MXPA99003195A - Process for making a detergent composition by non-tower process - Google Patents

Abstract

A non-tower process for continuously preparing granular detergent composition having a density of at least about 600 g/l is provided. The process comprises the steps of (a) dispersing a surfactant, and coating the surfactant with fine powder having a diameter from 0.1 to 500 microns, in a mixer, and (b) granulating the agglomerates in one or more fluidizing apparatus. The process can also comprise further step (a'), i.e., spraying finely atomized liquid onto the first agglomerates in a mixer, between step (a) and step (b).

Description

PROCEDURE TO MAKE A COMPOSITION DETERGENT BY A PROCEDURE THAT IS NOT OF TOWER FIELD OF THE INVENTION The present invention generally relates to a non-tower process for producing a particulate detergent composition. More particularly, the invention is directed to a continuous process during which detergent agglomerates are produced by feeding a surfactant and coating materials in a series of mixers. The process produces a free-flowing detergent composition, whose density can be adjusted for a wide range of consumer needs, and which can be sold commercially.

BACKGROUND OF THE INVENTION Recently, there has been considerable interest within the detergent industry for laundry detergents that are "compact" and, therefore, have low dosage volumes. To facilitate the production of these so-called low dosage detergents, many attempts have been made to produce high density global detergents, for example, with a density of 600 g / 1 or more. Low dosage detergents are currently in high demand because they conserve resources and can be marketed in small packages that are more convenient for consumers. However, the degree to which modern detergent products need to be "compact" in nature remains uncertain. In fact, many consumers, especially in developing countries, continue to prefer higher dosage levels in their respective laundry operations. In general, there are two primary types of procedures by which granules or detergent powders can be prepared. The first type of process involves spray drying an aqueous detergent suspension in a spray drying tower to produce highly porous detergent granules (eg, tower process for low density detergent compositions). In the second type of process, the different detergent components are mixed dry, after which they are agglomerated with a binder such as anionic or nonionic surfactant to produce high density detergent compositions (e.g., agglomeration process for produce high density detergent compositions). In the two previous processes, the important factors that determine the density of the resulting detergent granules are the shape, porosity and particle size distribution of said granules, the density of the different starting materials, the shape of the different starting materials. , and its respective chemical composition. There have been many attempts in the art to provide methods that increase the density of detergent granules or powders. Particular attention has been given to the densification of spray-dried granules by post-tower treatment. For example, an attempt involves an intermittent procedure in which granular or spray-dried detergent powders containing sodium tripolyphosphate and sodium sulfate are densified and spheronized in a Marumerizer®. This apparatus comprises a rotatable table, made rough and substantially horizontal, located inside and at the base of a substantially vertical smooth wall cylinder. However, this process is essentially an intermittent process and is therefore less convenient for the large-scale production of detergent powders. More recently, other attempts have been made to provide continuous processes to increase the density of spray-dried or post-tower detergent granules. Typically, said processes require a first apparatus that pulverizes or crushes the granules, and a second apparatus that increases the density of the pulverized granules by agglomeration. Although these procedures achieve the desired increase in density by treating or densifying spray-dried or post-tower granules, are limited in their ability to go further at the surfactant level without a subsequent coating step. In addition, the treatment or densification by "post tower" is not favorable in terms of economy (high capital cost) and complexity of operation. In addition, all of the aforementioned processes are directed primarily to densify or otherwise process spray-dried granules. Currently, the relative amounts and types of materials subjected to spray drying processes in the production of detergent granules have been limited. For example, it has been difficult to achieve high levels of agent ^ LO surfactant in the resulting detergent composition, a feature that facilitates the production of detergents more efficiently. Thus, it would be convenient to have a procedure by means of which detergent compositions can be produced without having the limitations imposed by the conventional spray drying techniques. To that end, the technique is also replete with descriptions of procedures involving agglomerating detergent compositions. For example, attempts have been made to agglomerate detergency builders by mixing zeolite and / or silicates stratified in a mixer to form free-flowing agglomerates. Although such attempts suggest that their process can be used to produce detergent agglomerates, they do not provide a mechanism by which starting detergent materials in the form of pastes, liquids and dry materials can be effectively agglomerated in brittle, free flowing agglomerates.

Accordingly, there is a need in the art to have an agglomeration process (other than tower) to continuously produce a detergent composition having high density and that is supplied directly from the starting detergent ingredients, and preferably that the Density can be achieved by adjusting the condition of the procedure. Likewise, there is a need for such a process that is more efficient, flexible and economical to facilitate the large-scale production of detergents (1) for flexibility in the final density of the final composition and (2) for flexibility in terms of incorporating Several different types of detergent ingredients (especially liquid ingredients) in the procedure. The following references are directed to densify spray-dried granules: Appel et al., US patent. No. 5,133,924 (Lever); Bortolotti et al., Patent of E.U. No. 5,160,657 (Lever); Johnson et al., British Patent No. 1,517,713 (Unilever); and Curtis, European patent application 451.894. The following references are directed to producing detergents by agglomeration: Beujean et al., Document open to the public No. 093 / 23,523 (Henkel), Lutz et al., US patent. No. 4,992,079 (FMC Corporation), Porasik et al., U.S. Patent. No. 4,427,417 (Korex); Beerse et al., Patent of E.U. No. 5,108,646 (Procter &Gamble); Capeci et al., Patent of E.U. No. 5,366,652 (Procter &Gamble); Hollingsworth et al., European patent application 351,937 (Unilever); Swatling et al., US patent. No. 5,205,958; Dhalewadikar et al., Open document No. O96 / 04359 (Unilever). For example, open document No. 093/23523 (Henkel) describes the process comprising pre-agglomeration by means of a low speed mixer and an additional agglomeration step by means of a high speed mixer to obtain a high density detergent composition, in where less than 25% by weight of the granules have a diameter greater than 2 mm. The patent of E.U. No. 4,427,417 (Korex) describes a continuous process for agglomeration that reduces the formation of cake and agglomerates of excessive size. None of the documents of the existing technique provides all the advantages and benefits of the present invention.

BRIEF DESCRIPTION OF THE INVENTION The present invention meets the aforementioned needs in the art by providing a process that allows to produce a low density granular detergent composition. The present invention also satisfies the aforementioned needs in the art, providing a process that allows to produce a granular detergent composition for flexibility in the final density of the final composition from an agglomeration process (for example, that is not tower) . The method of the proposed invention has the ability to adjust the density of the granules of the composition by controlling the shape thereof. Namely, the process of the present invention can be applied to obtain a granular detergent composition having a low density (for example, irregularly shaped granules having a density of about 300 to about 600 g / 1). The process does not make use of conventional spray drying towers, which is currently limited to produce high load compositions of surfactants. In addition, the process of the present invention is more efficient, economical and flexible with respect to the variety of detergent compositions that may be produced in the process. In addition, the process is more sensitive to environmental problems because it does not make use of spray-drying towers that typically emit particles and volatile organic compounds into the atmosphere. As used herein, the term "agglomerates" refers to particles formed by agglomerating raw materials with binder, such as surfactants and / or inorganic solutions / organic solvents and polymer solutions. As used herein, the term "granular" refers to fluidizing agglomerates intensively to produce granular agglomerates of round shape and free flow. As used herein, the term "average residence time" refers to the following definition: mean residence time (hr) = mass (kg) / flow out 5 (kg / hr) All percentages used in the present are expressed as "percent by weight", unless otherwise indicated. All relationships are weight ratios unless otherwise indicated. As used herein, ^ "Understand" means that other steps and other ingredients that do not affect the result can be added. This term encompasses the terms "consisting of" and "consisting essentially of". According to one aspect of the invention, a method for preparing a detergent composition is provided. granulate having a density of at least about 600 g / 1. The method comprises the steps of: (a) dispersing a surfactant and coating the surfactant with fine powders having a diameter from 0.1 to 500 microns, in a mixer in which mixer conditions include (i) from about 0.5 to about 15 minutes of average residence time and (ii) from about 0.15 to about 7 kj / kg condition of energy, where the agglomerates are formed; and (b) granulating the agglomerates in one or more fluidizing apparatuses wherein the conditions of each of the fluidizing apparatuses include (i) from about 1 to about 10 minutes of average residence time, (ii) of about 100 at about 300 mm depth of the fluidized bed, (iii) not more than about 50 microns 5 in dew drop size, (iv) from about 175 to about 250 mm in dew height, (v) from about 0.2 to about 1.4 m / s fluidized speed and (vi) from about 12 to about 100 ° C bed temperature. k10 A process for preparing a granular detergent composition having a density of at least about 600 g / 1 is also provided, the method comprising the steps of: (a) dispersing a surfactant and coating the surfactant with fine powders having a diameter of 0.1 to 500 microns, in a mixer in which the conditions of the mixer include (i) from about 0.5 to about 15 minutes of average residence time and (ii) from around 0.15 to about 7 kj / kg of condition energy, where the first agglomerates are formed; (a ') spraying a finely atomized liquid on the first agglomerates in a mixer in which the conditions of the mixer include (i) from about 0.2 to about 5 seconds of average residence time, (ii) from about 10 to about 30 m / s peak speed and (iii) from about 0.15 to about 5 kj / kg energy condition, where the second agglomerates are formed; and (b) granulating the agglomerated seconds in one or more fluidizing apparatuses wherein the conditions of each of the fluidizing apparatuses include (i) from about 1 to about 10 minutes of average residence time, (ii) of about 100 at about 300 mm depth of the fluidized bed, (iii) not more than about 50 microns in the size of the dewdrop, (iv) from about 175 to about 250 mm in dew height, (v) from about 0.2 to about 1.4 m / s fluidized speed and (vi) from about 12 to about 100 ° C bed temperature. Also provided are granulated detergent compositions having a high density of at least about 600 g / 1, produced by any of the process modalities described herein. Accordingly, an object of the invention is to provide a method for continuously producing a detergent composition having flexibility with respect to the density of the final products by controlling the energy input, residence time condition, and tip speed condition of the products. mixers It is also an object of the invention to provide a process that is more efficient, flexible and economical to facilitate large-scale production. These and other concomitant objects, features and advantages of the present invention will become apparent to those skilled in the art upon reading the following detailed description of the preferred embodiment and the appended claims.

DETAILED DESCRIPTION OF THE PREFERRED MODALITY The present invention is directed to a process that produces free flowing granular detergent agglomerates having a density of at least about 600 g / 1. The process produces granular detergent agglomerates from an aqueous and / or non-aqueous surfactant which is then coated with fine powders having a diameter of 0.1 to 500 microns, to obtain low density granules.

Process First step (i) [Step (a)] In the first step (i) of the process, a surfactant (s), ie, one or more aqueous surfactants and / or a surfactant are fed into a first mixer. non-aqueous, which are in the form of powder, paste and / or liquid, and fine powders having a diameter of 0.1 to 500 microns, preferably of about 1 to about 100 microns, to make agglomerates. (The definition of surfactants and fine powders is given in detail below). Optionally, an internal powder recirculation stream having a diameter of about 0.1 to about 300 microns generated from the fluidized apparatus (e.g., fluidized bed dryer and / or fluidized bed cooler), may be fed to the mixer in addition to fine powders. The amount of said internal powder recirculation stream may be from 0 to about 60% by weight of the final product. Preferably, grinders that are fixable to the second mixer can be used to break up and separate undesirable oversize agglomerates. Therefore, the process that includes the second mixer with grinders is useful to obtain a reduced amount of agglomerates of excessive size as final products, and said method is a preferred embodiment of the present invention. ? In another embodiment of the invention, the surfactant for the first step (i) may be initially fed into a mixer or pre-mixer (eg, a conventional worm extruder or other similar mixer) before the above, after which the mixed detergent materials are fed into the first mixer as described herein to achieve agglomeration. Generally speaking, preferably the The average residence time of the first mixer is on the scale of about 0.5 to about 15 minutes, and the energy per unit mass of the first mixer (energy condition) is on the scale of about 0.15 kj / kg to about 7 kj / kg, most preferably, the average residence time of the first mixer is from about 30 to about 6 minutes and the energy per unit mass of the first mixer (energy condition) is on the scale of about 0.15 kj / kg to about 4 kj / kg The examples of the first mixer can be any type of mixer known to those skilled in the art, as long as the mixer can maintain the condition mentioned above for the first step. An example can be the Lódige KM mixer manufactured by the company Lódige (Germany). As a result of the first step (i), the agglomerates (first agglomerates) are then obtained. The first agglomerates are then subjected to (1) the second step or (2) the first step (ii), followed by the second step.

First step (ii) [Step (a ') l The product resulting from the first step (i) (ie, the first agglomerates) is fed to a second mixer. The first agglomerates are fed to a second mixer and then finely atomized liquid is sprayed onto the agglomerates in the second mixer. Optionally, an excess of fine powders formed in the first step (i) is added to the first step (ii). If the excess of fine powders is added to the first step (ii), it is useful to spray the finely atomized liquid to bind the excess of fine powders on the surface of the agglomerates. Around 0-10%, most preferably about 2-5% of detergent powdered ingredients of the type used in the first step (i) and / or other detergent ingredients can be added to the second mixer. Speaking generally, preferably the average residence time of the second mixer is on the scale of about 0.2 to about 5 seconds and the tip speed of the second mixer is on the scale of about 10 m / s to about 30 m / s, the energy per unit mass of the second mixer (power condition ) is on the scale from about 0.15 kj / kg to about 5 kj / kg, most preferably, the average residence time of the first mixer is on the scale from about 0.2 to about 5 seconds and the tip speed of the second mixer is at the scale of approximately 10 m / s to approximately 30 m / s, the energy per unit mass of the second mixer (energy condition) is on the scale of from 0.15 kj / kg to about 5 kj / kg, more preferably the average residence time of the second mixer is on the scale of about 0.2 to about 5 seconds, the tip speed of the second mixer is on the scale of about 15 m / sa approximately 26 m / s, the energy per unit mass of the second mixer (energy condition) is on the scale of about 0.2 kj / kg to about 3 kj / kg Examples of the second mixer can be any type of mixer known to those skilled in the art, as long as the mixer can maintain the condition mentioned above for the first step (ii). An example can be the Flexomic model, manufactured by the company Schugi (The Netherlands). As a result of the first step (ii), the second agglomerates are then obtained.

Second step [Step (b) 3 In the second step, the first agglomerates of the first step (i) or the second agglomerates of the first step (ii) are fed to a fluidized apparatus, such as a fluidized bed, to improve the granulation and produce high density, free-flowing granules. The second step may proceed in one or more of a fluidized apparatus (e.g., by combining different types of fluidized devices such as fluidized bed dryer and fluidized bed cooler). Optionally, about 0 to about 10%, most preferably about 2-5% of detergent powder materials of the type used in the first step and / or other detergent ingredients can be added to the second step. Also optionally, from about 0 to about 20%, most preferably from about 2 to about 10% of liquid detergent materials of the type used in the first step (i), the first step (ii) and / or other detergent ingredients can be added at the step, to improve the granulation and to coat on the surface of the granules. Generally speaking, to achieve the density of at least about 600 g / 1, preferably more than 650 g / 1, the conditions of a fluidized apparatus may be: Average residence time: from about 1 to about 10 minutes Depth of the fluidized bed : from about 100 to about 300 mm Dew drop size: not more than about 50 microns Dew height: from about 175 to about 250 mm Fluidized speed: from about 0.2 to about 1.4 m / s Bed temperature: from about 12 at about 100 ° C, most preferably; Average residence time: from about 2 to about 6 minutes Depth of the fluidized bed: from about 100 to about 250 mm Dew drop size: less than about 50 microns Dew height: from about 175 to about 200 mm Fluidizing speed: from about 0.3 to about 1.0 m / s Bed temperature: from about 12 to about 80 ° C. If two different types of fluidized apparatuses are used, the average residence time of the second step j may be in total from about 2 to about 20 minutes, most preferably about 2 to 12 minutes. A coating agent may be added to improve the flowability and / or minimize over-agglomeration of the detergent composition in one or more of the following points of the present process: (1) the coating agent may be added directly after using the cooler or fluid bed dryer; (2) the coating agent can be added between the fluid bed dryer and the fluid bed cooler; and / or (3) the coating agent can be added directly to the fluid bed dryer. The coating agent is preferably selected from the group consisting of aluminosilicates, silicates, carbonates, and mixtures thereof. The coating agent not only improves the free fluidity of the resulting detergent composition, which is desirable by consumers since it allows easy evaluation of the detergent during use, but also serves to control the agglomeration, preventing or minimizing over agglomeration. As those skilled in the art will know, over-agglomeration can lead to very inconvenient flow and aesthetic properties of the final detergent product.

Starting detergent materials The total amount of the surfactants for the present invention, which include the following finally atomized liquid detergent materials and adjunct detergent ingredients, is generally from about 5% to about 60%, more preferably about 12%. % to about 40%, most preferably from about 15% to about 35%, on percentage scales. The surfactants that must be included in the above process can be from any point in the process of the present invention, for example, any of the first step (i), the first step (ii) and / or the second step of the present invention .

Detergent surfactant (aqueous / non-aqueous) The amount of the surfactant of the present process may be from about 5% to about 60%, more preferably from about 12% to about 40%, most preferably from about 15% to about 35%, in the total amount of the final product obtained by the process of the present invention. The surfactant of the present process, which is used as the starting detergent materials mentioned above in the first step, is in the form of paste or powder raw materials. The surfactant itself is preferably selected from anionic, nonionic, zwitterionic, amphoteric and cationic classes, and compatible mixtures thereof. Detergent surfactants useful herein are described in the U.S. patent. 3,664,961, Norris, issued May 23, 1972, and the US patent. 3,929,678, Laughlin et al., Issued December 30, 1975, which are incorporated herein by reference. Useful cationic surfactants also include those described in the U.S. patent. 4,222,905, Cockrell, issued September 16, 1980, and in the US patent. 4,239,659, Murphy, issued December 16, 1980, which are also incorporated herein by reference. Of the surfactants, anionics and nonionics are preferred, with anionics being more preferred. Non-limiting examples of surfactants useful herein include the conventional cll_c18 alkylbenzene sulphonates ("LAS" s), the primary, branched chain and random C 1 -C 8 alkylsulfates ("AS" s), the alkyl sulfates (2,3) secondary of C? o-C18 of the formula CH3 (CH2) x (CHOS03 ~ M +) CH3 and CH3 (CH2) and (CHOS03 ~ M +) CH2CH3 wherein xy (y + 1) are integers of at least about 7, preferably at least about 9, and M is a solubilization cation in water, especially sodium, unsaturated sulfates such as oleylsulfate and the alkylalkoxy sulfates of C? o_ci8 ("AEXS", especially ethoxysulfates EO 1-7). Useful anionic surfactants also include water-soluble salts of 2-acyloxy-alkanesulphonic acids containing about 2 to 9 carbon atoms in the acyl group, and from about 9 to about 23 carbon atoms in the alkane portion; water-soluble salts of olefin sulphonates containing about 12 to 24 carbon atoms; and beta-alkyloxy-alcansulfonates containing from about 1 to about 3 carbon atoms in the alkyl group, and about 8 to 20 carbon atoms in the alkane portion. Optionally, other examples of surfactants useful in the pulp of the invention include C 1 -C 18 alkylalkoxycarboxylates (especially the EO 1-5 ethoxycarboxylates), the glycerol ethers of C 1 -C 4 Q, the alkyl polyglycosides of 3 or 4 g And "their corresponding sulphated polyglycosides, and alphasulfonated fatty acid esters of C ^ -C ^ g ~ s ^ - are desired, the conventional amphoteric and nonionic surfactants such as alkylatoxylates of i2 ~ c18 (" AE ") including the so-called narrow-chain alkyl ethoxylates and Cg-C ?2 alkylphenol-alkoxylates (especially ethoxylates and ethoxy / mixed propoxy), amine oxides of C ± Q-CIQ, and the like, can also be included in the overall compositions. the N-alkyl polyhydroxy fatty acid amides of C ^ n- is- Typical examples include the C-2-C18 N-methylglucamides. See WO 9206154. Other sugar-derived surfactants include the N-alkoxy polyhydroxy fatty acid amides, such as N- (3-methoxypropyl) glucamide of ^ n ~ -] _ g. The N-propyl to N-hexyl glucamides of C ^ -C ^ g can be used for low foam formation. It is also possible to use 5 conventional soaps of C] _Q-C2O- If high foaming is desired, branched-chain C ^ Q-I Q soaps can be used. Mixtures of anionic and nonionic surfactants are especially useful. Other conventional useful surfactants are mentioned in normal texts. Cationic surfactants can also be used as a detergent surfactant herein, and suitable quaternary ammonium surfactants are selected from N-alkyl or alkenylammonium mono- or cycloalkanoic acid surfactants, preferably CQ-C ^ Q in Where the remaining N positions are substituted by methyl, hydroxyethyl or hydroxypropyl groups. Ampholytic surfactants can also be used as the detergent surfactant herein, which include aliphatic derivatives of heterocyclic secondary and tertiary amines; zwitterionic surfactants including derivatives of aliphatic quaternary ammonium, phosphonium and sulfonium compounds; water-soluble salts of esters of fatty acids alphasulfonated; alkyl ether sulfates; water-soluble salts of olefin sulfonates; beta-alkyloxy-alcansulfonates; betaines that have the formula R (R) 2 + R2COO ~ 'wherein R is a hydrocarbyl group of Cg-C ^ g, preferably an alkyl group of c10"c16 ° alkylacylamido group of i6, each R is typically Cj_alkyl -C, preferably methyl, and R2 is a C1-C5 hydrocarbyl group, preferably alkylene group of C] _C3, more preferably an alkylene group of C? -C2 Examples of suitable betaines include coconut acrylamidopropyldimethylbetaine; hexadecyldimethylbetaine; acylamidopropylbetaine; of Ci2 ~ cl '"acylamidohexyldietilbetaine of Cg-C] _4; 4 [C 14-16 acylmethylamidodiethylammonium] carboxybutane; acylamidodimethylbetaine of ^ -C ^; 2_C acrylamidopentanodiethylbetaine?; and acylmethylamidodimethylbetaine of C] _2 ~ 16- The preferred betaines are dimethylammonium hexanoate of 12-I8 and the acylamidopropane (or ethane) dimethyl (or diethyl) betaines of C ^ - ^ 18 • And the sultaines having the formula R (R ) 2 + R2S03 ~ where R is a hydrocarbyl group of Cg-C ^ g, preferably an alkyl group of C ^ oC ^ g, more preferably an alkyl group of Ci2 ~] _3, each R is typically C -C3 alkyl, preferably methyl, and R is a hydrocarbyl group of C ^ -Cg, preferably an alkylene of £ - £ 2 ° > Preferably, a hydroxyalkylene group of C 1 -C 3. Examples of suitable sultaines include dimethylammonium-2-hydroxypropyl sulfonate of c12 ~ < -: 14'-amidopropylammonium-2-hydroxypropyl sultaine of C] _2 ~ i4, dihydroxyethylammonium propanesulfonate of C12-14 and dimethylammonium hexasulfonate of C16 ~ C18 'with amidopropylammonium-2-hydroxypropyl sultaine of 12' ^ I being preferred - fine powders The amount of fine powders of the present process, which are used in the first step, may be from about 94% to 30%, preferably from 86% to 54%, in a total amount of the starting material for the first step. The starting fine powders of the present process are preferably selected from the group consisting of pulverized soda ash, sodium tripolyphosphate powder (STPP), hydrated tripolyphosphate, sodium base sulfate, aluminosilicates, layered crystalline silicates, nitrilotriacetates (NTA), phosphates , precipitated silicates, polymers, carbonates, citrates, powder surfactants (such as powdered alkanesulfonic acids) and recirculated fine particles that occur from the process of the present invention, wherein the average diameter of the powder is from 0.1 to 500 microns, preferably from 1 to 300 microns, more preferably from 5 to 100 microns. In case of using STPP hydrated as fine powders of the present invention, STPP which is hydrated to a level of not less than 50% is preferred: The aluminosilicate ion exchange materials used herein as builder have a high capacity of calcium ion exchange and a high exchange rate. Without being desired to be limited by theory, it is thought that such high capacity and rate of calcium ion exchange is a function of several interrelated factors that are derived from the method by which the aluminosilicate ion exchange material is produced. In this regard, the aluminosilicate ion exchange materials used herein are preferably produced in accordance with Corkill et al., U.S. Pat. No. 4,605,509 (Procter &Gamble), the disclosure of which is incorporated herein by reference. Preferably, the aluminosilicate ion exchange material is in the form of "sodium", since the potassium and hydrogen forms of the present aluminosilicate do not exhibit a capacity and an ion exchange rate as high as provided by the sodium form. Additionally, preferably the aluminosilicate ion exchange material is in dehydrated form to facilitate the production of crisp detergent agglomerates as described herein. The aluminosilicate ion exchange materials used herein preferably have particle size diameters that optimize their effectiveness as builders. The term "particle size diameter", as used herein, represents the average diameter of particle size of a given aluminosilicate ion exchange material determined by conventional analytical techniques, such as microscopic determination and with scanning electron microscopy. (SEM). The preferred particle size diameter of the aluminosilicate is from about 0.1 microns to about 10 microns, more preferably from about 0.5 microns to about 9 microns. Most preferably, the diameter of particle size is from about 1 miera to about 8 micras. Preferably, the aluminosilicate ion exchange material has the formula: Naz [(A102) z (Si02) y] xH20 where z and y are integers of at least 6, the molar ratio of z: y is from about 1 to about 5, and x is from about 10 to about 264. More preferably, the aluminosilicate has the formula: Na12 [(A102) 12 (SiO2) 2 2] xH20 wherein x is from about 20 to about 30, preferably about 27 These preferred aluminosilicates are commercially available, for example, under the designations Zeolite A, Zeolite B and Zeolite X. Alternatively, naturally occurring or synthetically derived aluminosilicate ion exchange materials suitable for use herein can be obtained as described in Krummel et al., US patent No. 3,985,669, the disclosure of which is incorporated herein by reference. The aluminosilicates used herein are further characterized by their ion exchange capacity which is at least about 200 mg hardness equivalent of CaCO3 / g, calculated on an anhydrous basis, and which is preferably on a scale of about 300. to 352 mg hardness equivalents of CaCO3 / g. Additionally, the aluminosilicate ion exchange materials of the present are further characterized by their calcium ion exchange rate, which is at least about 2 grains of Ca ++ / 3.785 liters / minute / gram / 3.785 liters, and more preferably on a scale of about 2 grains of Ca ++ / 3.785 liters / minute / gram / 3.785 liters to about 6 grains of Ca ++ / 3.785 liters / minute / gram / 3.785 liters.

Finely atomized ligule The amount of the finely atomized liquid of the present process may be from about 1% to about 10% (on an active basis), preferably from about 2% to about 6% (on an active basis) in a total amount of the final product obtained by the process of the present invention. The finely atomized liquid of the present process can be selected from the group consisting of liquid ionic or cationic silicate surfactants, which are in liquid form, aqueous or non-aqueous polymer solutions, water, and mixtures thereof. Other optional examples for the finely atomized liquid of the present invention may be a solution of sodium carboxymethylcellulose, polyethylene glycol (PED) and dimethylenetriaminepentamethylphosphonic acid (DETMP) solutions. Preferable examples of the anionic surfactant solutions which can be used as the finely atomized liquid in the present invention are HLAS about 88 to 97% active, NaLAS about 30 to 50% active, solution of AE3S about 28% active, liquid silicate about 40 to 50% active, etc. Cationic surfactants can also be used as the finely atomized liquid herein, and suitable quaternary ammonium surfactants are selected from C-N-alkyl or alkenyl ammonium surfactants. wherein the remaining N positions are substituted by methyl, hydroxyethyl or hydroxypropyl groups. Preferable examples of the aqueous or non-aqueous polymer solutions which can be used as the finely atomized liquid in the present invention are modified polyamines comprising a polyamine base structure corresponding to the formula: H [H 2 N -R] n + 1 - [ IN-R] m- [IN-R] n-NH2 having a modified polyamine formula V (n +?) MYnZ or a polyamine base structure corresponding to the formula: I H R III H2N-R] n-k + 1- CN ~ R] m "tN" R] n "tN ~ R] k" NH2 having a modified polyamine formula (n_] c +?) WmYnY 'i Z, where k is less than or equal to n, said polyamine base structure, prior to modification, has a molecular weight greater than about 200 daltons, wherein: i) units V are terminal units having the formula: EX "ENR- or E-N + -R- or EN? -R- III E E E ii) W units are base structure units that have the formula: iii) units Y are branching units having the formula: EX "-NR- or -N + -R- or -N? -R- III = Y iv) and the units Z are terminal units having the formula: X " wherein the basic structure linker units R are selected from the group consisting of C2-C12 alkylene, 4-C12 'alkenylene 3-C12 hydroxyalkylene, C4-C12 dihydroxyalkylene, C2-C2 dialkylarylene, (R10)? R1-, - (R ^ -OJxR5 (OR1) - ^, - (CH2CH (OR2) CH20) ^ R ^ y -R1- (OCH2CH (OR2) CH2) w-, -C (O) (R4) rC (0) -, -CH2CH (OR2) CH2-, and mixtures thereof, wherein R is C2-C alkylene, and mixtures thereof, R is hydrogen, - (R0) XB, and mixtures thereof, R3 is alkyl of] _C] _, arylalkyl of C7-C12 aryl substituted with alkyl of C -C ^ aryl of Cg-C] _2 and "mixtures thereof; R is alkylene of C? -C?, C4-C12 alkylalene arylalkylene of Cg-C ?, arylene of gC? And mixtures thereof, R5 is alkylene of C] _ C] _, hydroxy alkylene of C3-C ?, dihydroxyalkylene of - C12 / dialkylarylene of Cg-C] _, -C (0) -, -C (0) NHR6NHC (0) -, -R ^ OR1) -, -C (O) (R4) rC (0) -, CH2CH (OH) CH2-, CH2CH (OH) CH20- (R10) and R1OCH2CH (OH) CH2- and mixtures thereof, R is C2-C alkylene] 2 or arylene of Cg-C2, the E units are selected of the group consisting of hydrogen, alkyl, c-c22 alkenyl, 3-C22 arylalkyl, 7-C22 hydroxyalkyl, C2-C22, - (CH) pC02M, - (CH2) qS03M, CH (CH2C02M) C02M, - (CH2) pP03M, - (R10) xB, -C (0) R3, and mixtures thereof; oxide; B is hydrogen, C ^ -Cg alkyl, (CH2) qS03M, - (CH2) pC02M, - (CH2) q (CHSO3M) CH2S03M, - (CH2) q- (CHSO2M) CH2SO3M, - (CH2) pP03M, -PO3M and mixtures thereof; M is hydrogen or a cation soluble in water in an amount sufficient to satisfy the balance of the charge; X is a water-soluble anion, - m has a value from 4 to about 400; n has the value from 0 to about 200; p has the value of 1 to 6, q has the value of 0 to 6; r has the value of 0 or 1; w has the value of 0 or 1, - x has the value of 1 to 100; "y" has the value of 0 to 100; z has the value of 0 or 1. An example of the most preferred polyethylene imines would be a polyethylenimine having a molecular weight of 1800, which is further modified by ethoxylation to a degree of about 7 ethyleneoxy residues per nitrogen (PEI 1800, E7 ). It is preferred that the above polymer solution be premixed with an anionic surfactant such as NaLAS. Other preferred examples of the aqueous or non-aqueous polymer solutions which can be used as the finely atomized liquid in the present invention are polymeric polycarboxylate dispersants which can be prepared by polymerizing or copolymerizing suitable unsaturated monomers, preferably in their acid form. Unsaturated monomeric acids which can be polymerized to form suitable polymeric polycarboxylates include acrylic acid, maleic acid (or maleic anhydride), fumaric acid, itaconic acid, aconitic acid, mesaconic acid, citraconic acid and methylenemalonic acid. The presence, in the polymeric polycarboxylates of the present, of monomeric segments which do not contain carboxylate radicals such as vinyl methyl ether, styrene, ethylene, etc., is suitable, provided that said segments do not constitute more than about 40% by weight. Preferred are homopolymeric polycarboxylates having molecular weights greater than 4000, such as those described below. Particularly suitable homopolymeric polycarboxylates can be derived from acrylic acid. Said polymers based on acrylic acid, which are useful herein, are the water-soluble salts of polymerized acrylic acid: The average molecular weight of said polymers in acid form preferably ranges from more than 4,000 to 10,000, preferably from more than 4,000 to 7,000, and most preferably more than 4,000 to 5,000. The water-soluble salts of said acrylic acid polymers may include, for example, the alkali metal, ammonium and substituted ammonium salts. Copolymeric polycarboxylates such as a copolymer based on acrylic acid / maleic acid can also be used. Such materials include the water-soluble salts of the copolymer of acrylic acid and maleic acid. The average molecular weight of said copolymers in acid form preferably ranges from about 2,000 to 100,000, more preferably from about 5,000 to 75,000, and most preferably from about 7,000 to 65,000. The ratio of acrylate: maleate segments in said copolymers will generally vary from about 30: 1 to about 1: 1, more preferably from about 10: 1 to 2: 1. The water-soluble salts of said acrylic acid-maleic acid copolymers may include, for example, the alkali metal, ammonium and substituted ammonium salts. It is preferred that the above polymer solution be premixed with an anionic surfactant such as LAS.

Attached detergent ingredients The starting detergent material in the present process can include additional detergent ingredients, and / or any number of additional ingredients can be incorporated into the detergent composition during the subsequent steps of the present process. These adjunct ingredients include other detergency builders, bleaches, bleach activators, foaming enhancers, or foam suppressors, anti-rust and anti-corrosion agents, dirt suspending agents, dirt release agents, germicides, pH adjusting agents, alkalinity sources without detergency builder, chelating agents, smectite clays, enzymes, enzyme stabilizing agents, and perfumes. See the US patent. 3,936,537, issued February 3, 1976 to Baskerville, Jr., et al., Incorporated herein by reference. Other detergency builders can generally be selected from the different alkali metal and ammonium or substituted ammonium phosphates, polyphosphates, phosphonates, polyphosphonates, carbonates, borates, polyhydroxysulfonates, polyacetates, carboxylates and polycarboxylates. Alkali metal, especially sodium, salts of the above are preferred. Preferred for use herein are the phosphates, carbonates, fatty acids of C? Or? 8 'polycarboxylates, and mixtures thereof.

More preferred are sodium tripolyphosphate, tetrasodium pyrophosphate, citrate, tartrate, mono- and di-succinates, and mixtures thereof (see below).

Compared to the amorphous sodium silicates, the crystallized sodium silicate laminates exhibit a clearly increased calcium and magnesium ion exchange capacity. In addition, the stratified sodium silicates > they prefer magnesium ions over calcium ions, a necessary feature to ensure that substantially all of the "hardness" is removed from the wash water. However, these layered crystalline sodium silicates are generally more expensive than amorphous silicates, as well as other detergency builders. Consequently, in order to provide an economically feasible laundry detergent, the proportion of the crystalline layered sodium silicates used must be judiciously determined. Said stratified sodium silicates are described in Corkill et al., U.S. No. 4,605,509, previously incorporated herein by reference. Specific examples of inorganic phosphate builders are sodium and potassium tripolyphosphate, pyrophosphate, polymeric metaphosphate having a degree of polymerization of about 6 to 21, and orthophosphates. Examples of polyphosphonate builders are the sodium and potassium salts of ethylene diphosphonic acid, the sodium and potassium salts of ethane 1-hydroxy-l, 1-diphosphonic acid, and the sodium and potassium salts of acid 1, 1, 2 -triphosphonic acid. Other phosphorus builder compounds are described in the U.S. Patents. 3,159,581; 3,213,030; 3,422,021; 3,422,137; 3,400,176 and 3,400,148, all of which are incorporated herein by reference. Examples of inorganic detergency builders no > of phosphorus are tetraborate decahydrate and silicates having a weight ratio of SiO 2: alkali metal oxide of from about 0.5 to about 4.0, preferably from about 1.0 to about 2.4. The non-phosphorus water-soluble organic builders found useful herein include the various alkali metal, ammonium and substituted ammonium polyacetates, carboxylates, polycarboxylates and polyhydroxysulfonates. Examples of polyacetate builders and polycarboxylate builders are the sodium, potassium, lithium, ammonium and substituted ammonium salts of ethylenediaminetetraacetic acid, nitrilotriacetic acid, oxydisuccinic acid, mellitic acid, benzene polycarboxylic acids, and citric acid. Polycarboxylate polymeric detergency builders are described in the U.S. patent. 3,308,067, Diehl, issued March 7, 1967, the disclosure of which is incorporated herein by reference. Such materials include the water-soluble salts of homo- and co-polymers of aliphatic carboxylic acids such as maleic acid, itaconic acid, mesaconic acid, fumaric acid, aconitic acid, citraconic acid and methylenemalonic acid. Some of these materials are useful as the water-soluble anionic polymer as described below, but only if they are in intimate admixture with the non-soap anionic surfactant. Other polycarboxylates suitable for use herein are the polyacetal carboxylates described in the US patent. 4,144,226, issued March 13, 1979 to Crutchfield et al., And the US patent. 4,246,495, issued March 27, 1979 to Crutchfield et al., Which are incorporated herein by reference. These polyacetal carboxylates can be prepared by bringing together under conditions of The polymerization is a glyoxylic acid ester and a polymerization initiator. The resulting polyacetal carboxylate ester is then attached to chemically stable end groups to stabilize the polyacetal carboxylate against rapid depolymerization in alkaline solution, becomes to the corresponding salt, and added to a detergent composition. Particularly preferred polycarboxylate builders are ether carboxylate builder compositions which comprise a combination of tartrate monosuccinate and sodium disuccinate. tartrate disclosed in the US patent. 4,663,071, Bush et al., Issued May 5, 1987, the disclosure of which is incorporated herein by reference. Bleaching agents and activators are described in the U.S. patent. 4,412,934, Chung et al., Issued on 1 November 25, 1983, and in the US patent. 4,483,781, Hartman, issued November 20, 1984, which are incorporated herein by reference. Chelating agents are also described in the U.S. patent. 4,663,071, Bush et al., In column 17, line 54 to column 18, line 68, incorporated herein by reference. The modifiers of foams! they are also optional ingredients, and are described in the US patents. 3,933,672, issued January 20, 1976 to Bartolotta et al., And 4,136,045, issued January 23, 1979 to Gault et al., Which are incorporated herein by reference. Smectite clays suitable for use herein are described in the U.S. patent. 4,762,645, Tucker et al., Issued August 9, 1988, column 6, line 3 to column 7, line 24, incorporated herein by reference. Other builders suitable for use herein are listed in the Baskerville patent, column 13, line 54 to column 16, line 16, and in the U.S. patent. 4,663,071, Bush et al., Issued May 5, 1987, which are incorporated herein by reference.

Optional steps of the procedure Optionally, the method may comprise the step of spraying an additional binder into one or more of the first, second and / or third mixers for the present invention. A binder is added for the purpose of improving agglomeration by providing a "binder" or "adherent" agent for the detergent components. The binder is preferably selected from the group consisting of water, anionic surfactants, non-surface active agents. ionics, liquid silicates, polyethylene glycol, polyvinyl pyrrolidone, polyacrylates, citric acid, and mixtures thereof. Other suitable binding materials including those included herein are described in Beerse et al., U.S. No. 5,108,646 (Procter &Gamble Co.), the disclosure of which is incorporated herein by reference. Other optional steps contemplated by the present method include screening the oversized detergent agglomerates in a screening apparatus that can take various forms including, but not limited to, conventional screens selected for the desired particle size of the finished detergent product. Other optional steps include conditioning the detergent agglomerates by subjecting them to further drying, by the apparatus described above. Another optional step of the present process is to finish the resulting detergent agglomerates by various methods including spraying and / or mixing other conventional detergent ingredients. For example, the finishing step encompasses the spraying of perfumes, brighteners and enzymes onto the finished agglomerates to provide a more complete detergent composition. Said techniques and ingredients are well known in the art. Another optional step in the process includes a method of structuring surfactant paste, for example, curing an aqueous slurry of anionic surfactant, incorporating a paste hardening material by using an extruder, prior to the process of the present invention. invention. The details of the surfactant paste structuring process are described in co-application No. PCT / US96 / 15960 (filed October 4, 1996). To make the present invention more easily understood, reference is made to the following examples, which are intended to be illustrative only and not to be limiting of the present invention.

EXAMPLES EXAMPLE 1 The following is an example for obtaining agglomerates having high density using the Mixer KM Code (KM-600) followed by the Schugi FX-160 mixer, and then followed by the fluid bed apparatus. [Step 1] 120-160 kg / hr of HLAS (an active C9"C18 '95 alkylbenzenesulfonate acid precursor) at about 45-60 ° C is dispersed by the grinders and / or blades of the KM-600 mixer together with 220 kg / hr of STPP powder (average particle size of 40 to 75 microns), 160-280 kg / hr of micronized soda ash (average particle size 15 microns), 80-120 kg / hr of micronized sulphate (size 15 micron particle medium) and 200 kg / hr of recirculated fine particles Saw blades can be used as mixing elements in the KM mixer The shredders for the KM mixer can be used to reduce the amount of oversize agglomerates. The conditions of the KM mixer are as follows: Average residence time: 3 - 6 minutes Power condition: 0.15 - 2 kj / kg Mixer speed: 100 - 150 rpm Cover temperature: 30 - 50 ° C [Step 2] The agglomerates of the mixer KM-600 are fed to the Schug mixer i FX-160. 10 - 20 kg / hr of HLAS (an acidic alkylbenzenesulfonate precursor of C ^ ± -CI Q; 94-97% active) is dispersed as a finely atomized liquid in the Schugi mixer at approximately 50 ° to 60 ° C. Schugi mixer is added 20-80 kg / hr of micronized soda ash (average particle size of approximately 10 - 20 microns).

The Schugi mixer conditions are as follows: Average residence time: 0.2 - 5 seconds Top speed: 16 to 26 m / s Power condition: 0.15 - 2 kj / kg Mixer speed: 2000 - 3200 rpm [Step 3] The agglomerates of the Schugi mixer are fed to a fluidized bed drying apparatus to dry, round and grow the agglomerates. 20-80 kg / hr > of liquid silicate (43% solids, 2.0 R) can also be added in the fluidized bed drying apparatus at 35 ° C. The conditions of the fluidized bed drying apparatus are as follows: Average residence time: 4 - 8 minutes Depth of the non-fluidized bed: 200 mm Dew drop size: less than 50 microns Dew height: 175 - 250 mm (about distributor plate) Fluidized speed: 0.4 - 0.8 m / s Bed temperature: 40 - 70 ° C] The granules resulting from step 3 have a density of approximately 700 g / 1, and can optionally be subjected to optional cooling procedures, configuration and / or spraying.

EXAMPLE 2 The following is an example for obtaining agglomerates having high density using the Mixer KM Code (KM-600), followed by the Schugi FX-160 mixer and then the fluidized bed apparatus.

[Step 1] 15 kg / hr-30 kg / hr of HLAS (an acid precursor of alkylbenzenesulfonate of C] _] _- C] _g; 95% active) at about 45-60 ° C, is dispersed by the grinders and / or blades of the KM-600 mixer together with 220 kg / hr of STPP powder (average particle size of 40 to 75 microns), 160-280 kg / hr of micronized soda ash (average particle size 15 microns), 80-120 kg / hr of micronized sulphate (average particle size of 15 microns) and 200 kg / hr of recirculated fine particles. Serrated blades can be used as mixing elements in the KM mixer. The shredders for the KM mixer can be used to reduce the amount of oversized agglomerates. The conditions of the KM mixer are as follows: Average residence time: 3 - 6 minutes Power condition: 0.15 - 2 kj / kg Mixer speed: 100 - 150 rpm Cover temperature: 30 - 50 ° C [Step 2] The agglomerates of the KM-600 mixer are fed to the Schugi FX-160 mixer. 10-25 kg / hr of neutralized liquid AE3S (25-28% active) are dispersed as a finely atomized liquid in the Schugi mixer at approximately 30-40 ° C. 20-80 kg / hr of soda ash are added to the Schugi mixer. The Schugi mixer conditions are as follows: Average residence time: 0.2 - 5 seconds Tip speed: 16 - 26 m / s Power condition: 0.15 - 2 kj / kg Mixer speed: 2000 - 3200 rpm [Step 3] The agglomerates of the Schugi mixer are fed to a fluidized bed drying apparatus to dry, round and grow the agglomerates. 20-80 kg / hr of liquid silicate (43% solids, 2.0 R) can also be added in the fluidized bed drying apparatus at 35 ° C. The conditions of the fluidized bed drying apparatus are the following: Average residence time: 2-4 minutes Depth of the non-fluidized bed: 200 mm Dewdrop size: less than 50 microns Dew height: 175-250 mm (about distributor plate) Fluidized speed: 0.4 - 0.8 m / s Bed temperature: 40 - 70 ° C] The product of the resulting step 3 has a density of approximately 700 g / 1 and can be subjected to the optional configuration procedure and / or spray.

EXAMPLE 3 The following is an example for obtaining agglomerates having high density using the Mixer KM (KM-600), followed by the fluid bed apparatus for additional granulates.

[Step 1] 250 - 270 kg / hr of coconut fatty alcohol sulfate aqueous surfactant paste (C] _2-?, 71. 5% active), 40-80 kg / hr of HLAS (an acid precursor of alkylbenzenesulfonate of Cn-C ^ g; 94-97% active) are fed to a KM-600 mixer together with 220 kg / hr of STPP powder (average particle size of 40 to 75 microns), 160-200 kg / hr of micronised soda ash (average particle size 15 microns), 80-120 kg / hr of micronised sulfate (average particle size of 15 microns) and 200 kg / hr of recirculated fine particles. The surfactant paste is fed at about 40-52 ° C, and the powders are fed at room temperature. The shredders for the KM mixer can be used to reduce the amount of oversized agglomerates. The conditions of the KM mixer are as follows: Average residence time: 3 - 6 minutes Power condition: 0.15 - 2 kj / kg Mixer speed: 100 - 150 rpm Cover temperature: 30 - 50 ° C [Step 2] The agglomerates of the mixer KM are fed to a fluidized bed drying apparatus to dry, round and grow the agglomerates. 20-80 kg / hr of liquid silicate (43% solids, 2.0 R) can also be added in the fluidized bed drying apparatus at 35 ° C. The conditions of the fluidized bed drying apparatus are as follows: Average residence time: 2-4 minutes Depth of the non-fluidized bed: 200 mm Dew drop size: less than 50 microns Dew height: 175-250 mm (about distributor plate) Fluidized speed: 0.4 - 0.8 m / s Bed temperature: 40 - 70 ° C The granules resulting from step 3 have a density of approximately 700 g / 1, and can optionally undergo optional cooling procedures, configuration and / or spray. Having thus described the invention in detail, it will be apparent to those skilled in the art that various changes can be made without departing from the scope of the invention, and that the latter should not be considered to be limited to what is described in the specification.

Claims (10)

NOVELTY OF THE INVENTION CLAIMS

1. - A non-tower process for preparing a granular detergent composition having a density of at least about 600 g / 1, comprising the steps of: (a) dispersing a surfactant and coating the surfactant with fine powders that have a diameter of 0.1 to 500 microns, in a mixer in which mixer conditions include (i) from about 0.5 to about 15 minutes of average residence time and (ii) from about 0.15 to about 7 kj / kg of energy condition, where the agglomerates are formed; and (b) granulating the agglomerates in one or more fluidizing apparatuses wherein the conditions of each of the fluidizing apparatuses include (i) from about 1 to about 10 minutes of average residence time, (ii) of about 100 to about 300 mm depth of the fluidized bed, (iii) no more than about 50 microns of spray drop size, (iv) from about 175 to about 250 mm spray height, (v) from about 0.2 to about 1.4 m / s of fluidized speed and (vi) from about 12 to about 100 ° C bed temperature. 2. A non-tower process for preparing a granular detergent composition having a density of at least about 600 g / 1, comprising the steps of: (a) dispersing a surfactant and coating the surfactant with powders fines that have a diameter of 0.1 to 500 microns, in a mixer in which the conditions of > mixer include (i) from about 0.5 to about 15 minutes of average residence time and (ii) from about 0.15 to about 7 kj / kg energy condition, where the first agglomerates are formed; (a1) spraying a finely atomized liquid on the first agglomerates in

WHAT a mixer in which mixer conditions include (i) from about 0.2 to about 5 seconds of average residence time, (ii) from about 10 to about 30 m / s top speed and (iii) from around 0.15 to about 5 kj / kg condition of 15 energy, where the second agglomerates are formed; and (b) granulating the agglomerated seconds in one or more fluidized fluid apparatuses wherein the conditions of each of the fluidized apparatuses include (i) from about 1 to about 10 minutes of average residence time, (ii) 20 about 100 to about 300 mm depth of the fluidized bed, (iii) no more than about 50 microns of spray drop size, (iv) about 175 to about 250 mm spray height, (v) about 0.2 to approximately 1.4 m / s speed of 25 fluidized and (vi) from about 12 to about 100 ° C bed temperature.

3. - The method according to claim 1 or 2, further characterized in that said surfactant is selected from the group consisting of anionic surfactant, nonionic surfactant, cationic surfactant, zwitterionic surfactant, ampholytic surfactant and mixtures thereof .

4. The process according to claim 1 or 2, further characterized in that said surfactant is selected from the group consisting of alkylbenzenesulfonates, alkylalkoxy sulfates, alkylethoxylates, alkyl sulfates, coconut fatty alcohol sulfates and mixtures thereof.

5. The process according to claim 1 or 2, further characterized in that an aqueous or nonaqueous polymer solution is dispersed with said surfactant in step (a).

6. - The process according to claim 1 or 2, further characterized in that the fine powders are selected from the group consisting of sodium carbonate, sodium tripolyphosphate powder, hydrated tripolyphosphate, sodium sulfates, aluminosilicates, layered crystalline silicates, phosphates, precipitated silicates, polymers, carbonates, citrates, nitrilotriacetates, powder surfactants and mixtures thereof.

7. - The method according to claim 1 or 2, further characterized in that a stream of internal recirculation of the powder of the fluidizing apparatus is also added to step (a).

8. - The process according to claim 2, further characterized in that the finely atomized liquid is selected from the group consisting of liquid silicates, anionic surfactants, cationic surfactants, aqueous polymer solutions, non-aqueous polymer solutions, water and mixtures of the same.

9. The process according to claim 2, further characterized in that fine powders are formed in excess in step (a), and in which excess fine powders are added to step (a ').

10. A granular detergent composition made in accordance with the method of claims 1 or 2.