MXPA00000591A - Process for making a low density detergent composition by controlling agglomeration via particle size - Google Patents

Abstract

A process for preparing low density detergent agglomerates is provided. The process involves the step of:(a) agglomerating a detergent surfactant paste or precursor thereof and dry starting detergent material having a median particle size in a range from about 5 microns to about 70 microns in a first high speed mixer to obtain detergent agglomerates having a median particle size of from about 100 microns to about 250 microns;(b) mixing the detergent agglomerates with a binder in a second high speed mixer to obtain built-up agglomerates having a median particle size in a range of from about 140 microns to about 350 microns;and (c) feeding the built-up agglomerates into a fluid bed dryer in which the built-up agglomerates are agglomerated with another binder and dried to form detergent agglomerates having a median particle size in a range of from about 300 microns to about 700 microns and a density in a range about 300 g/l to about 550 g/l.

Description

PROCEDURE TO MAKE A COMPOSITION DETERGENT OF LOW DENSITY CONTROLLING THE AGGLOMERATION THROUGH PARTICLE SIZE FIELD OF THE INVENTION The present invention generally relates to a process for producing a low density detergent composition. More particularly, the invention relates to a process during which the low density detergent agglomerates are produced by supplying a paste of surfactant or liquid acid precursor of anionic surfactant and dry starting detergent material sequentially in two high speed mixers. followed by a fluidized bed dryer. The process produces a free-flowing, low-density detergent composition that can be sold commercially as a conventional non-compact detergent composition or used as a mixture in a low-dose detergent product, "compacta7 BACKGROUND OF THE INVENTION Recently there has been considerable interest in the detergent industry for laundry detergents that are "compact" and therefore therefore, they have low dose volumes. To facilitate the production of so-called low dose detergents, various attempts have been made to produce detergents of high volume density, for example in a density of 600 g / l or more. Low-dose detergents currently have a high demand because they conserve resources and can be sold in small packages that are more convenient for consumers. However, the extent to which modern detergent products need to be "compact" has not been fixed in nature. In fact, several consumers, especially in developed countries, continue to prefer higher dose levels and their respective laundry operations. Accordingly, there is a need in the art to produce modern detergent compositions for flexibility in the ultimate density of the final composition. Generally, there are two primary types of processes by which detergent granules or powders can be prepared. The first type of process involves the spray drying of an aqueous detergent suspension in a spray-drying tower to produce highly porous detergent granules. In the second type of process, the various detergent components are mixed dry after which they are agglomerated with a binder, such as nonionic or anionic surfactants. In both procedures, the most important factors that govern the density of the resulting detergent granules are density, porosity and surface area, shape of the , da ia -_ ^ _ £ > _ "." Various starting materials and their respective chemical composition. These parameters, however, may vary only within a limited scale. In this way, flexibility in substantial bulk density can only be achieved by additional processing steps that lead to a lower density of the detergent granules. There have been several attempts in the art to provide methods that increase the density of the detergent granules or powders. Particular attention has been paid to the densification of spray-dried granules by subsequent treatment in a tower. By For example, an attempt involves a batch process in which spray-dried detergent powders or granules containing sodium tripolyphosphate and sodium sulfate are densified and spheronized in a Marumerizer®. Said apparatus comprises a substantially horizontal, rough, rotatable table placed at the base of a substantially vertical cylinder, of walls smooth. Said process, however, in 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 procedures to increase the density of the detergent granules dried "afterwards in tower" or by spray.

Typically, said processes require a first apparatus that pulverizes or crushes the granules in a second apparatus that increases the density of the pulverized granules by agglomeration. Although these procedures achieve the desired increase in density by For the treatment or densification of granules dried "afterwards in tower" or by spray, they do not provide a procedure that has the flexibility to provide lower density granules using an agglomeration procedure or other procedures that do not They use tower. In addition, all of the aforementioned processes relate mainly to the densification or other process of 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 achieve high levels of surfactants in the resulting detergent composition, a feature that facilitates the production of detergents in a more efficient manner. In this way, it would be desirable to have a process by which detergent compositions can be produced without having the limitations imposed by spray drying techniques. conventional. To this end, the technique also has descriptions of procedures that allow the agglomeration of detergent compositions. For example, attempts have been made to agglomerate the detergent binders by mixing zeolite and / or layered silicates in a mixer to form the free-flowing agglomerates. Although such attempts suggest that their procedures can be used to produce detergent agglomerates, they do not provide a mechanism by which conventional starting detergent materials in the form -t ^ ^ _ ^? m ^^ mmáá ^ ^ surfactants or precursors thereof, liquid and dry materials can be agglomerated effectively in brittle, free-flowing detergent agglomerates having lower densities instead of high densities. Previously, attempts to produce such low density agglomerates involved an unconventional detergent ingredient that was typically expensive, thereby increasing the cost of the detergent product product. An example of the above involves an agglomeration process with inorganic double salts such as Burkeite to produce the desired low density agglomerates. Accordingly, there is still a need in the art to have a process for producing a low density detergent composition directly from the starting detergent ingredients without the need for relatively expensive specialty ingredients. Likewise, there is still a need for a process that is more efficient, flexible and economical to facilitate the large-scale production of low and high dose level detergents.

TECHNICAL BACKGROUND The following references refer to the spray-dried densification granules: Appel et al, U.S. Pat. No. 5,133,924 (Lever); Bortolotti et al, patent of E.U.A. 5,160,657 (Lever); Johnson et al, British Patent No. 1, 517,713 (Unilever); and Curtis, request for rtfiüu __ ^^ á_ÉÉt_f ^ lfl_i ____tti European patent 451, 894. The following references refer to the production of detergents by agglomeration: Beerse et al, patent of E.U.A. No. 5,108,646 (Procter &Gamble); Capeci et al, patent of E.U.A. No. 5,366,652 (Procter &Gamble); Hollingsworth et al, European patent application 351, 937 (Unilever); and Swartiing et al, patent of E.U.A. No. 5,205,958. The following references refer to inorganic double salts: Evans et al, U.S. No. 4,820,441 (Lever); Evans et al, patent of E.U.A. No. 4,818,424 (Lever); Atkinson et al, patent of E.U.A. No. 4,900,466 (Lever); and France et al, patent of E.U.A. No. 5,576,285 (Procter &Gamble); and Dhalewadika et al, PCT WO 96/04359 (Unilever).

BRIEF DESCRIPTION OF THE INVENTION The present invention meets the aforementioned needs in the art by providing a process that produces a low density detergent composition (below about 600 g / l) directly from the starting ingredients and the need for certain relatively expensive specialty ingredients. . The process does not use the conventional spray drying towers currently used and is therefore more efficient, economical and flexible with respect to the variety of detergent compositions that may be produced in the process. In addition, the procedure is more acceptable for environmental concerns since it does not use spray-drying towers that typically emit particulates and volatile organic compounds in the atmosphere. In essence, the process involves the agglomeration of a surfactant paste or precursor thereof and dry detergent ingredients in a high-speed mixer followed by another high-speed mixer to form agglomerates that have been accumulated or bonded by the growth of Controlled particle size, so that the resulting agglomerates are highly porous and have very low density. The accumulation of the low density agglomerates is also agglomerated in said mode and dried in a fluidized bed dryer to produce the agglomerated low density final detergents. As used herein, the term "agglomerate" refers to particles formed by the agglomeration of detergent granules or particles that typically have a smaller average particle size than the agglomerates formed. All the percentages used in The present are expressed as "percent by weight" on an anhydrous basis unless otherwise indicated. According to one aspect of the invention, a method for preparing low density detergent agglomerates is provided. The procedure comprises the steps of: (a) agglomerating an agent paste detergent surfactant or precursor thereof and a dry starting detergent material having an average particle size on a scale of about 5 microns about 70 microns in a first high speed mixer to obtain detergent agglomerates having a size of < _ ^ __ _ ^ _M_ «-. ^ ??? ^^^ lSi, - ^^^^ .___ J ____ ^ -. . __ > - average particle of around 100 microns to around 250 microns; (b) mixing the detergent agglomerates with a first binder in a second high-speed mixer to obtain accumulated agglomerates having an average particle size on a scale of about 140 microns to about 350 microns; and (c) supplying the agglomerates accumulated in a fluidized bed dryer in which the accumulated agglomerates are agglomerated with a second binder and dried to form detergent agglomerates having an average particle size on a scale of about 300 microns to about of 700 microns and a density on a scale of around 300 g / l around 550 g / l. According to another aspect of the invention, another method is provided for preparing low density detergent agglomerates. The method comprises the steps of: (a) agglomerating a first liquid acid precursor and an anionic surfactant and a dry starting detergent material having an average particle size on a scale of about 5 microns to about 50 microns in a first high-speed mixer for obtaining detergent agglomerates having an average particle size of about 100 microns to about 250 microns; (b) mixing the detergent agglomerates with a second liquid acid precursor of an anionic surfactant in a second high speed mixer to obtain accumulated agglomerates having an average particle size on a scale of about 140 microns to about 35 microns; and (c) supplying the accumulated agglomerates in a dryer fluidized bed in which the accumulated agglomerates are agglomerated with a third liquid acid precursor of an anionic surfactant and dried to form detergent agglomerates having an average particle size on a scale of about 300 microns to about 700 microns and a density on a scale of around 300 g / l around 550 g / l. Detergent products made in accordance with any of the methods of the process described herein are also provided. Accordingly, it is an object of the invention to provide a process for producing a low density detergent composition directly from the starting detergent ingredients that do not include relatively expensive specialty ingredients. It is also an object of the invention to provide such a process that is more efficient, flexible and economical to facilitate the large scale production of low and high dose level detergents. These and other 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 relates to a process in which low density agglomerates are produced by controlling the average particle size of the detergent ingredients in each step gUl I ^ __ Í ________ ¡_I_ of the procedure. "Average particle size" refers to the diameter value of particle size above which 50% of the particles have a larger particle size and below which 50% of the particles have a smaller particle size. The process forms free-flowing, low-density detergent agglomerates that can be used as a detergent product or as a mixture with conventional spray-dried detergent granules and / or high-density detergent agglomerates in a final commercial detergent product. It should be understood that the method described herein can be operated continuously or in a batch mode, depending on the particularly desired application. An important advantage of the present process is that it uses equipment that is currently used to make high-density or compact detergent products. However, the process described herein produces low density detergent compositions of said similar equipment by selective adjustment and modification in certain unit operations and parameters as detailed herein. In this way, a large-scale commercial detergent manufacturing equipment can be constructed to produce high or low density detergent compositions, depending on local consumer demand and its inevitable fluctuations between compact and non-compact detergent products.

Procedure In the first step of the process, a detergent surfactant paste or hammer thereof, as described in more detail below, and the starting detergent material having a selected average particle size, is introduced and agglomerated in a high speed mixer. Unlike the above procedures in this area, the starting material can include those relatively inexpensive detergent materials typically used in modern granular detergent products. Such ingredients influence, but are not limited to, binders, fillers, dry surfactants, and flow aids. Preferably, the binder includes aluminosilicates, crystalline layered silicates, phosphates, carbonates and mixtures thereof, which are the essential dry starting detergent ingredient within the scope of the current process. Relatively expensive materials such as Burkeite (Na2SO4 * Na2CO3) and the various silicas are not necessary to achieve the desired low density agglomerates produced by the process. Conversely, it has been found that by minute control, the average particle size of the input dry materials, particle accumulation can be achieved in a form that produces agglomerates having a high degree of porosity "nparticle" or "intragranule" or "intra-agglomerate", and therefore are of low density. The terms "intraparticle" or "intragranule" or "intra-agglomerate" are used similarly herein to refer to porosity or space vacuum within the formed accumulated agglomerates produced at any stage of the process. Accordingly, as in the first step of the process, the average particle size of the dry detergent material is preferably on the scale of about 5 microns about 70 microns, more preferably about 10 microns to about 60 microns , and more preferably from about 10 microns to about 50 microns. It is also preferable to include from 1% to about 40% by weight of recycled or "fine" undersized detergent particles in the first step of the process. The above can be conveniently achieved by screening the detergent particles formed after the fluidized bed dryer at a scale of average particle size from about 10 microns to about 150 microns and the supply of said "fine" particles back into the first high-speed mixer. The high speed mixer can be any of a variety of commercially available mixers, such as a Lodige BC 30 mixer or similar brand mixer. These types of mixers essentially consist of a horizontal, hollow, static cylinder, having a centrally mounted rotating shaft around which join several digging and rod-shaped blades having a tip speed of about 5 m / s to about 30 m / s, more preferably from about 6 m / s to about 26 m / s. On a scale of Lódige CB 30, the shaft rotates at a speed of around 100 rpm at ^ AiÉM | M ^ - | ^ j ^ ^^^^ ^^^^ g ^ j about 2500 rpm, more preferably around 300 rpm at about 1600 rpm. In other mixer scales, the preferred rotation speed is adjusted to maintain the tip speed of the tool equivalent to that of the CB 30 Code. The tip speed is calculated by multiplying the radius from the center of the axis to the tip of the tool by 2pN, where N is the rotation speed. Preferably, the average residence time of the detergent ingredients in the high-speed mixer is on the scale of about 2 seconds to about 45 seconds, and more preferably about 5 seconds to about 15 seconds. The average residence time is conveniently measured by dividing the weight of the mixer in a constant state by inflow (kg / hr). Another suitable mixer is any of the various Flexomix models available from Schugi (The Netherlands), which are vertically placed high speed mixers. This type of mixer is preferably operated at a Froude index of around 3 to about 32. See U.S. Patent 5,149,455 to Jacobs et al (issued September 22, 1992) for a detailed description of said Froude index. known, which is a smaller number that can be optimally selected by those skilled in the art. In a preferred embodiment of the process of the invention, a liquid acid precursor of an anionic surfactant is introduced with the dry starting detergent material including at least one agent ___ §Í __________ Jí_ttU__Í__ neutralizing, such as sodium carbonate. The preferred liquid acid surfactant precursor is the linear alkylbenzenesulfonate surfactant of C-n.-iß ("HLS"), although any acid precursor of an anionic surfactant can be used in the process. A more preferred embodiment involves the delivery of a linear acid precursor of C12-14 linear alkylbenzenesulfonate surfactant. with a C-io-iß linear alkylbenzenesulfonate surfactant ("AES") in the first high speed mixer, preferably in a weight ratio of about 5: 1 about 1: 5, and more preferably, in a scale of around 1: 1 to around 3: 1 (HLAS: AS). The result of said mixing is a "dry neutralization" reaction between the HLA and the sodium carbonate embedded in the dry starting detergent material, which forms agglomerates. It is preferred to add the HLAS before the addition of other surfactants, such as AES surfactants or alkyl sulfate ("AS") to ensure optimal mixing and neutralization of the HLAS in the first high-speed mixer. Preferably, after agglomeration in the first mixer, detergent agglomerates having an average particle size of about 100 microns are formed at about 250 microns, more preferably from about 80 microns to about 140 microns. microns, and more preferably from about 90 microns to about 120 microns. The particle size growth rate can be controlled in a variety of ways, including but not limited to HBMHf Ba ^^^ gasi | jU ^^^ || ga_ ^ g ^ | variation of residence time, temperature and mixing tool speed of the mixer, and control of the amount of binder liquid supplied in the mixer. In this regard, the particular controlled parameter is not critical, unless only the average particle size is within the scales previously described. In this way, the smallest particle size starting detergent material gradually accumulates in a controlled manner, so that the agglomerates have a large intragranule porosity scale, thus resulting in a low density detergent composition. As stated differently, the smaller sized starting detergent material is "glued" or "lightly" glued to form the porous accumulated agglomerates, which are controlled to maintain or increase the porosity by solidifying the particle bonds without consolidation or collapse of agglomerates. In the second step of the process, the detergent agglomerates formed in the first step are introduced into a second high-speed mixer and agglomerated with the atomized liquid binder. The second high-speed mixer can be the same piece of equipment as used in the first step or a different type of high-speed mixer. For example, a Lódige CB mixer can be used in the first step while the Schugi mixer is used in the second step. In this second step of the process, the agglomerates having an average particle size are previously observed as mixed and In addition, in a controlled manner, the detergent agglomerates emerging from the second high-speed mixer have an average particle size of about 140 microns to about 350 microns, more preferably about from 160 microns to 5 about 250 microns, and more preferably from about 180 microns to about 220 microns. As in the first step of the process, the agglomerates are agglomerated in a very controlled manner, so that they have an average particle size within the aforementioned scales. Again, the intragranule porosity of the particles is increased by the "adhesion" of smaller sized particles with a high degree of porosity between the particles (e.g., intraparticle porosity). In this step, the above is achieved by the operation of the high-speed mixer with sufficient binder atomization and spray coating to produce only agglomerates in the aforementioned average particle size scales. In this regard, a suitable binder is added to facilitate the formation of the desired agglomerates in this step. Typical binders include liquid sodium silicate, a liquid acid precursor of an anionic surfactant such as HLAS, surfactant non-ionic, polyethylene glycol or mixture thereof. In the next step of the process, the accumulated agglomerates are introduced into a fluidized bed dryer in which the agglomerates are dried and agglomerated and an average particle size of ___, _ - __i - ^ - - ** - * - "• * - *" * - about 300 microns to about 700 microns, and more preferably from about 250 microns to about 450 microns. The density of the formed agglomerates is around 300 g / l to around 550 g / l, more preferably from about 350 g / l to about 500 g / l, and even more preferably from about 400 g / l to about 480 g / l. All of these densities are generally below the typical detergent compositions formed of dense agglomerates or more typical spray-dried granules. Preferably, in such process modalities involving aqueous binders, the inlet air temperature of the fluidized bed drying is maintained on a scale of about 100 ° C to about 200 ° C to improve the formation of the agglomerates. desired. Although not intended to be limited by theory, it is believed that such a relatively high temperature ensures rapid evaporation of moisture to solidify the wet bonds of the agglomerates. accumulated to maintain a high degree of porosity of said granule. As with the first and second steps of the process, the agglomerates are formed from sized particles of smaller to larger sizes, having a high degree of intragranular porosity. The intragranule porosity degree of preference is from about 20% to about 40%, and more preferably from about 25% to about 35%. The porosity of the intragranule can be conveniently measured by the standard mercury porosimetry test. , ^ ^. .. ^ _ J X, ^^, ^ ...,. ^^^ »^ ^? 6b ^. ^, Optionally, a binder, as described above, can be added during this step in more than one place, so that at each end of the fluidized bed dryer the formation is driven of the desired agglomerates. The pure result of this method of the procedure involves the addition of a binder in the second high-speed mixer and at each end (for example, the inlet port and the outlet port) of the fluidized bed, thus totaling three points of addition of binder in the process that provides higher low density agglomerates. Particularly preferred binders in this regard are liquid sodium silicate and HLAS. Other optional steps contemplated by the present method include screening the oversized detergent agglomerates in a screening apparatus that can take a variety of forms, including but not limited to conventional screens selected for the desired particle size of the finished detergent product. Other optional steps include the conditioning of the detergent agglomerates by subjecting the agglomerates to further drying and / or cooling by the apparatus described above. Other optional steps of the instant procedure allow you to finish the resulting detergent agglomerates by a variety of procedures that include spraying and / or mixing other ingredients j ^^ i ^ ^. & a »¿g conventional detergents. For example, the determination step comprises the spray perfumes, brighteners and enzymes in the finished agglomerates to provide a more complete detergent composition. Such techniques and ingredients are well known in the art. 5 Detergent surfactant paste or surfactant acid precursor As mentioned above, a liquid acid precursor of surfactant is used in the first step of the process as well as in the second and third essential steps of the process as a binder. Said liquid acid precursor will typically have a viscosity when measured at 30 ° C of about 500 cps at about 5000 cps. The liquid acid is a precursor of the anionic surfactants described in more detail below. A paste of surfactant The detergent can also be used in the process and is preferably in the form of an aqueous viscous paste, although other forms are also contemplated by the invention. The so-called viscous surfactant paste has a viscosity of about 5000 cps at about 100,000 cps, more preferably about 10,000 cps a about 80,000 cps, and contains at least about 10% water, more preferably at least about 20% water. The viscosity is measured at 70 ° C and at shear rates of about 10 to 100 sec "7 In addition, the surfactant paste, if used, preferably "--- -stt '' -» - - "^ - - -. ? ********** comprises a detersive surfactant in the amounts specified above in the remainder of water and other conventional detergent ingredients. The surfactant itself is selected, in the viscous surfactant paste, preferably from the anionic, nonionic, zwitterionic, ampolytic and cationic classes., and compatible mixtures thereof. The surfactants useful herein are described in US Patent 3,664,961, Norris, issued May 23, 1972 and in US Patent 3,919,678, Laughiin et al., Issued December 30, 1975, which they are incorporated herein by reference. Useful cationic surfactants also include those described in US Pat. 4.22.905, Cockrell, issued September 16, 1980 and the patent E.U.A. 4,239,659, Murphy, issued December 16, 1980, which are incorporated herein by reference. Of the surfactants, anionics and nonionics are preferred and anionics are preferred above all. Some non-limiting examples of the preferred anionic surfactants useful in the surfactant paste, or from which the liquid acid precursor described herein derives, include alkylbenzenesulfate ("LAS") of Cu-Cie, alkyl sulfates ("AS") ) of branched and random chain C10 -C20, the secondary alkyl sulphates (2.3) of C-? 0 Cie of the formula CH3 (CH2) (CHOSO3-M +) CH3y (CH3) and (CHOSO3 -M +) CH2CH3 where xy ( and + 1) are integers of at least about 7, preferably at least about 9, and M is a cationThe water solubilizer 510, especially sodium, sulfates and saturates such as oleyl sulfate, and the alkylalkoxy sulfates of C-C-is ("AEXS", especially the ethoxysulfates of EO 1-7). Optionally, other exemplary surface active agents useful in the paste of the invention include the C 1 io C-iß alkylalkoxycarboxylates (especially the EO 1-5 ethoxycarboxylates), the glycerol ethers of C 0 -C 0 β, the alkyl polyglycosides of C-io-Ciß and their corresponding sulfated polyglycosides, and ethers of alpha-sulfonated fatty acids of C - ^. C-is. Also included in all compositions are conventional nonionic and amphoteric surfactants such as C12-C18 alkylethoxylates ("AE") including the so-called narrow-chain alkyl ethoxylates and C2-C alkylphenol ethoxylates. s (especially mixed ethoxylates and ethoxy / propoxy), C? 2-C-? 8 betaines and sulfobetaines ("sultaines"), C10-C18 amine oxides and the like. The amines of fatty acids can also be used N-C10-C-iß N-alkyl polyhydroxy Typical examples include N-methylglucamines of C-12-C18 See WO 9206154. Other surfactants derived from sugar include the N-alkoxy polyhydric fatty acid amides, such as N- (3-methoxypropyl) glucamide of C-IO-C-IS. The N-propyl can be used to N-hexylglucamines of C 10 -C 18 , due to its low foaming. Conventional C? O-C2o soaps can also be used - If high foaming is desired, branched-chain C10-C16 soaps can be used. Mixtures of anionic and non-surface active agents They are especially useful. Other conventional useful surfactants are listed in standard texts.

Dry starting detergent material The dry starting detergent material of the present process preferably comprises a builder and other chemical detergent ingredients, such as sodium carbonate, especially when a liquid acid precursor of a surfactant is used, which is needed as a neutralizing agent in the first step of the process. In this way, the preferable dry starting detergent material includes sodium carbonate and a phosphate or an aluminosilicate builder which is referred to as an aluminosilicate ion exchange material. A preferred builder is selected from the group consisting of aluminosilicate, crystalline layered silicates, phosphates, carbonates and mixtures thereof. Preferred phosphate builders include sodium tripolyphosphate, tetrasodium pyrophosphate, and mixtures thereof. Some additional specific examples in the inorganic phosphate builder are tripolyphosphate, pyrophosphate, polymeric metaphosphate having a degree of polymerization of about 6 to 21, and orthophosphate, sodium and potassium. Examples of polyphosphate builders are the sodium and potassium salts of ethylene phosphonic acid, the sodium and potassium salts of ethane-1-hydroxy-1,1-diphosphonic acid and the sodium and potassium salts of ethane-1 , 1, 2-triphosphonic. HE H! MM? £ igigH? ||| & bite other phosphorous builders 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, which are incorporated herein by reference. The aluminosilicate ion exchange materials that are used herein as builders preferably have both high calcium ion exchange capacity and high exchange rate. Without intending to be bound by theory, it is believed that such a high calcium ion exchange rate and capacity are a function of several interrelated factors that derive from the method by which the aluminosilicate ion exchange material is produced. In that regard, the aluminosilicate ion exchange materials that are used herein are produced, preferably according to Corkill et al, U.S. No. 4,605,509, (Procter &; Gamble), whose invention is incorporated herein by reference. Preferably, the aluminosilicate ion exchange material is in the "sodium" form, since the hydrogen potassium forms of the present aluminosilicate do not exhibit the high exchange rate and capacity as provided by the sodium form. Additionally, the aluminosilicate ion exchange material is preferably in is overdried, so that the production of agglomerates of brittle detergents as described herein is facilitated. The aluminosilicate ion exchange materials that are used herein preferably have particle size diameters that optimize their _H_IÍÉ ____ IB___ Í ___ Í effectiveness as detergency 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 additional analytical techniques, such as microscopic determination and electron microscopy. of exploration (SME). The preferred diameter of aluminosilicate particle size is from about 0.1 microns to about 10 microns, more preferably from about 0.5 microns to about 9 microns. More preferably, the particle size diameter of the particle size is from about 1 millimeter to about 8 microns. Preferably, the aluminosilicate ion exchange material has the formula. Naz [(AIO2) z. (SiO2) and] xH2O where z and "y" are integers of at least 6, the molar ratio of zay is from about 1 to about 5 and x is from about 10 to about 264. More preferably, the Aluminosilicate has the formula. Na? 2 [(AI02)? 2. (SiO2)? 2] xH2O wherein x is from about 20 to about 30, preferably from about 27. Said preferred aluminosilicates are commercially preferred, for example, with the Zeolite A, Zeolite B and Zeolite X assignments. Alternatively , aluminosilicate ion exchange materials can be made which are naturally present for derivatives synthetically for use herein, as described in Krummel et al. l? itin -? i? rffi? rrr - r - al, US Patent No. 3,985,669, the disclosure of which is hereby incorporated by reference.The aluminosilicates used herein are further characterized by their ion exchange capacity which is at least of about 200 mg of CaCO3 hardness equivalent / grams, calculated on anhydrous basis, and which is preferably in the range of about 600 to 352 mg of CaCO3 hardness equivalent / grams. aluminosilicate are still further characterized in that their calcium ion exchange rate is at least about 2oCa ++ / 3.785 liters / minute / -gmo / 3.685 liters and more preferably in a range of about 2gm Ca ++ / 3.785 liters / minute / -gram / 3,685 liters normally 6 degree of Ca ++ / 3,785 liters / minute / -gram / 3,685 liters.

Deputy detergent ingredients The starting dry 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 of the subsequent steps of the present procedure. These adjunct ingredients include other detergency builders, bleaches, bleach activators, foam or foam thicknesses, anti-rust and anti-corrosion agents, soil suspending agents, soil release agents, germicides, ^ a ^.-.- yja- pH adjusting agents, alkalinity sources, non-builders, chelating agents, smectite rings, enzymes, enzyme and enzyme stagnant agents. See in the patent of E.U.A. 3,936,537, issued February 3, 1976 to Baskerville, Jr, eta I, incorporated herein by reference. Other detergency builders may be pre-selected among various borates, polyhydrosulfonates, polyacetates, carboxylates, citrates, tartra, mono- and di-succinates, and mixtures thereof. Alkali metal salts, especially sodium salts, are preferred. In addition to the amorphous sodium silicates, the crystalline layered sodium silicates exhibit a clearly increased calcium and magnesium ion exchange capacity. further, the stratified sodium silicates prefer the magnesium ions to the calcium ions, a characteristic necessary to ensure that substantially all of the "hardness" of the wash water is removed. Said crystalline layered sodium silicates, however, are generally more expensive than amorphous silicates, as well as other detergency builders. Accordingly, in order to provide an economically viable laundry detergent, the proportion of crystalline layered sodium silicates must be judiciously determined. The crystalline layered sodium silicates suitable for use herein preferably have the formula NaMSixO2x +? and H 2 O 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 NaMS¡205.yH2O 5 wherein M is sodium or hydrogen and "and" is from about 0 to about 20. These and other crystalline layered sodium silicates are described in Corkill et al, US Patent No. 4,605,509, previously incorporated herein by reference. reference. Some examples of non-phosphorous inorganic builders are tetraborate decahydrate and silicates having a weight ratio of S02 to alkali metal acid of about 0.5 to about 4.0, preferably from about 1.0 to about 2.4. . The non-phosphorous, water-soluble organic builders, useful herein, include the various polyacetates, carboxylates, polycarboxylates and polyhydroxysulfonates of alkali metals, ammonium and substituted ammonium. Some examples of polyacetate and polycarboxylate detergent builders are the sodium, potassium, lithium, ammonium, and substituted ammonium salts of ethylenediaminetetraacetic acid, notrilotriacetic acid, oxydisuccinic acid, mellitic acid, benzenepolycarboxylic acid, and citric acid. Polymeric polycarboxylate detergent builders are discussed in the U.S.A. 3,308,067, Diehl, issued March 7, 1967, the disclosure of which is incorporated herein by reference, three materials include the water soluble salts of homo- and copolymers of aliphatic carboxylic acids such as maleic acid, itaconic acid, mesaconic acid, fumaric acid, aconitic acid, citraconic acid and methylenemalonic acid. Some of these materials are useful as the water-soluble anionic polymer, as described hereinafter, but only if they are in an intimate mixture with the anionic surfactant other than soap. Other polycarboxylates suitable for use herein are the carboxylates described in U.S. Patent 4,144,226, issued March 13, 1979 to Crutchfield et al, and the U.S. patent. 4,246,495, issued March 27, 1979 to Crutchfield et al, which are incorporated herein by reference. Such polyacetalcarboxylates can be prepared by coupling an ester of glyoxylic acid and a polymerization initiator under polymerization conditions. The resulting polyacetal carboxylate ester is then attached to the 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 comprising a combination of tartrate monosuccinate and tartrate disuccinate described in the U.S.A. 4,663,071 ,, Bush et al., Issued May 5, 1987, the description of which is incorporated herein by reference.

Bleaches and activators are described in the U.S.A. 4,412,934, Chung et al., Issued November 1, 1983, and the patent of E.U.A. 4,483,781, Hartman, issued November 20, 1984, which are incorporated herein by reference. Chelating agents are also described in the U.S.A. 4,663,071, Bush et al., From column 17, line 54 to column 18, line 68, incorporated herein by reference. Foam modifiers are also optional ingredients and are described in US Patents. 3,933,672, issued January 20, 1976 to Bartoletta et al., And 4,136,045, issued January 23, 1979 to Gault et al., Incorporated herein by reference. Smectite clays suitable for use herein are described in the US patent. 4,762,645, Tucker et al, issued August 9, 1988, column 6 line 3 to column 7, line 24, incorporated herein by reference. Additional builders suitable for use herein are listed in U.S. Patent No. 4,663,071, Bush et al, issued May 5, 1987, which are incorporated herein by reference. In order to make the present invention more easily understood, reference is made to the following example, which is intended to be illustrative only and is not intended to be limiting in scope. -, ^ fc_U__ .., .OMM.

EXAMPLE This example illustrates the invention of the process in which a low density agglomerated detergent composition is prepared. A Lódige CB 30 high speed mixer is charged with a powder mixture, namely, sodium carbonate (average particle size 15 microns), sodium tripolyphosphate ("STPP") with an average particle size of 25. mieras A liquid acid precursor of sodium alkylbenzenesulfonate surfactant (C? 2H25-C6H4-SO3H or "HLAS" as indicated below) and a surfactant sulfate-ethoxylated paste of active aqueous C10-18 70% is also introduced. (EO = 3, "AES") to a Lódige CB 30 mixer, where the HLAS is first added. The mixer is operated at 1600 rpm and the sodium carbonate of STPP, HLAS and AES is transformed into agglomerates having an average particle size of approximately 110 microns after an average residence time in the Lódige CB 30 mixer of approximately 5 seconds. The agglomerates are then supplied to a Schugi high speed mixer (Model # FX160) which is operated at 2800 rpms with average residence time of approximately 2 seconds. A binder of HLAS to the Schugi mixer (Model # FX160) during this step which results in forming shaped agglomerates having an average particle size and approximately 180 microns. Subsequently, the formed agglomerates are passed through the bed dryer ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^ ^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^^ of spray are placed in the first and fourth zones of the fluidized bed dryer. The fluidized bed is operated at an air temperature of about 125 ° C. At each end of the fluid bed dryer, liquid sodium silicate binder is fed to the fluid bed dryer resulting in agglomerates of finished detergents having a density of about 485 g / l and an average particle size of about 360 mieras Unexpectedly, the finished agglomerates have excellent physical properties because they are free-flowing, as they exhibit their higher cake strengths. It is given below that in table I the composition of the agglomerates.

TABLE I (% by weight) 15 Component I LAS (Na) 15.8 AES (EO = 3) 4.7 Sodium carbonate 48.0 STPP 22.7 Sodium silicate 5.5 Water 3.3 100.0 produced by this procedure. By opening the invention described in detail, it will be apparent to those skilled in the art that several changes can be made without the effort of The scope of the invention can not be considered and the invention is not to be limited to what is described in the specification.

Claims (10)

NOVELTY OF THE INVENTION CLAIMS

1. A process for preparing a low density detergent composition, characterized by the steps of: (a) agglomerating a detergent surfactant paste or precursor thereof and drying the starting detergent material having an average particle size on a scale of 5 microns to 70 microns in a first high speed mixer to obtain agglomerates ío having an average particle size of 100 microns to 250 microns; (B) mixing said detergent agglomerates with a first binder into a high speed mixer to obtain built-up agglomerates having an average particle size on a scale of 140 microns to 350 microns; and (c) supplying said agglomerates 15 accumulated and a binder in a fluidized bed dryer in which the accumulated agglomerates are agglomerated with a second binder and dried to form detergent agglomerates having an average particle size on a scale of 300 microns to 700 microns and a density in a scale of 300 g / l to 550 g / l.

2. The process according to claim 1, further characterized in that said first binder is sodium silicate. ^^^^^ ¿^^^^^^^^^^^^^ to ^^^^^^^^^^^^^ FES K ^

3. The process according to claim 1, further characterized because the first binder and said second binder are a liquid acid precursor of an anionic surfactant.

4. The method according to claim 1, 5 further characterized in that in said step (c), said second binder is added at each end or to said fluidized bed dryer.

5. The process according to claim 1, further characterized in that the intragranule porosity of said detergent agglomerates is from 20% to 40%.

6. The process according to claim 1, further characterized in that said first binder and said second binder are sodium silicate.

7. The process according to claim 1, further characterized in that said step (a) includes the agglomeration of a liquid acid precursor of linear alkylbenzenesulfonate surfactant of C? P8 and an ethoxylated alkyl sulfate surfactant of C- io-iß-

8. The method according to claim 1, further characterized in that said step (c) includes maintaining the temperature of said fluidized bed dryer to be at a scale of 100 ° C to 200 ° C. .

9. The process according to claim 1, further characterized in that said dry starting material comprises a The agglutinant selected from the group consisting of aluminosilicate, crystalline layered silicates, phosphates, carbonates and mixtures thereof.

10. A detergent composition made according to the method according to claim 1. -__ to afc, u * -_. > . ^^ * ^ * - - = ~ ------ - - * - »-.-, - * •