CA2267291C

CA2267291C - Process for making a low density detergent composition by non-tower process

Info

Publication number: CA2267291C
Application number: CA002267291A
Authority: CA
Inventors: Manivannan Kandasamy; Angela Gloria Del Greco
Original assignee: Procter and Gamble Co
Current assignee: Procter and Gamble Co
Priority date: 1996-10-04
Filing date: 1996-10-04
Publication date: 2002-12-10
Anticipated expiration: 2016-10-04
Also published as: CA2267424A1; CN1239995A; CA2268060A1; ATE255159T1; EP0929649B1; CN1156560C; CA2268068A1; CA2268067C; JP2000503715A; EP0929655A1; BR9712490A; BR9711861A; ES2178778T3; CA2268063A1; JP3299985B2; DE69723986D1; BR9612732A; CA2268063C; JP2000503716A; CN1133738C

Abstract

A non-tower process for continuously preparing granular detergent compositio n having a low density, preferably about 300 g/l to about 600 g/l is provided. The process comprises the steps of (a)(i) dispersing an aqueous or non-aqueous surfactant, and (ii) coating the surfactant with fine powders having a diameter from 0.1 to 500 microns, in the mixer which is operated under certain conditions to obtain irregular shape granules and excessive fine powders and, (b) spraying on finely atomized liquid to the irregular shape granules and excessive fine powders from step (a), in a mixer which is operated under certain conditions to bind the excessive fine powders onto the irregular-shaped granules.

Description

_1_ PROCESS FOR MAKING A LOW DENSITY DETERGENT COMPOSITION BY NON
TOWER PROCESS
FIELD OF THE INVENTION
The present invention generally relates to a non-tower process for producing a low L0 density 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 into a series of mixers. The process produces a free flowing, detergent composition whose density can be adjusted for wide range of consumer needs, and which can be commercially sold.
IS
BACKGROUND OF THE INVENTION
Recently, there has been considerable interest within the detergent industry for laundry detergents which are "compact" and therefore, have low dosage volumes. To facilitate production of these so-called low dosage detergents, many attempts have been made to produce 20 high bulk density detergents, for example with a density of 600 g/1 or higher. The low dosage detergents are currently in high demand as they conserve resources and can be sold in small packages which are more convenient for consumers. However, the extent to which modern detergent products need to be "compact" in nature remains unsettled. In fact, many consumers, especially in developing countries, continue to prefer a higher dosage levels in their respective 25 laundering operations. One characteristic common to the existing process for producing modern detergent composition by agglomeration, namely, non-tower process, is that the apparent density of the granules by such process is typically not less than 600 g/1.
Consequently, there is a need in the art of agglomeration (e.g., non-tower process) to produce modern detergent compositions for flexibility in the ultimate density of the final composition, especially for the low density (for 30 example, the range of the density is from about 300g/1 to about 600 g/1).
- Generally, there are three primary types of processes by which detergent granules or powders can be prepared. The first type of process involves spray-drying an aqueous detergent slurry in a spray-drying tower to produce highly porous detergent granules (e.g., tower process for low density detergent compositions). The second type of process involves spray-drying an 35 aqueous detergent slung in a spray-drying tower as the first step, then, the resultant granules are WO 98/14549 PCTlUS96/15881 _2_ agglomerated with a binder such as a nonionic or anionic surfactant, finally, various detergent components are dry mixed to produce detergent granules (e.g., tower process plus agglomeration process for high density detergent compositions) . In the third type of process, the various detergent components are dry mixed after which they are agglomerated with a binder such as a nonionic or anionic surfactant, to produce high density detergent compositions (e.g., agglomeration process for high density detergent compositions). In the above three processes, the important factors which govern the density of the resulting detergent granules are the shape, porosity and particle size distribution of said granules, the density of the various starting materials, the shape of the various starting materials, and their respective chemical composition.
There have been many attempts in the art for providing processes which increase the density of detergent granules or powders. Particular attention has been given to densification of spray-dried granules by post tower treatment. For example, one attempt involves a batch process in which spray-dried or granulated detergent powders containing sodium tripolyphosphate and sodium sulfate are densified and spheronized in a Marumerizer~. This apparatus comprises a substantially horizontal, roughened, rotatable table positioned within and at the base .of a substantially vertical, smooth walled cylinder. This process, however, is essentially a batch process and is therefore less suitable for the large scale production of detergent powders. More recently, other attempts have been made to provide continuous processes for increasing the density of "post-tower" or spray dried detergent granules. Typically, such processes require a first apparatus which pulverizes or grinds the granules and a second apparatus which increases the density of the pulverized granules by agglomeration. While these processes achieve the desired increase in density by treating or densifying "post tower" or spray dried granules, they are limited in their ability to go higher in surfactant active level without subsequent coating step.
In addition, treating or densifying by "post tower" is not favourable in terms of economics (high capital cost) and complexity of operation. Moreover, all of the aforementioned processes are directed primarily for densifying or otherwise processing spray dried granules. Currently, the relative amounts and types of materials subjected to spray drying processes in the production of detergent granules has been limited. For example, it has been difficult to attain high levels of surfactant in the resulting detergent composition, a feature which facilitates production of detergents in a more efficient manner. Thus, it would be desirable to have a process by which detergent compositions can be produced without having the limitations imposed by conventional spray drying techniques.
To that end, the art is also replete with disclosures of processes which entail agglomerating detergent compositions. For example, attempts have been made to agglomerate detergent builders by mixing zeolite and/or layered silicates in a mixer to form free flowing agglomerates. While 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 into crisp, free flowing detergent agglomerates having low densities.
Accordingly, there remains a need in the art to have an agglomeration (non-tower) process for continuously producing a detergent composition having low density delivered directly from starting detergent ingredients, and preferably the density can be achieved by adjusting the process condition. Also, there remains a need for such a process which is more efficient, flexible and economical to facilitate large-scale production of detergents for flexibility in the ultimate density of the final composition.
BACKGROUND ART
The following references are directed to densifying spray-dried granules:
Appel et al, U.S. Patent No. 5,133,924 (Lever); Bortolotti et al, U.S. Patent No. 5,160,657 (Lever); Johnson et al, British patent No. /,S 17,713 (Unilever); and Curtis, European Patent Application 451,894.
The following references are directed to producing detergents by agglomeration: Charles et al, U. S. Patent No. 4,992,079 (FMC Corporation), Beujean et al, Laid-open No.W093/23,523 (Henkel), Beerse et al, U.S. Patent No. 5,108,646 (Procter & Gamble); Capeci et al, U.S. Patent No. 5,366,652 (Procter & Gamble); H.ollingsworth et al, European Patent Application 351,937 (Unilever); and Swatling et al, U.S. Patent No. 5,205,958.
For example, the Laid-open No.W093l23,523 describes the process comprising pre-agglomeration by a low speed mixer and further agglomeration step by high speed mixer for obtaining high density detergent composition with less than 25 wt % of the granules having a diameter over 2 mm. This disclosure also describes a process by which the density of the final agglomerate can be adjusted by adjusting the amount of liquid binder added in the second mixer.
It is not clear from the disclosure on what contributes to the density reduction. The process in Laid-open No. W093/23,523 differs from the invention disclosed herein which will be apparent to those skilled in the art.
The U. S. Patent No. 4,992,079 describes agglomeration process for low density non-phosphate detergents having increased resistance to non ionic bleeding. The first process step agglomerates detergent ingredients with non aqueous liquid surfactant. The first step is, followed by a second agglomeration step where the surfactant loaded particles are dispersed into an inert gaseous medium, wetting the dispersed particles with atomized stream of aqueous sodium silicate or with separate atomized streams of water and concentrated sodium silicate to form the agglomerate detergent. It is not clear from the disclosure on what contributes to the low density.

In addition, the disclosure does not include aqueous surfactants and phosphate containing detergents. The process in the U.S. Patent No. 4,992,079 differs from the invention disclosed herein which will be apparent to those skilled in the art.

The present invention meets the aforementioned needs in the art by providing a process which produces a low density granular detergent composition. The present invention also meets the aforementioned needs in the art by providing a process which produces a granular detergent composition for flexibility in the ultimate density of the final composition from agglomeration (e.g., non-tower) process. The process of the proposed invention has capability of adjusting the density of the granules of the composition by controlling shape of the granules. Namely, the process of the present invention can be applied to obtain a granular detergent composition which has low density (e.g., irregular-shaped granules having a density from about 300 to about 600 g/1). The process does not use the conventional spray drying towers currently which is limited in producing high surfactant loading compositions.
In addition, the process of the present invention is more efficient, economical and flexible with regard to the variety of detergent compositions which can be produced in the process.
Moreover, the process is more amenable to environmental concerns in that it does not use spray drying towers which typically emit particulates 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 "irregular-shaped granules" refers to particles wherein the shape of the granules having irregular shape in the case of low density formed by agglomerating starting detergent materials, fine powders and finely atomized liquid. All percentages used herein are expressed as "percent-by-weight" unless indicated otherwise.
In accordance with one aspect of the invention, there is provided a non-tower process for preparing a granular detergent composition having a density from about 300 g/1 to about 550 g/1, comprising the steps of (a) (i) dispersing an aqueous or non-aqueous surfactant, and (ii) coating the surfactant with fine powders having a diameter from 0.1 to 500 microns, in a mixer to obtain irregular-shaped granules, wherein conditions of the mixer include (1) from about 5 to about 15 seconds of mean residence time, (2) from about 5 to about 10 m/s of tip speed, (3) from about 0.15 to about 4.2 kj/kg of energy condition;

-4a-(b) spraying finely atomized liquid onto the irregular-shaped granules and excessive fine powders from step (a), in a second mixer to bind the excessive fme powders on the irregular-shaped granules, wherein conditions of the mixer include (1) from about 0.2 to about 5 seconds of mean residence time, (2) from 13 to about 23 m/s of tip speed, (3) from about 0.15 to about 2.9 kj/kg of energy condition.

WJ-Also provided are the granular detergent compositions having a low density preferably from about 300 g/1 to about 600g/1, produced by any one of the process embodiments described herein.
Accordingly, it is an object of the invention fo provide a process for continuously producing a detergent composition which has flexibility with respect to density of the final products by controlling energy input, residence time condition, and tip speed condition in the mixers. It is also an object of the invention to provide a process which is more efficient, flexible and economical to facilitate large-scale production of detergents of low as well as high dosage levels. These and other objects, features and attendant advantages of the present invention will become apparent to those skilled in the art from a reading of the following detailed description of the preferred embodiment and the appended claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG.1 is a photograph showing irregular-shaped agglomerates after the first step of the process of the present invention, having low density (about 475 - 530 g/1 ).
FIG.2 is a photograph showing irregular-shaped agglomerates after the first and the second steps of the present invention, having low density (about 475 - 500 g/1).
F1G.3 is a photograph showing irregular-shaped agglomerates after the first and the second steps of the present invention and drying and cooling process, having low density (about 450 - 475 g/1).
FIG.4 is a photograph showing round-shaped agglomerates after agglomeration process for obtaining high density {about 700-800 g/1).
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The present invention is directed to a process which produces free flowing, granular detergent agglomerates having a low density of not less than about 300 g/1, preferably from about 300 to about 600 g/1. The process produces granular detergent agglomerates from an aqueous or non-aqueous surfactant which is then coated with fine powders having a diameter from 0.1 to 500 microns, in order to obtain low density granules.
Pry First Sten In the first step of the process, one or more of aqueous or non-aqueous surfactants) which is/are in the form of powder, paste or liquid, and fine powders having a diameter from 0.1 to 500 microns, preferably from about 1 to about 100 microns are fed into the mixer. (The definition of the surfactants and the fine powders are described in detail hereinafter.) . In another embodiment of the invention which is discussed more fully below, the surfactants) can be initially fed into a mixer or pre-mixer (e.g. a conventional screw extruder or other similar mixer) prior to agglomeration, after which the mixed detergent materials are fed into the first step mixer as described herein for agglomeration.
Generally speaking, to achieve the low density (from about 300 g/1 to about 600 g/1), preferably, the mean residence time in the mixer is from about 5 to about 30 seconds and tip speed for the mixer is in range from about 5 m/s to about 10 m/s, the energy per unit mass in the mixer is from about 0.15 kj/kg to about 4.20 kj/kg, more preferably, the mean residence time in the mixer is from about 10 to about 15 seconds and tip speed for the mixer is in range from about 6 mls to about 8 m/s, the energy per unit mass for the mixer is from about 0.15 kj/kg to I S about 2.5 kjJkg, and most preferably, the mean residence time in the mixer is from about 10 to about 15 seconds and tip speed for the mixer is in range from about 6.5 m/s to about 7.5 m/s, the energy per unit mass for the mixer is from about 0.15 kj/kg to about 1:30 kj/kg.
The examples of mixers for the first step can be any types of mixer known to the skilled in the art, as long as the mixer can maintain the above mentioned condition for the first step. An Example can be Lodige CB Mixer manufactured by the LISdige Company (Germany).
As the result of the first step, granules having fine powders on the surface of the granules can be obtained (FIG. I ).
Second Step In the second step of the process, the resultant product of the first step (granules and excess fine powders) is fed into a second mixer, and then finely atomized liquid is sprayed on the granules in the mixer. In order to bind the excessive fine powders onto the granules from the first step, about 0-10% , more preferably about 2-S% of powder detergent ingredients of the kind used in the first step and/or other detergent ingredients can be added to the second step.
Generally speaking, to achieve the low density (from about 300 g/1 to about 600 g/1), preferably, the mean residence time of the mixer for the second step is from about 0.2 to about 5 seconds and tip speed of the mixer for the second step is in range from about 10 m/s to about 23 m/s, the energy per unit mass for the mixer (energy condition) for the second step is from about 0.15 kj/kg to about 2.9 kj/kg, more preferably, the mean residence time of the mixer is from about 0.5 to about 2 seconds and tip speed for the mixer is in range from about t3 m/s to about 20 m/s, the energy per unit mass for the mixer from about 0.15 kj/kg to about 1.9 kj/kg, the most preferably, the mean residence time in the mixer is from about 0.5 to about 2 seconds, tip speed for the mixer is in range from about 15 m/s to about 17.5 m/s, the energy per unit mass for the mixer is from about 0.15 kj/kg to about 1.0 kj/kg.
The examples of mixers for the second step can be any types of mixer known to the skilled in the art, as long as the mixer can maintain the above mentioned condition for the first step. An Example can be Flexomic Model manufactured by the Schugi Company (Netherlands).
As the result of the second step, granular detergent composition can be obtained (FIG. 2).
The process in the present invention surprisingly reduce the amount of excess recycle fines from the second step, comparing to the amount of excess recycle fines due to common agglomeration processes known to the skilled in the art. The existence of excess fines leads to excessive recycle streams which disrupt the process and are therefore not economically favourable.
According to the present invention, recycle fines from the second step will typically comprise from about 10 % to 40 % of the total amount of fine powders used in the first step.
Starting Detergent Materials The total amount of the surfactants for the present invention, which are included in the following detergent materials, finely atomized liquid and adjunct detergent ingredients is generally from about 5 % to about 60 %, more preferably from about 12% to about 40 %, more preferably, from about 15 to about 35%, in total amount of the final product obtained by the process of the present invention. The surfactants which should be included in the above can be from any part of the process of the present invention., e.g., from either one of the first step or the second step, or both steps of the present invention.
Detereent Surfactant (Agueous /Non-actueous) The amount of the aqueous or non-aqueous surfactant of the present process can be from about 5 % to about b0 %, more preferably from about 12% to about 40 %, more preferably, from about I S to about 35%, in total amount of the final product obtained by the process of the present invention.
The aqueous or non-aqueous surfactant of the present process, which is used as the above mentioned starting detergent materials in the first step, is in the form of powdered or pasted raw materials.
The surfactant itself is preferably selected from anionic, nonionic, zwitterionic, ampholytic and cationic classes and compatible mixtures thereof. Detergent surfactants useful -$-herein are described in U.S. Patent 3,6ti4,961, Norris, issued May 23, 1972;
and in U.S. Patent 3,929,678, Laughlin et al., issued December 30, 1975. Useful cationic surfactants also include those described in U.S. Patent 4,222,905, Cockrell, issued September 16, 1980, and in U.S. Patent 4,239,659, Murphy, issued December 16, 1980. Of the surfactants, anionics and nonionics are preferred and avionics are most preferred.
Nonlimiting examples of the preferred anionic surfactants useful in the present invention include the conventional CI l-Clg alkyl benzene sulfonates {"LAS"), primary, branched-chain and random C 1 p-C2p alkyl sulfates ("AS"), the C I p-C 1 g secondary (2,3) alkyl sulfates of the formula CH3(CH2)x(CHOS03 M+) CH3 and CH3 (CH2)y(CHOS03-M+) CH2CH3 where x and (y + 1 ) are integers of at least about 7, preferably at least about 9, and M is a water-solubilizing cation, especially sodium, unsaturated sulfates such as oleyl sulfate, and the CIQ-Clg alkyl alkoxy sulfates ("AEXS"; especially EO 1-7 ethoxy sulfates).
Useful anionic surfactants also include water-soluble salts of 2-acyloxy-alkane-1 sulfonic acids containing from about 2 to 9 carbon atoms in the acyl group and from about 9 to about 23 carbon atoms in the alkane moiety; water-soluble salts of olefin sulfonates containing from about 12 to 24 carbon atoms; and beta-alkyloxy alkane sulfonates containing from about t to 3 carbon atoms in the alkyl group and from about 8 to 20 carbon atoms in the alkane moiety .
Optionally, other exemplary surfactants useful in the paste of the invention include C I p-C I g alkyl alkoxy carboxylates (especially the EO 1-5 ethoxycarboxyiates), the C 10-18 glycerol ethers, the C 1 p-C 1 g alkyl polygiycosides and the corresponding sulfated polyglycosides, and C12-Clg alpha-sulfonated fatty acid esters. If desired, the conventional nonionic and amphoteric surfactants such as the C 12-C 1 g alkyl ethoxylates ("AE") including the so-called narrow peaked alkyl ethoxylates and C6-C 12 alkyl phenol alkoxyiates (especially ethoxylates and mixed ethoxy/propoxy), C I p-C I g amine oxides, and the like, can also be included in the overall compositions. The C 1 p-C I g N-alkyl polyhydroxy fatty acid amides can also be used. Typical examples include the C 12-C 1 g N-methylglucamides. See WO 92/06154.
Other sugar-derived surfactants include the N-alkoxy polyhydroxy fatty acid amides, such as C I p-C I g N-(3-methoxypropyl) glucamide. The N-propyl through N-hexyl Cl2-C
I g glucamides can be used for low sudsing. C 1 p-C2p conventional soaps may also be used. if high sudsing is desired, the branched-chain Clp-C16 soaps may be used. Mixtures of anionic and nonionic surfactants are especially useful. Other conventional useful surfactants are listed in standard texts.
Cationic surfactants can also be used as a detergent surfactant herein and suitable quaternary ammonium surfactants are selected from mono C6-C i (, preferably C6-C 1 p N-alkyl _g_ or alkenyl ammonium surfactants wherein remaining N positions are substituted by methyl, hydroxyethyl or hydroxypropyl groups.
Ampholytic surfactants can also be used as a detergent surfactant herein, which include aliphatic derivatives of heterocyclic secondary and tertiary amines;
zwitterionic S surfactants which include derivatives of aliphatic quaternary ammonium, phosphonium and sulfonium compounds; water-soluble salts of esters of alpha-sulfonated fatty acids; alkyl ether sulfates; water-soluble salts of olefin sulfonates; beta-alkyloxy alkane sulfonates; betaines having the formula R(RI)2N+R2C00-, wherein R is a C6-Clg hydrocarby) group, preferably a C I 0-C 16 alkyl group or C 1 p-C 16 acylamido alkyl group, each R 1 is typically C 1-C3 alkyl, preferably methyl and R2 is a C 1-CS hydrocarbyl group, preferably a C 1-C3 alkylene group, more preferably a C1-C2 alkylene group. Examples of suitable betaines include coconut acylamidopropyldimethyl betaine; hexadecyl dimethyl betaine; C 12_ 14 .
acylamidopropylbetaine; Cg_14 acylamidohexyldiethyl betaine; 4[C14-16 - acylmethylamidodiethylammonio]-1-carboxybutane; C16_lg acylamidodimethylbetaine;
C12-i6 acylamidopentanediethylbetaine; and [C12-16 acylmethylamidodimethylbetaine. Preferred betaines are C12-18 dimethyl-ammonio hexanoate and the C10-18 acylamidopropane (or ethane) dimethyl (or diethyl) betaines; and the sultaines having the formula (R(RI)2N+R2S03- wherein R is a C6-Clg hydrocarbyl group, preferably a C 10-C 16 alkyl group, more preferably a C 1,2-C 13 alkyl group, each R 1 is typically C 1-C3 alkyl, preferably methyl, and R2 is a C 1-C6 hydrocarbyl group, preferably a CI-C3 alkylene or, preferably, hydroxyalkylene group. Examples of suitable sultaines include C 12-C ~ 4 dimethylammonio-2-hydroxypropyl sulfonate, C 12-C 14 amido propyl ammonio-2-hydroxypropyl sultaine, C 12-C 14 dihydroxyethylammonio propane sulfonate, and dimethylammonio hexane sulfonate, with C12-14 amido propyl ammonio-2-hydroxypropyl sultaine being preferred.
Fine Powders The amount of the fine powders of the present process, which is used in the first step, can be from about 94% to 30%, preferably from 86% to 54%, in total amount of starting material for the first step . The starting fine powders of the present process preferably selected from the group consisting of ground soda ash, powdered sodium tripolyphosphate (STPP), hydrated tripolyphosphate, ground sodium sulphates, aluminosilicates, crystalline layered silicates, nitrilotriacetates (NTA), phosphates, precipitated silicates, polymers, carbonates, citrates, powdered surfactants (such as powdered alkane sulfonic acids) and recycle fines occurring 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 the case of using hydrated STPP as the fine powders of the present invention, STPP
which is hydrated to a level of not less than 50% is preferable. The aluminosilicate ion exchange materials used herein as a detergent builder preferably have both a high calcium ion exchange capacity and a high exchange rate. Without intending to be limited by theory, it is believed that such high calcium ion exchange rate and capacity are a function of several interrelated factors which derive from the method by which the aluminosilicate ion exchange material is produced. In that regard, the aluminosilicate ion exchange materials used herein are preferably produced in accordance with Corkill et al, U.S. Patent No.
4,605,509 (Procter &
Gamble).
Preferably, the aluminosilicate ion exchange material is in "sodium" form since the potassium and hydrogen forms of the instant aluminosilicate do not exhibit as high of an exchange rate and capacity as provided by the sodium form. Additionally, the aluminosilicate ion exchange material preferably is in over dried form so as to facilitate production of crisp detergent agglomerates as described herein. The aluminosilicate ion exchange materials used herein preferably have particle size diameters which optimize their effectiveness as detergent builders. The term "particle size diameter" as used herein represents the average particle size diameter of a given aluminosilicate ion exchange material as determined by conventional analytical techniques, such as microscopic determination and scanning electron microscope (SEM). The preferred particle size diameter of the aluminosilicate is from about 0.1 micron to about 10 microns, more preferably from about 0.5 microns to about 9 microns.
Most preferably, the particle size diameter is from about 1 microns to about 8 microns.
Preferably, the aluminosilicate ion exchange material has the formula Naz~(Ai02)z~(St02~,1xH20 wherein z and y are integers of at least 6, 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 has the formula Nal2[(A102)12.(Si02)12)~20 wherein x is from about 20 to about 30, preferably about 27. These preferred aluminosilicates are available commercially, for example under designations Zeolite A, Zeolite B and Zeolite X.
Alternatively, naturally-occurring or synthetically derived aluminosilicate ion exchange materials suitable for use herein can be made as described in Krummel et al, U.S. Patent No.
3,985,669.
The aluminosilicates used herein are further characterized by their ion exchange capacity which is at least about 200 mg equivalent of CaC03 hardnesslgram, calculated on an anhydrous basis, and which is preferably in a range from about 300 to 352 mg equivalent of CaC03 hardness/gram. Additionally, the instant aluminosilicate ion exchange materials are still further characterized by their calcium ion exchange rate which is at least about 2 grains Ca++/gallon/minute/-gram/gailon, and more preferably in a range from about 2 grains Ca~/gallon/minute/-gram/gallon to about 6 grains Ca'~'/gallon/minute/-gram/gallon.
Finely Atomized Liquid The amount of the finely atomized liquid of the present process, which is used in the second step, can be from about 1 % to about 10% (active basis), preferably from 2% to about 6% (active basis) in total amount of the final product obtained by the process of the present IO invention. The finely atomized liquid of the present process can be selected from the group consisting of liquid silicate, anionic or cationic surfactants which are in liquid form, aqueous or non-aqueous polymer solutions, water and mixtures thereof. The aqueous or non-aqueous polymer solution is dispersed with the surfactant in step (a)(i). Other optional examples for the finely atomized liquid of the present invention can be sodium carboxy methyl cellulose solution, polyethylene glycol I 5 (PEG), and solutions of dimethylene triamine pentamethyl phosphoric acid (DETMP).
The preferable examples of the anionic surfactant solutions which can be used as the finely atomized liquid in the present inventions are about 88 - 97% active I3L,AS, about 30 -50% active NaLAS, about 28% active AE3S solution, about 40-50% active liquid silicate, and so on.
20 Cationic surfactants can also be used as finely atomized liquid herein and suitable quaternary ammonium surfactants are selected from mono C6-C 16, preferably C6-C 10 N-alkyl or alkenyl ammonium surfactants wherein 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 25 as the finely atomized liquid in the present inventions are modified polyamines which comprise a poiyamine backbone corresponding to the formula:
IH~-~rn-'~-I~1-~-IN-~n-~
having a modified polyamine formula V(n+1)WmYnZ or a polyamine backbone 30 corresponding to the formula:
f~-~rrk+rf~~rn-f~'t~rr--f~~k-r~-h having a modified polyamine formula V(n-k+1)WmYn1'~kZ~ wherein k is less than or equal to n, said polyamine backbone prior to modification has a molecular weight greater than about 200 daltons, wherein i) V units are terminal units having the formula:
FX- p?, E-N-R- or ~N=F~- or ~rv-R-E E E
ii) W units are backbone units having the formula:
E X_ -N-~ or -N~ ~ or -N-F~-iii) Y units are branching units having the formula:
X
or -(~ f~-- or - i -R-and iv) Z units are terminal units having the formula:
X
-N-E or E
wherein backbone linking R units are selected from the group consisting of C2-C 12 alkylene, C4-C 12 alkenylene, C3-C 12 hydroxyalkylene, C4-C 12 dihydroxy-alkylene, Cg-C

dialkylarylene, -(R10)xRl-, -(R10)xRS(ORI)x-, -(CH2CH(OR2)CH20)Z(R 1 O)yR I (OCH2CH(OR2)CH2~,-, -C(O)(R4)rC(O)-, -CH2CH(OR2)CH2-, and mixtures thereof; wherein RI is C2-C6 alkylene and mixtures thereof; R2 is hydrogen, -(R10)xB, and mixtures thereof; R3 is CI-Clg alkyl, C~-C12 aryfalkyl, C~-C 12 alkyl substituted aryl, C6-C 12 aryl, and mixtures thereof;
R4 is C 1-C 12 alkylene, C4-C I 2 alkenylene, Cg-C 12 arylalkylene, C6-C 1 p arylene, and mixtures thereof; RS is C I-C 12 aikylene, C3-C 12 hydroxyalkylene, C4-C 12 dihydroxy-alkylene, Cg-C
l2 dialkylarylene, -C(O)-, -C(O)NHR6NHC(O)-, -R1(OR1)-, -C(O)(R4)rC(O)-, -CH2CH(OH)CH2-, -CH2CH(OH)CH20(R10)yR10CH2CH(OH)CH2-, and mixtures thereof; R6 is C2-CI2 alkylene or C6-C12 arylene; E units are selected from the group consisting of hydrogen, CI-C22 alkyl, C3-C22 alkenyl, C~-C22 arylalkyl, C2-C22 hydroxyalkyl, -(CH2)pC02M, -(CH2)qS03M, -CH(CH2C02M)C02M, -(CH2)pP03M, -(R10)xB, -C(O)R3, and mixtures thereof oxide; B
is hydrogen, C1-C6 alkyl, -(CH2)qS03M, -(CH2)pC02M, -(CH2)q(CHS03M)CH2S03M, -(CH2)q-(CHS02M)CH2S03M, -(CH2)pP03M, -P03M, and mixtures thereof; M is hydrogen or a water soluble cation in sufficient amount to satisfy charge balance; X is a water soluble anion;
m has the value from 4 to about 400; n has the value from 0 to about 200; p has the value from 1 to 6, q has the value from 0 to 6; r has the value of 0 or 1; w has the value 0 or 1; x has the value from 1 to 100; y has the value from 0 to 100; z has the value 0 or 1. One example of the most preferred potyethyleneimines would be a polyethyleneimine having a molecular weight of 1800 which is further modified by ethoxylation to a degree of approximately 7 ethyleneoxy residues per nitrogen (PEI 1800, E7). It is preferable for the above polymer solution to be pre-complex with anionic surfactant such as NaLAS.
Other preferable examples of the aqueous or non-aqueous polymer solutions which can be used as the finely atomized liquid in the present inventions are polymeric polycarboxylate dispersants which can be prepared by polymerizing or copolymerizing suitable unsaturated monomers, preferably in their acid form. Unsaturated monomeric acids that can be polymerized to form suitable polymeric polycarboxylates include acrylic acid, malefic acid (or malefic anhydride), fumaric acid, itaconic acid, aconitic acid, mesaconic acid, citraconic acid and methylenemalonic acid. The presence in the polymeric polycarboxylates herein of monomeric segments, containing no carboxylate radicals such as vinylmethyl ether, styrene, ethylene, etc. is suitable provided that such segments do not constitute more than about 40% by weight.
Homo-polymeric polycarboxylates which have molecular weights above 4000, such as described next are preferred. Particularly suitable homo-polymeric polycarboxylates can be derived from acrylic acid. Such acrylic acid-based polymers which are useful herein are the water-soluble salts of polymerized acrylic acid. The average molecular weight of such polymers in the acid form preferably ranges from above 4,000 to 10,000, preferably from above 4,000 to 7,000, and most preferably from above 4,000 to 5,000. Water-soluble salts of such acrylic acid polymers can include, for example, the alkali metal, ammonium and substituted ammonium salts.
Co-polymeric polycarboxylates such as a Acrylic/maleic-based copolymers may also be used. Such materials include the water-soluble salts of copolymers of acrylic acid and malefic acid. The average molecular weight of such copolymers in the acid form preferably ranges from about 2,000 to 100,000, more preferably from about 5,000 to 75,000, most preferably from about 7,000 to 65,000. The ratio of acrylate to maleate segments in such copolymers will generally range from about 30:1 to about 1:1, more preferably from about 10:1 to 2:1.
Water-soluble salts of such acrylic acid/maleic acid copolymers can include, for example, the alkali metal, ammonium and substituted ammonium salts. It is preferable for the above polymer solution to be pre-complexed with anionic surfactant such as LAS .
Adjunct Deterstent Inttredients The starting detergent material in the present process can include additional detergent ingredients and/or, any number of additional ingredients can be incorporated in the detergent composition during subsequent steps of the present process. These adjunct ingredients include other detergency builders, bleaches, bleach activators, suds boosters or suds suppressors, anti-tarnish and anticorrosion agents, soil suspending agents, soil release agents, germicides, pH
adjusting agents, non-builder alkalinity sources, chelating agents, smectite clays, enzymes, I S enzyme-stabilizing agents and perfumes. See U.S. Patent 3,936,S37, issued February 3, 1976 to Baskerviile, Jr. et al.
Other builders can be generally selected from the various water-soluble, alkali metal, ammonium or substituted ammonium phosphates, polyphosphates, phosphonates, polyphosphonates, carbonates, borates, polyhydroxy sulfonates, polyacetates, carboxylates, and polycarboxylates. Preferred are the alkali metal, especially sodium, salts of the above.
Preferred for use herein are the phosphates, carbonates, C 10-lg fatty acids, polycarboxylates, and mixtures thereof. More preferred are sodium tripolyphosphate, tetrasodium pyrophosphate, citrate, tartrate mono- and di-succinates, and mixtures thereof (see below).
In comparison with amorphous sodium silicates, crystalline layered sodium silicates exhibit a clearly increased calcium and magnesium ion exchange capacity. In addition, the layered sodium silicates prefer magnesium ions over calcium ions, a feature necessary to insure that substantially all of the "hardness" is removed from the wash water. These crystalline layered sodium silicates, however, are generally more expensive than amorphous silicates as well as other builders. Accordingly, in order to provide an economically feasible laundry detergent, the proportion of crystalline layered sodium silicates used must be determined judiciously.
The crystalline layered sodium silicates suitable for use herein preferably have the formula NaMSixO2x+1 ~YH2~

-~~J-wherein M is sodium or hydrogen, x is from about 1.9 to about 4 and y is from about 0 to about 20. More preferably, the crystalline layered sodium silicate has the formula NaMSi205.yH20 wherein M is sodium or hydrogen, and y is from about 0 to about 20. These and other crystalline layered sodium silicates are discussed in Corkill et al, U.S.
Patent No. 4,605,509.
Specific examples of inorganic phosphate builders are sodium and potassium tripolyphosphate, pyrophosphate, polymeric metaphosphate having a degree of polymerization of from 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 ethane, 1,1,2-triphosphonic acid. Other phosphorus builder compounds are disclosed in U.S. Patents 3,159,581; 3,213,030; 3,422,021; 3,422,137; 3,400,176 and 3,400,148.
Examples of nonphosphorus, inorganic builders are tetraborate decahydrate and silicates having a weight ratio of Si02 to alkali metal oxide of from about 0.5 to about 4.0, preferably from about 1.0 to about 2.4. Water-soluble, nonphosphorus organic builders useful herein include the various alkali metal, ammonium and substituted ammonium polyacetates, carboxylates, polycarboxylates and polyhydroxy sulfonates. Examples of polyacetate and polycarboxylate builders are the sodium, potassium, lithium, ammonium and substituted ammonium salts of ethylene diamine tetraacetie acid, nitrilotriacetic acid, oxydisuccinic acid, mellitic acid, benzene polycarboxylic acids, and citric acid.
Polymeric polycarboxylate builders are set forth in U.S.
Patent 3,308,067, Diehl, issued March 7, 1967. Such materials include the water soluble salts of homo- and copolymers of aliphatic carboxylic acids such as malefic acid, itaconic acid, mesaconic acid, fumaric acid, aconitic acid, citraconic acid and methylene malonic acid. Some of these materials are useful as the water-soluble anionic polymer as hereinafter described, but only if in intimate admixture with the non-soap anionic surfactant.
Other suitable polycarboxylates for use herein are the polyacetal carboxylates described in U.S. Patent 4,144,226, issued March 13, 1979 to Crutchfield et al, and U.S.
Patent 4,246,495, issued March 27, 1979 to Crutchfield et al.
These polyacetal carboxylates can be prepared by bringing together under polymerization conditions an ester of glyoxylic acid 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, converted to the corresponding salt, and added to a detergent composition. Particularly preferred polycarboxylate builders are the ether carboxylate builder compositions comprising a combination of tartrate monosuccinate and tartrate disuccinate described in U.S. Patent 4,663,071, Bush et al., issued May 5, 1987.
Bleaching agents and activators are described in U.S. Patent 4,412,934, Chung et al., issued November 1, 1983, and in U.S. Patent 4,483,781, Hartman, issued November 20,1984.
Chelating agents are also described in U.S. Patent 4,663,071, Bush et al., from Column 17, line 54 through Column 18, line 68. Suds modifiers are also optional ingredients and are described in U.S. Patents 3,933,672, issued January 20, 1976 to Bartoletta et al., and 4,136,045, issued January 23, 1979 to Gault et al.
Suitable smectite clays for use herein are described in U.S. Patent 4,762,645, Tucker et al, issued August 9, 1988, Column 6, line 3 through Column 7, line 24.
I S Suitable additional detergency builders for use herein are enumerated in the Baskerville patent, Column 13, line 54 through Column 16, line 16, and in U.S.
Patent 4,663,071, Hush et al, issued May 5, 1987.
As for a comparison to the present invention, a photograph of high density agglomerates (an average density is about 700 - 800g/1) obtained by a series of the mixers operated under different conditions from the present invention is shown as F1G. 4. For F1G.
4, Liidige CB
mixer (CB-30, operated at 550 RPM), then Schugi Flexomic mixer (operated at 2800RPM),finally Lodige KM mixer (KM-600, operated at 100 RPM with normal plows) were used for agglomeration. The material used for obtaining agglomerates of F1G.4 is the same as Example 2, filly described in the "EXAMPLES".
Ootiona) Process Steps One optional step in the process is drying, if it is desired to reduce level of moisture in the agglomerates from the second step. This can be accomplished by a variety of apparatus, well known to these skilled in the art. Fluid bed apparatus is preferred, and will be referred to in the discussion which follows.
In another optional step of the present process, the detergent agglomerates exiting the fluid bed dryer are further conditioned by additional cooling in cooling apparatus. The preferred apparatus is a fluid bed. Another optional process step involves adding a coating agent to improve flowability and/or minimize over agglomeration of the detergent composition in one or more of the following locations of the instant process: ( 1 ) the coating agent can be added -t7-directly after the fluid bed cooler or dryer; (2) the coating agent may be added between the fluid bed dryer and the fluid bed cooler; (3) the coating agent may be added between the fluid bed dryer and a moderate speed mixer for agglomeration which is commonly known to the skilled in the art ; and/or (4) the coating agent may be added directly to a moderate speed mixer for agglomeration which is commonly known to the skilled in the art and 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 enhances the free flowability of the resulting detergent composition which is desirable by consumers in that it permits easy scooping for detergent during use, but also serves to control agglomeration by preventing or minimizing over agglomeration, especially when added directly to the moderate speed mixer. As those skilled in the art are well aware, over agglomeration can lead to very undesirable flow properties and aesthetics of the final detergent product.
Optionally, the process can comprise the step of spraying an additional binder in one or both of the first and second mixers for the present invention or fluid bed dryers and/or fluid bed coolers. A binder is added for purposes of enhancing agglomeration by providing a "binding" or "sticking" age~t for the detergent components. The binder is preferably selected from the group consisting of water, anionic surfactants, nonionic surfactants, liquid silicates, polyethylene glycol, polyvinyl pyrrolidone polyacrylates, citric acid and mixtures thereof.
Other suitable binder materials including those listed herein are described in Beerse et al, U.S. Patent No.
5,108,646 (Procter & Gamble Co.).
Other optional steps contemplated by the present process include screening the oversized detergent agglomerates in a screening apparatus which can take a variety of forms including but not limited to conventional screens chosen for the desired particle size of the finished detergent product. Other optional steps include conditioning of the detergent agglomerates by subjecting the agglomerates to additional drying by way of apparatus discussed previously.
Another optional step of the instant process entails finishing the resulting detergent agglomerates by a variety of processes including spraying and/or admixing other conventional detergent ingredients. For example, the finishing step ~ encompasses spraying perfumes, brighteners and enzymes onto the finished agglomerates to provide a more complete detergent composition. Such techniques and ingredients are well known in the art.
The representative examples of the series of mixers to make granular detergent compositions according to the process of the present invention plus optional processes are as follows:
A. ( 1 )agglomeration in Lt3dige CH Model--(2) and then in Schugi Flexomic Model --(3) sizing in a Mogensens sizer to remover panicles over 4.5 mm --(4) drying in a Fluid Bed Dryer --(5) cooling in a Fluid Bed Cooler --(6) sizing in a Mogensen sizer to remove over 1.2 mm --(7) grinding to reduce over size agglomerates from the sizers-- and (8) feeding ground agglomerates back to the fluid bed dryer or fluid bed cooler or Lbdige CB mixer;
B. (1) agglomeration in Lodige CB Model--(2) then in Lddige KM Model-(3) further in Schugi Flexomic Model --(4) sizing in a Mogensens sizer to remove panicles over 4.5 mm ---(5) drying in a Fluid Bed Dryer -=(6) cooling in a Fluid Hed Cooler-- (7) sizing in a Mogensen sizer to remove over 1.2 mm --(8) grinding to reduce over size agglomerates from the sizers-- and (9) feeding ground agglomerates back to the fluid bed dryer or fluid bed cooler or Ltidige CB mixer.
The other essential step in the process involves high active paste structuring process, e.g., hardening an aqueous anionic surfactant paste by incorporating a paste-hardening material by using an extruder, prior to the process of the present invention. The details of the high active paste structuring process is disclosed in CA 2,268,057.
In order to make the present invention more readily understood, reference is made to the following examples, which are intended to be illustrative only and not intended to be limiting in scope.
EXAMPLES
Example 1: (lrreaular-shayed aQalomerates after the first step of the present invention) The following is an example for obtaining agglomerates using only Lodige CB
mixer (CB-30) followed by fluid bed dryer (FBD), fluid bed cooler (FBC), then sizing and grinding.
The 259 kg/hr of aqueous coconut fatty alcohol sulfate surfactant paste (71.5%
active) is dispersed by the pin tools of a CB-30 mixer along with the 217 kglhr of powder STPP (mean particle size of 40 - 75 microns), the 169 kg/hr of micronized soda ash (mean particle size of 5 - 30 microns), the 103 kg/hr of micronized sulfate (mean particle size of 5 -30 microns), and the 288 kg/hr of recycle fines. The surfactant paste is fed at about 40 to 55°C, and the powders are fed at room temperature. The condition of the CB-30 mixer is as follows:
Mean residence time : 14-20 seconds Tip speed : 6.5 to 7.0 m/s Energy condition : 0.15 to 1.0 kj/kg After the agglomeration, bed temperature of the FBD is maintained between 40 -60 °C and bed temperature of the FBC is maintained between 15 - 30 °C.
The resulting granules have density of 475 - 530 g/1 (Figure 1 ). The level of fines after CB 30 mixer is 30 - 50% vs. target 25%.

Example 2: (Irregular-shaped agglomerates obtained after the first and second steps of the present invention) The following is an example for obtaining agglomerates using Lodige CB mixer (CB
30), then Schugi Flexomic mixer, followed by fluid bed dryer (FBD), fluid bed cooler (FBC), then sizing and grinding (e.g., the process and the material contents are the same as Example 1 , except for adding an agglomeration step by Schugi Flexomic mixer after the agglomeration step by Lodige CB mixer).
The agglomerates from the CB-30 mixer are fed to the Schugi Flexomic mixer.
The 30 kg/hr of HLAS is atomized and sprayed in the Schugi Flexomic mixer. The condition of the Schugi mixer is as follows:
Mean residence time : 0.5 to 2 seconds Tip speed : I S to 18 m/s Energy condition : 0.15 to 1.0 kj/kg i S Resulting granules after Schugi mixer have density of 475-500 g/1 (Figure 2), and resulting granules after sizing and grinding have the density of 450 - 475 g/1 (Figure 3). The level of fines from the Schugi Flexomic mixer is 22 - 30%.
Example 3: (Irregular-shat~eda~1omerates obtained from the process of the present invention The following is an example for obtaining agglomerates using Lodige CB mixer (CB-30), then Schugi Flexomic mixer, followed by fluid bed cooler (FBC), then sizing and grinding.
The 220 kg/hr of non aqueous Linear alkyl Benzene Sulfonic acid (94 - 96%
active) is dispersed by the pin tools of a CB-30 mixer along with the 300 kg/hr of powder STPP
(mean particle size of 40 - 75 microns), the 230 kg/hr of micronized soda ash (mean particle size of 5 - 30 microns), the 100 kg/hr of micronized sulfate (mean particle size of 5 - 30 microns), the 90 kg/hr of Zeolite and the 100 kg/hr of recycle fines. The surfactant is fed at about 40 to 55°C, and the powders are fed at room temperature. The condition of the CB-30 mixer is as follows:
Mean residence time : 10 - 18 seconds Tip speed : 6 to 13 m/s Energy condition : 0.15 to 3.5 kj/kg The agglomerates from the CB-30 mixer are fed to the Schugi Flexomic mixer.
The 30 kg/hr of HLAS is atomized and sprayed in the Schugi Flexomic mixer and 20 kg/hr of carbonate is added to the Schugi mixer. The condition of the Schugi mixer is as follows:
Mean residence time : 0.5 to 2 seconds Tip speed : 15 to 18 m/s Energy condition : 0.15 to 1.0 kj/kg Resulting granules after Schugi mixer and after sizing and grinding have the density of S00 - 550 g/1.
Example 4: (IrreQUlar-shayed agglomerates obtained from the process of the present invention) The following is an example for obtaining agglomerates using Lodige CB mixer (CB-30), then Lodige KM mixer (KM-600) and Schugi Flexomic mixer, followed by fluid bed cooler (FBC), then sizing and grinding The 220 kg/hr of non aqueous Linear alkyl Benzene Sulfonic acid (94 - 96%
active) is dispersed by the pin tools of a CB-30 mixer along with 300 kg/hr of powder STPP (Mean particle size of 40 - 75 microns), 230 kg/hr of micronized soda ash (5 - 30 microns), 100 kg/hr of micronized sulfate (5 - 30 microns), 90 kg/hr of Zeolite and fines recycle of 100 kg/hr. The surfactant is fed at about 40 to SSC, and the powders are fed at room temperature. The condition of the CB-30 mixer is as follows:
Mean residence time : 10 - 18 seconds Tip speed : 6 to 13 m/s Energy condition : 0.15 to 3.5 kj/kg The agglomerates from the CB mixer is charged to a KM-Mixer where a retention is about 40 - 60 kgs. The plow RPM is 100 and chopper RPM is 1300 (three choppers are on the mixer). The agglomerates from the KM-Mixer have the density of 750 - 800 g/1.
The agglomerates from the KM-Mixer are fed to a Schugi Flexomix (FX-160) mixer.
The 30 kg/hr of HLAS is atomized and sprayed in the Schugi Flexomic mixer and 20 kg/hr of carbonate is added to the Schugi mixer. The condition of the Schugi mixer is as follows:
Mean residence time : 0.5 to 2 seconds Tip speed : 1 S to I 8 m/s Energy condition : 0.15 to 1.0 kj/kg Resulting granules after Schugi mixer and after sizing and grinding have the density of about 600 g/1.
Having thus described the invention in detail, it will be obvious to those skilled in the art that various changes may be made without departing from the scope of the invention and the invention is not to be considered limited to what is described in the specification.

Claims

CLAIMS:

1. A non-tower process for preparing a granular detergent composition having a density from about 300 g/l to about 550 g/l, comprising the steps of:
(a) (i) dispersing an aqueous or non-aqueous surfactant, and (ii) coating the surfactant with fine powders having a diameter from 0.1 to 500 microns, in a mixer to obtain irregular-shaped granules, wherein conditions of the mixer include (1) from about 5 to about 15 seconds of mean residence time, (2) from about 5 to about 10 m/s of tip speed, (3) from about 0.15 to about 4.2 kj/kg of energy condition;
(b) spraying finely atomized liquid onto the irregular-shaped granules and excessive fine powders from step (a), in a second mixer to bind the excessive fine powders on the irregular-shaped granules, wherein conditions of the mixer include (1) from about 0.2 to about 5 seconds of mean residence time, (2) from 13 to about 23 m/s of tip speed, (3) from about 0.15 to about 2.9 kj/kg of energy condition.

2. The process according to claim 1 wherein said surfactant is selected from the group consisting of anionic surfactant, nonionic surfactant, cationic surfactant, zwitterionic, ampholytic and mixtures thereof.

3. The process according to claim 1 wherein said surfactant is selected from the group consisting of alkyl benzene sulfonates, alkyl alkoxy sulfates, alkyl ethoxylates, alkyl sulfates, coconut fatty alcohol sulfates and mixtures thereof.

4. The process according to claim 1 wherein an aqueous or non-aqueous polymer solution is dispersed with said surfactant in step (a) (i).

5. The process according to claim 1 wherein the fine powders is selected from the group consisting of soda ash, powdered sodium tripolyphosphate, hydrated tripolyphosphate, sodium sulphates, aluminosilicates, crystalline layered silicates, phosphates, precipitated silicates, polymers, carbonates, citrates, nitrilotriacetates (NTA), powdered surfactants, recycle fine powders from the step (b) and mixtures thereof.

6. The process according to claim 1 wherein 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 thereof.

7. The process according to claim 1 wherein the mean residence time in the mixer of step (a) is in the range from about 10 seconds to about 15 seconds, the tip speed of said mixer is in the range from about 6 m/s to about 8 m/s, and the range of the energy condition of said mixer is from about 0.15 kj/kg to about 2.5 kj/kg.

8. The process according to claim 1 wherein the mean residence time in the mixer of step (b) is in the range from about 0.5 seconds to about 2 seconds, the tip speed of said mixer is in the range from 13 m/s to about 20 m/s, and the range of the energy condition of said mixer is from about 0.15 kj/kg to about 1.9 kj/kg.

9. The process according to claim 1 wherein the total amount of recycle fine powders from the result of step (b) in total amount of the fine powders for step (a) is from about 10% to about 40%.

10. The process according to claim 1 wherein the fine powder is sodium tripolyphosphate which is hydrated at the level of not less than 50%.

11. The process according to claim 1 wherein the total amount of surfactants is from about 5% to about 60% of the final composition.