MXPA99003201A - 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, while wetting the surfactant coated with the fine powder with finely atomized liquid, in a mixer, and (b) thoroughly mixing the agglomerates in a mixer. Step (b) can also be followed by further step (c), i. e., granulating the agglomerates from step (b) in one or more fluidizing apparatus.

Description

PROCEDURE TO MAKE A COMPOSITION DETERGENT BY A PROCEDURE THAT IS NOT A 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, the density of which 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 / l 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 three 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 dry blended, 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 surfactant in the resulting detergent composition, a feature that facilitates the production of detergents more efficiently. Thus, it would be convenient to have a method by which detergent compositions can be produced without having the limitations imposed by 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 builders by mixing zeolite and / or layered silicates 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 effectively agglomerate into crisp and free-flowing detergent 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 and others, patent of? .U. No. 5,108,646 (Procter &Gamble); Capeci et al., Patent of E.U. No. 5,366,652 (Procter &Gamble); Hollings orth et al., European patent application 351 937 (Unilever); Swatling et al., US patent. No. 5,205,958; Dhale adikar 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 cake formation and oversized agglomerates. 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 (eg, irregularly shaped granules having a density of about 300 to about 600 g / l). 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 formed particles / 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 (kg / hr) All percentages used herein they are expressed as "percent by weight", unless otherwise indicated. All relationships are weight ratios unless otherwise indicated. As used herein, "comprises" means that other steps and other ingredients may be added that do not affect the result. This term encompasses the terms "consisting of" and "consisting essentially of". According to one aspect of the invention, there is provided a process for preparing a granular detergent composition having a density of at least about 600 g / l. The method comprises the steps of: (a) dispersing a surfactant and coating the surfactant with fine powders having a diameter of 0.1 to 500 microns, wetting the surfactant coated with the fine powders with finely atomized liquid, in a mixer in which 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 about 0.15 to about 5 kj / kg of energy condition, where the agglomerates are formed; (b) completely mixing the first agglomerates in a mixer where the conditions of the 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 of energy condition . A process for preparing a granular detergent composition having a density of at least about 600 g / l 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, wetting the surfactant coated with the fine powders with finely atomized liquid, in a mixer in which the conditions 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 first agglomerates are formed; (b) completely mixing the first agglomerates in a mixer where the conditions of the 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 of energy condition , where second agglomerates are formed; and (c) granulating the agglomerated seconds in one or more fluidizing apparatuses wherein the conditions of each of the fluidizing apparatuses include (i) of about 1 to about 10 minutes of average residence time, (ii) of about 100 at 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 fluidized speed and (vi) from about 12 to about 100 ° C bed temperature. Also provided are granular detergent compositions having a density of at least about 600 g / l, 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 / l. 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 TPaso (aH) In the first step of the process, a surfactant (s), ie one or more aqueous and / or non-aqueous surfactants which are in powder form, are fed into a first mixer. , 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 During the process, the surface of the surfactant that is coated by the fine powders It is moistened by a finely atomized liquid to add more fine powders to the surface of the agglomerates. (The definition of surfactants and fine powders is given in detail below.) Optionally, a stream of internal recirculation of powders having a diameter of about 0.1 to about 300 microns generated from the fluidizing apparatus (e.g., fluidized bed dryer and / or fluidized bed cooler), can be fed to the mixer in addition to the fine powders. The amount of said internal powder recirculation stream may be from 0 to about 60% by weight of the final product. In another embodiment of the invention, the surfactant for the first step can be initially fed into a mixer or premixer (eg, a conventional worm extruder or other similar mixer) before the above, after which the mixed detergent materials they are fed into the mixer of the first step as described herein to achieve agglomeration. Generally speaking, preferably the average residence time in the first mixer is on the scale of about 0.2 to about 5 seconds, and the tip speed of the first mixer is on the scale of about 10 m / s to about 30 m / s, the energy per unit mass of the first mixer (energy condition) is about 0.15 kj / kg to about 5 kj / kg, most preferably, the average residence time of the first mixer is on the scale of about 0.2 to about 5 seconds, and the tip speed of the first mixer is on the scale of about 10 m / s to about 30 m / s, the energy per unit mass of the first mixer (power condition) is on the scale of about 0.15 kj / kg to about 5 kj / kg, and most preferably, the average residence time of the first mixer is in the range of about 0.2 to about 5 seconds, and the tip speed of the first mixer is on the scale of about 15 m / s to about 26 m / s, and the energy per unit mass of the first mixer (power condition) is on the scale of about 0.2 kj / kg to about 3 kj / kg . Examples of the 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 Flexomic model, manufactured by the company Schugi (The Netherlands). As a result of the first step, the first agglomerates are obtained.

Second step TPaso (b) 1 The product resulting from the first step (ie, the first agglomerates) is fed to a second mixer. Namely, the first agglomerates are mixed and subjected to shear stress completely to round and grow the agglomerates in the second mixer. Optionally, about 0-10%, most preferably about 2-5% of detergent powdered ingredients of the type used in the first step and / or other detergent ingredients can be added to the second step. Preferably, shredders that are fixable to the third mixer can be used to break up and separate undesirable oversized agglomerates. Therefore, the process that includes the second mixer with grinders is useful to obtain a reduced amount of oversize agglomerates as final products, and said method is a preferred embodiment of the present ntion. Generally speaking, preferably the average residence time of the second mixer is on the scale of about 0.5 to about 15 minutes, and the energy per unit mass of the second mixer (energy condition) is on the scale of about 0.15 to about 7 kj / kg, most preferably, the average residence time of the second mixer is in the range of about 3 to about 6 minutes and the energy per unit mass of the second mixer (energy condition) is about 0.15 kj / kg at approximately 4 kj / kg. The 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 second step. An example can be the Lódige KM mixer manufactured by the company Lódige (Germany). As a result of the second step, the second agglomerates with round shape are then obtained.

Third step TPaso (c) 1 If the second agglomerates measure less than 600 g / l, or if the additional agglomeration is preferred to satisfy the optimum condition as the final product of the process of the present invention, the second agglomerates are fed to an apparatus fluidized, such as a fluidized bed, to further improve the granulation and produce high density, free-flowing granules. The third step may proceed in one or more of a fluidized apparatus (e.g., by combining different types of fluidized apparatuses 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, about 0 to about 20%, most preferably about 2 to about 10% of liquid detergent materials of the type used in the first step, the second step and / or other detergent ingredients can be added to the step, to improve the granulation and coating on the surface of the granules. Generally speaking, to achieve the density of at least about 600 g / l, preferably more than 650 g / l, 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 to about 100 ° C, most preferably; Average residence time: from about 2 to about 6 minutes Depth of the fluidized bed: from about 100 to approximately 250 mm Dew drop size: less than approximately 50 microns Dew height: from approximately 175 to approximately 200 mm Fluidizing velocity: from approximately 0.3 to approximately 1.0 m / s Bed temperature: from approximately 12 to approximately 80 ° C. If two different types of fluidized apparatuses are used, the average residence time of the third step can 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 the over-aeration 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 use the fluid bed cooler or 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 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, the second step and / or the third 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 sulfonates ("LAS"), the C10-C20 ("AS") primary alkyl, branched chain and random alkyl sulphates, the secondary alkyl sulfates (2.3) C? O_cl8 of formula CH3 (CH2) x (CHOS03"M +) CH3 and CH3 (CH2) and (CHOS03 ~ M +) CH CH3 f where xy (y +1) are integers of at least about 7, preferably at least about 9, and M is a cation for solubilization in water, especially sodium, unsaturated sulfates such as oleyl sulfate and the C 1 or C 8 alkylalkoxysulfates ("AEXS", especially ethoxysulfates EO 1-7). Useful anionic surfactants also include water-soluble salts of 2-acyloxy-alkane-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 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 paste of the invention include C] _o-Ci8 alkylalkoxycarboxylates (especially the EO 1-5 ethoxycarboxylates), the glycerol ethers of the C 1 or C 8 alkyl polyglycosides and their corresponding sulfated polyglycosides, and aliphatic acid fatty acid esters of C.sub.Cis.substituted, the conventional amphoteric and nonionic surfactants such as 12-C18 alkyl ethoxylates ("AE") including the so-called narrow peak alkyl ethoxylates and the Cg- alkylphenolalkoxylates. C] ^ (especially ethoxylates and ethoxy / mixed propoxy), amine oxides of C ^ Q -C ^ Q, and the like, can also be included in the overall compositions. The N-alkyl polyhydroxy fatty acid amides of -CIQ can also be used. Typical examples include the N-methylglucamides of Ci2_ci8- See WO 9,206,154. Other surfactants derived from sugar include the N-alkoxy polyhydroxy fatty acid amides, such as N (3-methoxypropyl) glucamide from IQ-CIS- The N-propyl to N-hexyl glucamides of Ci2-Ci8 can be used for a low formation of foams. Conventional C? N-C20 soaps can also be used. If high foaming is desired, branched chain C? Or? Ci6 soaps can be used. Mixtures of anionic and nonionic surfactants are especially useful. Other conventional useful surfactants are mentioned in normal texts. Cationic surfactants may also be used as a detergent surfactant herein, and suitable quaternary ammonium surfactants are selected from N-alkyl or alkenyl ammonium surfactants of Cg-C ^ g, preferably Cg-C ^ n wherein 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 alphasulfonated fatty acids; alkyl ether sulfates; water-soluble salts of olefin sulfonates; beta-alkyloxy-alcansulfonates; betaines having the formula RÍR1) 2N + R2COO- / wherein R is a C -Cis hydrocarbyl group, preferably an alkyl group of 10"c16 ° Ci-Cig alkylacylamido group, each R1 is typically C1-C3 alkyl, preferably methyl, and R2 is a C1-C5 hydrocarbyl group, preferably C1-C3 alkylene group, more preferably an alkylene group of C1-C2.

Examples of suitable betaines include coconut acylamidopropyl dimethylbetaine; hexadecyldimethylbetaine; Ci2-Cl4-acylamidopropylbetaine "C8-C14-acylamidohexyldiethylbetaine; 4 [C1-1'-1'-carboxybutane acylmethylamidodiethylammonium; Ci6-c18-acylamido dimethylbetaine"; Ci2-Cl6 acylamidopentadiene-ethylbetaine>; And Ci2-16 acylmethylamidodimethylbetaine. Preferred betaines are C12-18 dimethylammonium hexanoate and the acylamidopropane (or ethane) dimethyl (or diethyl) betaines of CIQ-c18; And the sultaines having the formula R R1) 2N + R2S03 ~ wherein R is a hydrocarbyl group of CQ -C ^ Q, preferably an alkyl group of CiQ-C ^ g ^ more preferably a C12-C13 alkyl group, each R1 is typically C3-alkyl, preferably methyl, and R2 is a Ci-Cg hydrocarbyl group, preferably a C1-C3 alkylene or, preferably, a C1-C3 hydroxyalkylene group. Examples of suitable sultaines include dimethylammonium-2-hydroxypropyl sulfonate of Ci2-Ci4, amidopropylammonium-2-hydroxypropyl sultaine of Ci2 ~ ci4 / dihydroxyethylammonium propanesulfonate of Ci2-C! I4 and dimethylammonium hexasulfonate of C16-C18 'with amidopropylammonium-2- being preferred hydroxypropyl sultaine of Ci2_cl4- 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 He passed. 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. While not wishing to be limited by theory, it is thought that such high capacity and rate of calcium ion exchange are 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 "sodium" form, 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 dry 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) and] 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) 12] 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 Pat. 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 liquid The amount of the finely atomized liquid of the present process can be from about 1% to about 10% (on an active basis), preferably from about 2% to about 6% (on an active base) 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 (PEG) and dimethylenetriaminepentamethylphosphonic acid (DETMP) solutions. Preferable examples of the anionic surfactant solutions that 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 may also be used as the finely atomized liquid herein, and suitable quaternary ammonium surfactants are selected from N-alkyl or alkenyl ammonium surfactants of C -C or, 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 finely atomized liquid in the present invention are modified polyamines. > which comprise a polyamine base structure corresponding to the formula: H 15 [H 2 N -R] n + 1 - [N IR] m- [Ni-R] n-NH 2 having a modified polyamine formula V (n +? ) WmYnZ or a polyamine base structure corresponding to the formula: HR 20 H2N-R] n-k +? - [N IR] m- [NI-R] n- [NI-R] k-NH2 having a modified polyamine formula (n _]? + I) W ^^ Y '^ z, where k is less than or equal to n, said polyamine base structure, before modification, has a weight Molecular molecule greater than approximately 200 daltons, wherein: i) units V are terminal units having the formula: EX "ENR- OR E-N + -R- OR IN? -R- ii) units W are base structure units that have the formula: EX" -NR- -N -R- -? NR EEE iii) Y units are branching units having the formula: EX "-NR- or -N + -R- or -N? NR- I: and iv) and the Z units are terminal units having the formula: X" wherein the base structure linking units R are selected from the group consisting of C2-C12 alkylene, C4-C2 alkenylene, C3-C12 hydroxyalkylene, C4-C2 dihydroxyalkylene, C8-C12 dialkylarylene, ( R ^ -OJxR1-, - (R10) xR5 (OR1) x, - (CH2CH (OR2) CH20) z (R ^ O) and R1- (OCH2CH (OR2) CH2) w ~, -C (O) (R4) rC (0) -, -CH2CH (OR2) CH2-, and mixtures thereof, wherein R1 is C2-C alkylene, and mixtures thereof, R2 is hydrogen, - (R- ^ OJxB, and mixtures of the same; R3 is Ci-Cis alkyl, C7-C2 arylalkyl, aryl substituted with C7-C12 alkyl, Cg-C2 aryl and mixtures thereof; R is C1-C12 alkylene, C4-C12 alkenylene, C3-C12 arylalkylene, Cg-Cig arylene and mixtures thereof; R5 is C -C12 alkylene, C3-C2 hydroxyalkylene, C4-C2 dihydroxyalkylene, C8-C12 dialkylarylene, -C (0) -, -C (0) NHR6NHC (0) -, -R ^ OR1 ) -, -C (0) (R4) rC (0) -, CH2CH (0H) CH2-, CH2CH (0H) CH20- (R10) and R10CH2CH (0H) CH2- and mixtures thereof; R6 is C2-C12 alkylene or Cg-C2 arylene; the E units are selected from the group consisting of hydrogen, C3-C22 alkenyl C3-C22 alkenyl / C7-C22 arylalkyl / C2-C22 hydroxyalkyl / "(CH2) pC02M, - (CH2) gS03M, CH ( CH2C02M) C02M, - (CH2) pP03M, - (R ^ -O) ^, -C (0) R3, and mixtures thereof; oxide; B is hydrogen, C? -C alkyl, (CH2) qS03M, - (CH2) pC02M, - (CH2) q (CHSO3M) CH2S03M, - (CH2) q- (CHS02) CH2S03, -. {CH2) pP? 3M, -PO3M and mixtures thereof, M is hydrogen or a cation soluble in water in sufficient quantity to satisfy the charge balance, X is a water soluble anion, m has the value of 4 to about 400, n has the value of 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, and "y" has the value of 0 to 100; it has the value of 0 or 1. An example of the most preferred polyethyleneimines would be a polyethyleneimine having a molecular weight of 1800, which is still modified. more 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 copolymers of acrylic acid: maleic acid 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 may include additional detergent ingredients, and / or any number of additional ingredients may 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, soil suspending agents, soil release agents, germicides, pH adjusting agents, fountains. alkalinity without 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 may generally be selected from the various water-soluble alkali metal and ammonium or ammonium phosphates, phosphonates, 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 CIQ ~ 18 '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, stratified sodium silicates prefer magnesium ions over calcium ions, a feature necessary 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-1,1-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 non-phosphorus inorganic builders are tetraborate decahydrate and silicates having a weight ratio of SiO 2: alkali metal oxide of about 0.5 to about 4.0, preferably about 1.0 to about 2.4. The non-phosphorus water-soluble organic builders useful herein include the various alkali metal, L-ammonium, and substituted ammonium polyacetates, carboxylates, polycarboxylates, and polyhydroxysulfonates. Examples of polyacetate 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, 5 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 0 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 5 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 U.S. 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 a glyoxylic acid ester and a polymerization initiator under polymerization conditions. 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 ether carboxylate builder compositions which comprise a combination of tartrate monosuccinate and tartrate disuccinate described 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 November 1, 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. Foam modifiers 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 detergency builders suitable for use herein are listed in the patent of Baskerville, 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, nonionic surfactants, liquid silicates, polyethylene glycol, polyvinylpyrrolidone, 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, 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). In order 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 Schugi FX-160 mixer, followed by the Lódige KM mixer (KM-600), and then the fluid bed apparatus for additional granulates. [Step 1] 120-160 kg / hr of HLAS (an acid precursor of Cn-Cis alkylbenzenesulfonate, 96% active) is dispersed in a highly turbulent air stream of the Schugi FX-160 mixer together with 220 kg / hr of STPP powder (average particle size of 40 to 75 microns), 160-280 kg / hr of micronised soda ash (average particle size 15 microns), 80-120 kg / hr of micronized sulphate (average particle size of 15 microns). microns) and 200 kg / hr of fine recirculated particles. The surfactant paste is fed at about 50-60 ° C, and the powders are fed at room temperature. Then, 30 kg / hr of HLAS (an acid precursor of Cn-Cig alkylbenzenesulfonate, 94-97% active) is dispersed as a finely atomized liquid in the FX-160 mixer at about 50 to 60 ° C. To the Schugi mixer are added 1 lb. 20-80 kg / hr of soda ash (average particle size of about 10-20 microns). The conditions of the Schugi mixer are as follows: Average residence time: 0.2 - 5 seconds Top speed: 16 to 26 m / s 15 Power condition: 0.15 - 2 kj / kg Mixer speed: 2000 - 3200 rpm [Step 2 ] The agglomerates of the Schugi FX-160 mixer are fed to the KM-600 mixer for additional agglomeration, for rounding and growth of the agglomerates. 30 20 kg / hr of Zeolite can also be added to 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 25 Power condition: 0.15 - 2 kj / kg Mixer speed: 100 - 150 rpm Cover temperature: 30-40 ° C [Step 3] 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 the following: 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 / l, and can optionally be subjected to the optional cooling procedures, configuration and / or spray.

EXAMPLE 2 The following is an example for obtaining agglomerates having high density using the Schugi FX-160 mixer, followed by the Mixer KM Code (KM-600). [Step 1] 120 - 200 kg / hr of HLAS (an active 95% active n-Cis alkylbenzenesulfonate acid precursor) at about 50 ° C, is dispersed in a highly turbulent air stream of the Schugi FX-160 mixer together with 220 kg / hr of STPP powder (average particle size of 40 to 75 microns), 160 - 280 kg / hr of micronised 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. The conditions of the Schugi mixer are as follows: Average residence time: 0.2 - 5 seconds Peak speed: 16 - 26 m / s Power condition: 0.15 - 2 kj / kg Mixer speed: 2000 - 3200 rpm [Step 2] The agglomerates of the mixer FX-160 are fed to the mixer KM-600 for additional agglomeration, for rounding and growth of the agglomerates. 60 kg / hr of micronized soda ash (average particle size 15 microns) are also added to the KM mixer. You can use the shredders for the KM mixer to reduce the amount of oversized agglomerates. The conditions of the KM mixer are as follows: Average residence time: 3-6 minutes Energy condition: 0.15 - 2 kj / kg Mixer speed: 100 - 150 rpm Cover temperature: 30-40 ° C The granules of step 2 The resulting products have a density of approximately 650 g / l and can optionally be subjected to the optional configuration and / or spraying process. 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 (9)

NOVELTY OF THE INVENTION CLAIMS

1. - A non-tower process for producing a granular detergent composition having a density of at least about 600 g / l, comprising the steps of: (a) dispersing a surfactant and coating the surfactant with fine powders having a diameter of 0.1 to 500 microns, moistening the surfactant coated with the fine powders with finely atomized liquid, in a mixer in which the 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 about 0.15 to about 5 kj / kg energy condition, where the agglomerates are formed; and (b) completely mixing the agglomerates in a mixer wherein the conditions of the 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 of energy condition .

2. - A non-tower process for preparing a granular detergent composition having a density of at least about 600 g / l, comprising the steps of: (a) dispersing a surfactant and coating the surfactant with powders fines having a diameter of 0.1 to 500 microns, wetting the surfactant coated with the fine powders with finely atomized liquid, in a mixer in which the conditions 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 first agglomerates are formed; (b) completely mixing the first agglomerates in a mixer where the conditions of the 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 of energy condition , where second agglomerates are formed; and (c) 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) 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 fluidized speed and (vi) from about 12 to about 100 ° C bed temperature.

3. The process 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. the same .

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 polymeric solution is dispersed with said surfactant in step (a).

6. The process according to claims 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, crystalline silicates stratified, phosphates, precipitated silicates, polymers, carbonates, citrates, nitrilotriacetates, powder surfactants and mixtures thereof.

7. The process according to claim 1 or 2, further characterized in that the finely atomized liquid is selected from the group consisting of liquid silicates, anionic surfactants, cationic surfactants, aqueous polymeric solutions, non-aqueous polymer solutions, water and mixtures thereof.

8. - 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).

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