a Schugi FX-160 mixer, and finally further granulation For obtaining agglomerates with high density using a fluidized bed apparatus (FB) You.   [Step 1] HLAS (C at about 50 ° C.₁₁-C₁₈Alkylbenzenesulfone Acid precursor; 95% activity) 15-30 kg / hr and AE₃S liquid (C_Ten-C₁₈ Alkyl alkoxy sulfate, EO-3, 28% activity) STPP (40-75 micron average particle size) 220 kg / hr, ground soda ash (15 160-200 kg / hr, average particle size of micron, pulverized sodium sulfate (15 micron 80-120 kg / hr and internal recycle flow of powder 200 kg / hr Together with the pin tool of the CB-30 mixer. Surfactant page The strike is supplied at about 40-52 ° C and the powder is supplied at room temperature. CB-30 mixer The conditions 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)] CB-30 mixer having a density of 600 to 700 g / l Aggregates from the KM for further aggregation, spheroidization and growth of the aggregates. Feed to 600 mixer. Ground soda ash (15 micron average particle size) 0-60 kg / hr or 0-30 kg / hr of zeolite can also be added to the KM mixer. A KM mixer chopper may be used to reduce the amount of excessive agglomerates. 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 2 (ii)] Aggregate from KM mixer is transferred to Schugi FX-160 mixer Supply. HLAS (C₁₁-C₁₈Acid precursors of alkylbenzenesulfonates; 9 5% activity) Disperse 30 kg / hr as a fine spray in a Schugi mixer at about 50-60 ° C. Let it. 20-80 kg / hr of soda ash is added to the Schugi mixer. 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 650 g / l, It can optionally be subjected to any process of jing and / or grinding.Example 3   Below is Lodige CB mixer (CB-30), then Lodige KM mixer (KM-600), and then using a Schugi FX-160 mixer, 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, powder STPP (average particle size of 40-75 microns) 220 kg / hr, Ground soda ash (15 micron average particle size) 160-200kg / hr, ground sodium sulfate 80-120 kg / hr of lithium (15 micron average particle size) and internal recycling of powder Disperse with the pin tool of the CB-30 mixer together with the You. The surfactant paste is supplied at about 40-52 ° C and the powder is supplied at room temperature. C The conditions for the B-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 (ii)] Agglomerate from the CB-30 mixer is further aggregated. Feed to KM-600 mixer for collection, spheronization and growth. Crushed soda ash 60 kg / hr (average particle size of 15 microns) is also added to the KM-600 mixer. KM A mixer chopper may be used to reduce the amount of excessive agglomerates. KM The conditions for the -600 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 2 (i)] Agglomerate from the KM-600 mixer is transferred to the Schugi FX-160 mixer. Supply to Ksar. Neutralized AE_Three35 kg / hr of S liquid (28% active) for about 30 Disperse as a fine spray in a Schugi mixer at ４０40 ° C. 20-80 kg of soda ash Add / 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 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.   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) Mix the first aggregate sufficiently with a mixer (mixer conditions include (i ) An average residence time of about 0.5 to about 15 minutes and (ii) an average residence time of about 0.15 to about 7 kj / kg. Energy conditions, a second aggregate is 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) Mix the first aggregate sufficiently with a mixer (mixer conditions include (i ) An average residence time of about 0.5 to about 15 minutes and (ii) an average residence time of about 0.15 to about 7 kj / kg. Energy conditions, a second aggregate is formed);   (B ′) Spraying the finely sprayed liquid onto the second 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. Including tip speed and (iii) energy conditions of about 0.15 to about 5 kj / kg; Aggregates are 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 / or step (b). 3. The process of claim 2, wherein excess fine powder is added to step (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 3. The process of claim 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.