MXPA97002099A - Procedure to make a high density detergent composition that includes recirculation currents select - Google Patents

Abstract

A method for continuously preparing a high density detergent composition is provided, the method comprising the steps of: (a) continuously charging a detergent surfactant paste and dry starting detergent material into a high speed mixer / densifier to obtain the agglomerates (b) mixing the agglomerates in a moderate speed mixer / densifier to densify the agglomerates in a conditioning apparatus to improve the flow properties of the agglomerates and to separate the agglomerates in a first agglomeration mix and a second agglomeration mix (d) recirculating the first agglomeration mixture in the high speed mixer / densifier for further agglomeration; (e) mixing the adjunct detergent ingredients in the second agglomeration mixture to thereby form the detergent density composition at

Description

PROCEDURE TO MAKE A HIGH DENSITY DETERGENT COMPOSITION THAT INCLUDES SELECTED RECIRCULATION CURRENTS FIELD OF THE INVENTION 5 The present invention generally relates to a process for producing a high density laundry detergent composition. More particularly, the invention is directed to a continuous process which lasts Lü agglomerated high-density detergents are produced by feeding a paste of surfactant and drying the starting detergent material in two mixer / densx fieadores placed in series form and then in a drying, cooling and sieving apparatus. The procedure optimally includes recirculation current confi urations selected to thereby produce a high density detergent composition with improved flow and particle size properties. Said improved properties improve the consumer acceptance of the detergent composition produced by the process 0 instan-te.

BACKGROUND OF THE INVENTION Recently, there has been considerable interest in the of the laundry detergent for laundry detergents are "compact" and therefore, have volumes of laundry.

To facilitate the production of these so-called low-dose detergents, many attempts have been made to produce detergents of high overall density, for example, with a density of 500 g / 1 or more. Low dosing detergents are currently in high demand as they conserve sources and can be sold in small packages that are convenient for consumers. Generally, there are two primary types of procedures where detergent particles or 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 particles. In the second type of process, the different detergent components are dry blended after they are agglomerated with a binder such as an ammonium or nonionic surfactant. In both procedures, the most important factors that govern the density of the resulting detergent material are the density, porosity, particle size and surface area of the different starting materials and their respective chemical composition. These parameters, however, can only be varied within a limited scale. In this way, a substantial increase in overall density can be achieved only by means of additional procedural steps that lead to the densification of the detergent granules. Many attempts have been made in the art to provide processes that increase the density of granules or powders of detergents. Particular adaptation has been the densification of spray-dried granules by post-tower spray-drying treatment. For example, an attempt involves an intermittent procedure in which spray-dried detergent powders or granules containing tp sodium polyphosphate and sodium sulfate are densified and spheronized in a MarumenzerCR). This apparatus comprises a substantially horizontal, hardened, rotating table placed inside and at the base of a substantially vertical cylinder with smooth walls. This procedure, however, is essentially an intermittent process and is therefore less suitable for large-scale production of detergent powders. More recently, other attempts have been made to provide a continuous process for increasing the density of spray-dried detergent granules or "post-tower" spray-drying. Typically, said processes require a first apparatus that pulverizes or grinds the granules and a second apparatus that increases the density of the pulverized granules or agglomeration, these processes achieve the desired increase in density only by treating or densifying granules spray dried or "post". "Spray drying tower. However, all of the aforementioned processes are directed primarily to densify or otherwise process "spray-dried" granules.

Currently, the relative amounts and types of materials subject to spray drying procedures 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 low-dose detergents. In this way, it would be desirable to have a method by which the detergent compositions can be produced are to have the limitations imposed by conventional spray drying techniques. In that extreme, the technique is also replete with descriptions of procedures comprising agglomerating the detergent compositions. For example, attempts have been made to agglomerate the detergency builders by mixing zeolLta and / or layered silicates in a mixer to form free flowing agglomerates. While such attempts suggest that their process can be used for the production of detergent agglomerates, they do not provide a mechanism by which the starting detergent materials in the form of pastes, liquids and dry materials can effectively agglomerate in free flowing detergent agglomerates that have a high density of at least 650 g / 1. In addition, said agglomeration processes have produced detergent agglomerates that contain a wide range of particle sizes, for example "excesses" and "fines" are typically produced. Particles of agglomerates of "excess" or larger than desired have a tendency to decrease the total solubility of the detergent composition in the wash solution leading to poor cleaning and the presence of "clumps" which ultimately result in dissatisfaction. of the consumer. "Thin" or smaller particles of agglomerates have a tendency to "gel" in the wash solution and also give the detergent product an undesired "powdery" feel. In addition, past attempts to recirculate such "excesses" or "fines" have resulted in the exponential growth of additional unwanted agglomerates of larger size or smaller size since the "excesses" typically provide a nucleation site or seed for the agglomeration of even larger particles, while the recirculation of the "fines" inhibits the agglomeration that leads to the production of more "excesses" in the process. Accordingly, a need remains in the art for a process that produces a high density detergent composition having improved flow and particle size properties. Also, a need remains for a process as such that is more efficient and economical to facilitate the large-scale production of low-dose or compact detergents.

ANTECEDENT TECHNIQUE The following references are directed to densify spray-dried granules: Appel et al., US patent. . No. 5,133,924 (Lever); ortolotti et al., patent of E.U.A. 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 intended to produce detergents by agglomeration: Beerse et al., U.S. Pat. No. 5,108,646 (Procter to Gamble); Hollmgsworth et al., European Patent Application 351,937 (Unilever); and S atling et al., U.S. Patent. No. 5,205,958.

BRIEF DESCRIPTION OF THE INVENTION The present invention meets the aforementioned needs in the art by providing a process that continuously produces a high density detergent composition from starting detergent ingredients. Accordingly, the process achieves the desired high density detergent composition without unnecessary process parameters, such as the use of relatively high spray drying techniques and operating temperatures, which increase manufacturing costs. The process of the invention described herein also provides a detergent composition containing agglomerates having improved particle size and flow properties (i.e., more uniform) that finally result in a low or compact dose detergent product that is more acceptable to consumers. As used herein, the term "agglomerates" refers to particles formed by agglomerating starting detergent ingredients (liquid and / or particles) which typically have a smaller average particle size than the agglomerates formed. All percentages, and proportions used herein are expressed as percentages by weight (anhydrous base) unless otherwise indicated. All documents are incorporated herein by reference. All the viscosities referred to herein are measured at 70 ° C (+ _5 ° C) and at shear rates of about 10 to 100 sec-1. In accordance with an aspect of the invention, a method for continuously preparing a high density detergent composition is provided. The method comprises the steps of: (a) continuously charging a detergent paste of surfactant and dry batch detergent material into a high speed mixer / densifier to obtain the agglomerates; (b) mixing the agglomerates in a moderate speed mixer / hardener to densify, form and agglomerate the agglomerates so that the finished agglomerates have an average particle size of from about 300 microns to about 900 microns; (c) feeding the agglomerates in a conditioning apparatus to improve the flow properties of the agglomerates and to separate the agglomerates in a first agglomeration mixture and a second agglomeration mixture, wherein the first agglomeration mixture has substantially a size of particle of less than about 150 microns and The second agglomeration mixture has a particle size of at least about 150 microns; (d) recirculating the first agglomeration mixture in the high speed mixer / densifier for additional agglomeration; (e) mixing the adjunct detergent ingredients in the second agglomeration mixture to thereby form the high density detergent composition. In accordance with another aspect of the invention, another method for continuously preparing the high density detergent composition is provided. . This process comprises the steps of: (a) continuously charging a detergent paste of surfactant and dry starting detergent material into a high-speed mixer / densifier to obtain the agglomerates; (b) mixing the agglomerates in a moderate speed mixer / densifier to densify, form and agglomerate the agglomerates so that the finished agglomerates have an average particle size of about 300 microns to about 900 microns; (c) sieving the agglomerates to thereby form a first agglomeration mixture having substantially a particle size of at least about 6 mm and a second agglomeration mixture having substantially a particle size of less than about 6 nm; (d) feeding the first agglomeration mixture in a milling unit and the second agglomeration mixture in a conditioning apparatus to improve the flow properties of the second agglomeration mixture and to separate the second agglomeration mixture in a third mixing of agglomeration and a fourth agglomeration mixture, wherein the third agglomeration mixture has a particle size of less than about 150 microns and the fourth agglomeration mixture has substantially a particle size of at least about 150 microns. mieras; (e) recirculating the third agglomeration mixture in the high speed mixer- / densifier for further agglomeration; (f) separating the fourth agglomeration mixture into a fifth agglomeration mixture and a sixth agglomeration mixture, wherein the fifth agglomeration mixture has substically no particle size of at least about 900 microns and the sixth agglomeration mixture < It usually has an average particle size of about 50 microns to about 1400 microns; (g) including the fifth agglomeration mixture on the grinding apparatus for grinding with the first agglomeration mixture to form a base agglomeration mixture which is recirculated in the conditioning apparatus; and (h) mixing the adjunct detergent ingredients in the sixth blending mixture to thereby form the high density composition. Another aspect of the invention is directed to a high density detergent composition made in accordance with any of the instant process modalities. Accordingly, an object of the invention is to provide a process that produces a high density detergent composition containing agglomerates having improved flow properties and particle size. It is also an object of the invention to provide a method such that it is more efficient and economical to facilitate the large-scale production of low-dose or compact detergents. These and other objects, features and advantages appended to the present invention will be apparent to those skilled in the art from a reading of the following detailed description of the preferred embodiment and the appended claims.

BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 is a flow diagram of a process according to an embodiment of the invention wherein the smaller detergent agglomerates are recirculated in the high speed mixer / densifier from the conditioning apparatus; and Figure 2 is a flow chart of a method according to another embodiment of the invention similar to Figure 1 wherein an additional recirculation operation is included for purposes of improving the properties of the resulting detergent product.

DETAILED DESCRIPTION OF THE PREFERRED MODALITY Reference is made to Figures 1 and 2 for purposes of illustrating various embodiments of the method of the invention described herein. Figure 1 illustrates a procedure 10 while Figure 2 describes a procedure LO 'which is a modified version of the LO procedure.

PROCESS Initially, the method shown in FIG. 1 comprises continuously charging a detergent surfactant paste 12 and dry starting detergent material 14 into a high speed injector / densifier 16 to obtain agglomerates 18. The different ingredients that can be selected for the surfactant paste 12 and the dry starting detergent material are more fully described hereinbelow. However, it is preferable that the ratio of the surfactant paste to the dry detergent material be from about 1:10 to about 10: 1 and more preferably from about 1: 4 to about 4: 1. The agglomerates L8 are then sent or fed in a moderate speed mixer / densifier to further densify and agglomerate the agglomerates 18 so that they have the preferred average particle size scale of about 300 microns to approximately 900 micras It should be understood that the dry starting detergent material 14 and the surfactant paste 12 begin to accumulate in agglomerates in the mixer / densifier of LO high speed 16, in this way resulting in agglomerates 18. The agglomerates 18 are then further accumulated in the moderate speed mixer / densifier 20 resulting in densified or accumulated agglomerates 22 that are ready for further processing to increase their L5 flow properties. Typical apparatuses used in the process 10 for the high speed mixer / densifier 16 include but are not limited to a Lodige Recycler CB-30 and while a moderate speed ezclador / densificador 20 can be a "Ploughshare" of Lodige Recycler KM-600. Other devices that can be used include double-propelled mixers, commercial mixers sold with Eipch, Schugí, O'Brien, and Drais mixers, and combinations of these and other mixers. The residence times of the agglomerates / ? 5 ingredients in such mixers / densifiers will vary depending on the particular mixer / densifier and operating parameters. However, the preferred residence time in the nezclador / densifi er of the speed at a 16 is around: from 2 seconds to approximately 45 seconds, preferably around 5 to 30 seconds, while the residence time in the The moderate rate / densifier is about 0.5 minutes to about 15 minutes, preferably about 10 minutes. The moderate speed mixer / ensiler 20 preferably imparts a required amount of energy to the agglomerates 18 for further accumulation or agglomeration. More particularly, the moderate speed mixer / densifier 20 imparts about 5 x 10% erg / L to about 2 x 1012 erg / kg at a rate of about 3 x 108 erg / kg-sec to about 3 x 109 erg / g-sec to form the agglomerates 22. The energy input and the speed of entry can be determined by calculations from powder readings par-to the mixer / moderate speed densitator 20 with and without agglomerates, residence time of the agglomerates, and the mass of the agglomerates in the moderate speed mixer / densitator 20. Such calculations are clearly within the reach of the person skilled in the art. Optionally, a reversing agent can be added just before, in or after the mixer / ensiler 20 to control or inhibit the degree of agglomeration. This optional step provides a means by the desired agglomeration particle size can be achieved. Preferably, the coating agent is selected from the group consisting of alu nosilicates, carbonates, silicates and mixtures thereof. Another optional step comprises spraying a binder material in the high speed mixer / densitator 16 to thereby facilitate the accumulation agglomeration. Preferably, the binder is selected from the group consisting of water, ammonium surfactants, nonionic surfactants, polyethylene glycol, polyvinyl pyrrolidone, polyacrylates, citric acid and mixtures thereof. Another step in the process 10 comprises feeding the further densified agglomerates 22 into a conditioning apparatus 24 which preferably includes one or more feeding apparatus and a cooling apparatus (not shown individually). The conditioning apparatus 24 in any form (fluid bed dryer, fluid bed cooler, air conveyor, etc.) is included to improve the flow properties of the agglomerates 22 and to separate them into a first agglomeration mixture 26 and a second agglomeration mixture 28. Preferably, the agglomeration mixture 26 has substantially a particle size of less than about 150 microns and the agglomeration mixture 28 has substantially a particle size of at least about 150 microns. Of course, it should be understood by those skilled in the art that said separation procedures are not always perfect and may exict a small portion of agglomeration particles in the agglomeration mixture 26 or 28 which is outside the recited size scale. The final goal of the process 10, however, is to divide a substantial portion of the "fines" or agglomerates of smaller size 26 from the agglomerates 28 of more desired size which are then sent to one or more completion steps 30. The mixture of agglomeration 26 is recirculated in the high speed mixer / densitator 16 for further agglomeration so that the agglomerates in the mixture 26 are finally accumulated to the desired agglomeration particle size. Preferably, the termination steps 30 will include mixing the adjunct detergent ingredients in the agglomeration mixture 2B to thereby form a fully formulated high density detergent composition 32 that is ready for commercialization. In a preterm embodiment, the detergent composition 32 has a density of at least 650 g / 1. Optionally, the termination steps 30 include mixing the conventional spray-dried detergent particles in the agglomeration mixture 28 together with the detergent ingredients attached to form the detergent composition 32. In this case, the detergent composition 32 preferably comprises about 10. % to about 40% by weight of the agglomeration mixture 28 and the rest of the spray-dried detergent particles and the attached ingredients. Reference is now made to Figure 2 which describes the process 10 'for making a high density detergent composition according to the invention. Process 10 ', similar to procedure 10, comprises the steps of continuously charging a detergent surfactant paste 34 and dry starting detergent material 36 into a high speed mixer- / scaler 38 to obtain the agglomerates 40 and mixing the agglomerates 40 in a moderate speed mixer / densifier 42 to densify and accumulate more and agglomerate the agglomerates 40 into agglomerates 44. The agglomerates 44 preferably have an average particle size of about 300 microns to about 900 microns. After, the agglomerates 44 are screened in a screening apparatus 46 to thereby form a first agglomeration mixture 48 having substantially a particle size of at least 6 mm and a second agglomeration mixture 50 having substantially a particle size smaller than about 6 mm. The agglomeration mixture 48 contains agglomerates of greater size-re latíva hume <The and generally represents about 2% to 5% of the agglomerates 44 before sieving. The agglomeration mixture 48 is fed into a milling unit 52 while the agglomeration mixture 50 is fed into a conditioning apparatus 54 to improve the flow properties of the agglomeration mixture 50 and to separate the mixture from the agglomeration mixture 50. agglomeration 50 in a third agglomeration mixture 56 and a fourth agglomeration mixture 58. Preferably, the agglomeration mixture 56 substantially has a particle size of less than about 150 microns and the agglomeration mixture 58 has substantially a particle size of At least 150 micras. The process 10 'comprises the recirculation of the agglomeration mixture 56 in the high speed mixer / densifier 38 for further agglomeration as described with respect to the process 10 of Figure 1. Then, the agglomeration mixture 58 is separated by means of any known process / apparatus such as the conventional screening apparatus 66 or the like in a fifth agglomeration mixture 60 and a sixth agglomeration mixture 62. Preferably, the agglomeration mixture 60 has substantially a particle size of at least 900. microns (preferably greater than 1180 microns) and the agglomeration mixture 62 has an average particle size of about 50 microns to about 1400 microns (preferably about 50 microns to about 1180 microns). The agglomeration mixture 60 containing additional agglomeration particles of larger size is introduced into the grinding apparatus 52 for grinding with the base agglomeration mixture 64. By continuing with the above operations, the agglomeration mixture 64 is recirculated in the apparatus. of conditioning 54 which may include one or more drier and fluid bed coolers as previously described. In such cases, the recycle stream of the agglomeration mixture 64 can be sent to any or a combination of said fluid bed dryers and coolers without departing from the scope of the invention. The agglomeration mixture 62 is then subjected to one or more termination steps 68 as previously described. Preferably, the method 10 'includes the step of mixing the adjunct detergent ingredients in the agglomeration mixture 62 to thereby form the high density detergent composition 70 having a density of at least 650 g / 1. The optional steps discussed with respect to method 10 are equally applicable with respect to method LO '. By way of examples, a coating agent may be added in or after the moderate speed mixer / densifier 42 to control or inhibit the degree of agglomeration. It has been found that adding a coating agent to the agglomeration mixture 62 or 58, say, before or after between the screening apparatus 66, produces a detergent composition with surprisingly improved flow properties. As previously mentioned, the coating agent is preferably selected from the group consisting of alu inosilicates, carbonates, silicates and mixtures thereof. The other optional steps such as spraying a binder material in the high speed mixer / blender 38 are useful in the process 10 'for the purpose of facilitating accumulation agglomeration. The residence times, energy input parameters, characteristics of the surfactant paste and the relationships with dry starting detergent ingredients are also preferably incorporated in the 10 'process.

PASTE AGENT SURGICAL DETERGENT The detergent surfactant paste useful in processes 10 and 10 'is preferably in the form of a viscous, aqueous paste, although the forms are also contemplated by the invention. This so-called viscous surfactant paste has a viscosity of about 5,000 cps to about 100,000 cps, most preferred of about 10,000 cps to about 80,000 cps, and contains about L? less than about 10% water, most preferred at least about 20% water. The viscosity is measured at 7Q ° C and at shear rates of about LO at 100 sec-i. In addition, the surfactant paste, if used, preferably comprises a detersive surfactant in the amounts specified above and the remainder of water and other conventional detergent ingredients. The surfactant itself, in the viscous surfactant paste, is preferably selected from non-ionic, non-ionic, zwitterionic, anti-caustic and cationic classes and compatible mixtures thereof. The detersive surfactants useful herein are described in the U.S.A. 3,664,961, Norris, issued May 23, 1972, and in the US patent. . 3,919,678, Laughlin et al., Issued December 30, 1975. Useful cationic surfactants also include those described in U.S. Pat. . 4,222,905, Coc rell, issued on September 16, 1980, and in the US patent. . 4,239,659, Murphy, issued December 16, 1980, both of which are also incorporated herein by reference. Of the surfactants, the preferred ones are ammonium and nonionic and the ammonia are the most preferred. Non-limiting examples of the preferred ammonium surfactants useful in the surfactant paste include conventional di-Ciß alkylbenzenesulfonates ("LAS") and branched chain primary C10-C20 ("AS") alkyl sulfates ("AS"). random, the secondary alkyl sulfates (2,3) of Cio-Ciß of the formula OH3 (CH2) (CH0S03"M +) CH3 and CH3 (CH2) and (CH0S03 ~ M +) CH2CH3 where xy (y +1) are whole of at least 7, preferably at least about 9, and M is a cation of solubilization in water, especially sodium, unsaturated sulfates such as oleyl sulfate, and those to C? o ~ C? s cycloalkoxides ("AEKS" especially, EO 1-7 ethoxylates) Optionally, other examples of surfactants useful in the pulp of the invention include the Cι-Ciß alkylalkoxycarboxylates (especially the EO 1-5 ethoxycarboxylates), the glycolic ethers of Cι-Ciß , the alkyl polyglycosides of Cio-Ciß and their sulfated polyglycosides sponges, and high sulfonated fatty acid esters of C12-C18. If desired, conventional amphoteric and nonionic surfactants such as C12-C18 alkyl ethoxylates ("AE") including the so-called narrow peak alkyl ethoxylates and the C6-C12 alkyl phenolalkylates (especially ethoxylates and ethoxy / mixed propoxy), betaines of C12 -Cie and sulfobetamas ("suLtainas"), Cio-Ciß amine oxides and the like, may also be included in the overall compositions. Typical examples include the C12-C18 N-methylglucamides. See UO 92/06154. Other surfactants derived from sugar include the N-alkoxy polyhydroxy fatty acid amides, such as N- (3-methox? Pro?) Gluca ida of Cio-Ciß- The N-propyl glucanides via N- C12-C18 hexyl can be used for low foaming. Conventional C10-C20 soaps can also be used. If high spurnation is desired, Cio-Cie soaps of branched chains can be used. Mixtures of surfactants to ionic and nonionic agents are especially useful. Other conventional useful surfactants are listed in the standard texts. 0 0 DRY DETERGENT MATERIAL The dry starting detergent material of processes 10 and 10 'preferably comprises a detergency improver selected from the group consisting of alurninosilicates, crystalline layered silicates and mixtures thereof, and carbonate, preferably sodium carbonate. The aluminosilicates or ion exchange materials used in the present invention as a detergency builder preferably have a high calcium ion exchange capacity and a high exchange rate. Without being limited by theory, it is believed that said high ion exchange rate and capacity are a function of several interrelated factors that are derived from the method by which the ion exchange material of alu inositol is produced. In this regard, the urninosilicate ion exchange materials used herein are preferably produced in accordance with the US patent. No. 4,605,509 to Cor ill et al. (Procter to Gamble), the disclosure of which is incorporated herein by reference. Preferably, the alumina ion exchange material is in the form of "sodium" since the potassium and hydrogen forms of the instant nosylate do not exhibit the high exchange rate and capacity as provided by the sodium form. Additionally, the alkylsilicate ion interchange material is preferably in the drier form to facilitate the production of quenched detergent agglomerates as described herein. The alumina ion exchange materials used herein preferably have particle size diameters that optimize their effectiveness as detergent builders. The term "particle size diameter" as used herein represents the average particle size diameter of a given aluminum ion exchange material as determined by conventional analytical techniques, such as microscopic determination. and scanning electron microscope (SEM). The preferred particle size diameter of the aluninosilicate is from about 0.1 micron to about 10 microns, more preferably from about 0.5 microns to about 9 microns. More preferably, the particle size diameter is about 1 to about 8 microns. Preferably, the aluininosilicate ion exchange material has the formula Naz C (Ai? 2) r (l? 2) and l H2? where yy are integers of at least 6, the molar-to-zay ratio is from about 1 to about 5 and x is from about 10 to about 264. More preferably, the aluminosilicate has the formula i2f (A102) l2 ( S1O2) 12 JXH O wherein x is from about 20 to about 30, especially about 27. These preferred aluminosilicates are commercially available, for example under the designations Zeolite A, Zeolite B and Zeolite X. Alternatively, the exchange materials of synthetically derived or naturally occurring alurninosilicate ions suitable for use can be made as described in Kru mel et al., US Patent No. 3,985,669, the description of which is incorporated herein by reference. The amininosilicates used herein are further characterized by their ion exchange capacity which is at least about 200 rng equivalent to hardness / g of CaC 3, calculated on an anhydrous basis, and which is preferably on the scale from about 300 to 352 rng equivalent to hardness / gram of CaC? 3 - Additionally, the instantaneous ion exchange materials are still characterized by their calcium ion exchange rate which is at least about 2 grains Ca + + / gallon / minute / -gum / gallon, and more preferably on the scale of about 2 grains Ca ++ / gallon / rninuto / -gram / gallon to about 6 grains Ca ++ / gallon / minute / - rarno / gallon.

INGREDIENTS DETERGENTS ATTACHED The dry starting detergent material in the present 75 The 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 builders, bleach activators, bleach activators, foam impellers or foam suppressors, anti-rust and amphi- corrosion agents, soil suspending agents, soil release agents, germicides, pH adjusters. , sources of alkalinity without detergency detergent, chelating agents, clays of type is ect ta, enzymes, enzyme stabilizing agents and perfumes. See the patent of E.U.A. 3,936,537, Baskerville, 3rd. and others, incorporated herein by reference. Other gene enhancers can generally be selected from the different phosphates, polyphosphates, phosphates, polyto-tonatos, carbonates, silicates, borates, polyhydroxysuiponates, polyacetates, carboxylates, and water-soluble polycarboxylates, alkali metal, ammonium or substituted ammonium. Preferred are the alkali metal salts, especially sodium, of the foregoing. Preferred for use herein are the phosphates, carbonates, silicates, Cι-is fatty acids, polycarboxylates and mixtures thereof. More preferred are sodium tppolium phosphate, tetrasodium pyrophosphate, citrate, tartrate, mono- and disuccinates, sodium silicate, and mixtures thereof (see below). Compared to amorphous sodium silicates, the crystalline layered sodium silicates exhibit a clearly increased calcium and magnesium ion exchange capacity. In addition, stratified sodium silicates prefer magnesium ions over calcium ions, a necessary feature to ensure that substantially all of the "hardness" is removed from the wash water. However, these crystalline layered sodium silicates are generally more expensive than amorphous silicates as well as other detergency builders. Accordingly, in order to provide a laundry detergent that can be purchased economically, the proportion of the crystalline layered sodium silicates used must be determined judiciously. The sodium silicates are crystalline ratites suitable for use in the present preferably have the formula NaMSl "? 2? + L and H2? 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 crystallized sodium silicate has the formula NaM i2? s and Hb.0 wherein M is sodium or hydrogen, and y is from about 0 to about 20. These and other crystalline stratified sodium silicates are discussed in the US patent. A. No. 4,605,509, Corkill et al., Previously incorporated herein by reference. Specific examples of inorganic phosphate builders are sodium and potassium ripolisphosphate, pyrophosphate, polymecophate metaphosphate having a degree of polymerization of about 6 to 21, and orthophosphates. Examples of polyphosphonate detergency builders are the sodium and potassium salts of ethylene diphosphate acid, the sodium and potassium salts of acid 1-d? phosphonic ethane l-h? drox? -1 and the sodium and potassium salts of acid 1, 1, 2-t ritosfonico ethane. Other phosphorus detergency builder compounds are described in the U.S. Patents. . 3,159,581; 3,213,030; 3,422,021; 3,422,137; 3,400,176 and 3,400,148, all of which are incorporated herein by reference. Examples of inorganic builders without phosphorus are tetraborate decahydrate and silicates having a weight ratio of S1O2 to alkali metal oxide of about 0.5 to about 4.0, preferably about 1.0 to about 2.4. The water-soluble non-phosphorus organic builders useful in the present include the different alkali metal, substituted ammonium and ammonium polyacetates, carboxylates, polyarboxylates and polyhydroxy sulfonates. Examples of polyacetate and polycarboxylate buil are the sodium, potassium, lithium, ammonium and ammonium salts substituted with tetraacetic acid of ethylendia, acid or trilotipaetic acid, oxydisuccinic acid, ethylic acid, benzene polycarboxylic acids, and citric acid. Polimepco polycarboxy buil are established in the F.U.A. patent. 3,308.06 ?, Diehl, issued March 7, 1967, the description of which is incorporated herein by reference. Such materials include the water-soluble salts of aliphatic carboxylic acids such as rnalene acid, taconic acid, rnesaconic acid, fumaric acid, aconitic acid, citraconic acid and methalene methacrylic acid. Some of these materials are useful with the water soluble ammonium polymer as described below, but only if in intimate admixture with the ammonium surfactant without soap. Other polycarboxylates suitable for use in the present are the polyacetal carboxylates described in the U.S. patent. . 4,144,226, issued March 13, 1979, to Crutchfield et al., And US patent. A. 4,246,495, issued March 27, 1979 to Crutchf eld and others, both of which are incorporated herein by reference. These polyacetal carboxylates can be prepared by joining a glyoxylic acid ester and a polymerization initiator unpolymerization conditions. The resultant polyacetal carboxylate ester is then added to chemically stable end groups to stabilize the polyacetal carboxylate against rapid descaling in alkaline solution, converted to the corresponding salt, and added to a detergent composition. Particularly preferred polycarboxylate buil are ether carboxylate builcompositions which comprise a combination of tartrate monosuccinate and tartrate disuccinate described in US Pat. 4,663,071, Bush et al., Issued May 5, 1987, the description of which is incorporated herein by reference. Bleaching agents and activators are described in the US patent. . 4,412,934, Chung et al., Issued November 1, 1983, and in the US patent. A. 4,483,781, Hartnan, issued November 20, 1984, both incorporated herein by reference. Chelating agents are also described in the US patent. . 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 the 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., Both incorporated herein by reference. Smectite-type 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. Additional buil suitable for use herein are listed in the Bas erviel patent, column 13, line 54 to column 16, line 16, and in the US patent. . 4,663,071, Bush et al., Issued May 5, 1987, both incorporated herein by reference. To make the present invention better untood, reference is made to the following examples, which are intended to be illustrative only and to limit the scope.

EXAMPLE 1 This example illustrates the process of the invention that produces high density, free flowing, cleansing detergent composition. Two charging streams of several starting detergent ingredients are continuously fed, at a rate of 2800 kg / hr, into a CB-30 buffer mix / densifier, one of which comprises a surfactant paste containing surfactant and water and the stream containing dry starting detergent material containing aluminosilicate and sodium carbonate. The rotary speed of the arrow in the Lodige CB-30 mixer / ensix is approximately 1400 rpm and the average residence time is approximately 10 seconds. The agglomerates of the Lodige CB-30 mixer / densifier are continuously fed into a Lodige KM-600 densifier / densifier for further agglomeration when said average residence time is about 6 minutes. The resulting detergent agglomerates are then fed to a conditioning apparatus including a fluid bed dryer and then to a fluid bed cooler, the residence time being around LO minutes and 15 minutes, respectively. Minor size or "fine" agglomeration particles (less than about 150 microns) from a dryer and fluid bed cooler are recirculated in the Lodige CB-30 mixer / blender. A coating agent, aluminosiliate, is fed immediately after the Lodige KM-600 mixer / densifier but before the fluid bed dryer to improve the flow of the agglomerates. The detergent agglomerates exiting the fluid bed cooler are screened, after the detergent ingredients attached thereto are mixed therewith to give a fully formulated detergent product having a uniform particle size distribution, the composition of the detergent agglomerates which Exit the fluid bed cooler set out in Table 1 below: TABLE I Component% by weight Alkyl Sulfate / C14-15 Alkylethoxysulfate 30.0 Aluminosilicate 37.8 Sodium carbonate 19.1 Mise, (water, perfume, etc.) 13.1 100.0 The density of the agglomerates in Table I is 750 g / 1 and the average particle size is 475 microns. The attached liquid detergent ingredients including perfumes, brighteners and enzymes are sprayed in or mixed for the agglomerates / particles described above in the finishing step to give a fully formulated finished detergent composition. The relative proportions of the overall finished detergent composition produced by the instant process procedure are presented in Table II below: TABLE II Component (% by weight) Alkyl sulfate of C? - i5 / to the uiletoxisul f "• of Ci4- i5 / linear alkylbenzene fonate d ': \ 2 21 .6 Polyacrylate (molecular weight 4500) 2.5 Polyethylene glycol (molecular weight 4000) 1.7 Sodium sulfate 6.9 Aminosinosilicate 25.6 Sodium carbonate 17.9 Enzyme p otase 0.3 Ceiulase enzyme 0.4 Enzyme 1ipasa 0.3 Minors (water, perfume, etc.) 22.8 100.0 The density of the detergent composition in Table II is 660 g / 1.

EXAMPLE II This example illustrates another method according to the invention wherein the steps described in example I are carried out in addition to the following steps: (1) sieving the agglomerates that leave the LODGE KM-600 so that the particles of larger size (per at least about 4 rnn) are sent to a grinder; (2) sieving the agglomeration particles of larger size (at least about 1180 microns) that leave the fluid bed cooler and send those larger particles to the grinder, likewise; and (3) introducing the larger base size particles in the fluid bed dryer and / or fluid bed cooler and the termination steps (mixing and / or spraying of the attached ingredients). The composition of the detergent agglomerates that come out of the fluid bed cooler is established in Table III a below: TABLE III Component% by weight Alq? Ils? I fato / alqui letox i sul fato de Cm - i s 30.0 Alurninosilicate 37.8 Sodium carbonate 19. L Mise, (water, perfume, etc.) 13. 1 100.0 The density of the agglomerates in Table I is 750 g / 1 and the average particle size is 425 microns. The agglomerates also surprisingly have a narrower particle size distribution, wherein more than 90% of the agglomerates have a particle size between about 150 microns to about 1180 microns. This result is unexpectedly equal to the particle size distribution of agglomeration (ie, all agglomerates below 1180 microns) more closely. The attached liquid detergent ingredients including perfumes, brighteners and enzymes are sprayed on or mixed for the agglomerates / particles described above in the step of finishing to give a fully formulated finished detergent composition. The relative proportions of the overall finished detergent composition produced by the procedure of the instant procedure is presented in Table IV below: TABLE IV Component (X in 1 weight) B Ci ^ -is alkylsulfate / alkylethoxy Ci4-i5 ulfate / linear C12 alkylene lsencene sulfonate 21. 6 Poliacplato (molecular weight 4500) 2. 5 Polyethylene glycol (molecular weight 4000) 1. 7 Sodium sulphate 6. 9 Al urninosi licato 25. 6 Sodium carbonate 17. 9 Enzyme protea a 0. 3 Cellulase enzyme 0. 4 Enzyme Lipase 0. 3 Minors (water, perfume, etc.) 22. 8 100.0 The density of the detergent composition in the quadr TV is 660 g / l. In this way, after having described the invention in detail, it will be clear to those skilled in the art that various changes can be made without departing from the scope of the invention and the invention should not be considered as limiting to what has been described in specification.

Claims (20)

NOVELTY OF THE INVENTION CLAIMS

1. - A method for continuously preparing a high density detergent composition comprising the steps of: (a) continuously charging a detergent surfactant paste and dry starting detergent material in a high speed mixer / densifier to obtain the agglomerates; (b) mixing said agglomerates in a moderate speed softener / densifier to further densify, agglomerate and agglomerate said agglomerates so that said agglomerates have an average particle size of from about 300 microns to about 900 microns; (c) feeding said agglomerates in a conditioning apparatus to improve the flow properties of said agglomerates and to separate said agglomerates in a first agglomeration mixture and a second agglomeration mixture, wherein said first agglomeration mixture has a substantially one size of particle less than about 150 microns and said second agglomeration mixture has substantially a particle size of at least about 150 microns; (d) recirculating said first agglomeration mixture in said high speed mixer / ensiler for further agglomeration; (e) mixing the adjunct detergent ingredients in said second agglomeration mixture to thereby form said high density detergent composition.

2. A method according to claim 1, further characterized in that said conditioning apparatus comprises a fluid bed dryer and a fluid bed cooler.

3. A process according to claim 1, further characterized in that the ratio of said surfactant paste and said dry detergent material is from about 1:10 to about 10: 1.

4. A process according to claim 1, further characterized in that said dry starting material comprises a builder selected from the group consisting of alu-silicates, crystalline layered silicates, and mixtures thereof and carbonate of sodium.

5. A process according to claim 1, further characterized in that the density of said detergent composition is at least 650 g / 1.

6. A method according to claim 1, further characterized in that it comprises the step of adding a coating agent after said moderate speed mixer / densifier, wherein said coating agent is selected from the group consisting of urní nosi licatos, carbonates, silicates and mixtures thereof.

7. A method according to claim 1, further characterized in that the average residence time of said agglomerates in said high speed mixer / densifier is on a scale of about 2 seconds to about 45 seconds.

8. A method according to claim 1, further characterized in that the average residence time of said agglomerates in said moderate speed mixer / densifier is in the range of about 0.5 minutes to about 1.5 minutes.

9. A method according to claim 1, further characterized by compressing the passage of the spray to a binder material in said high speed mixer / densifier.

10. A method according to claim 9, further characterized in that said binder is selected from the group consisting of water, ammonium surfactants, nonionic surfactants, polyethylene glyool, polyvinyl pyrrolidone, polyacrylates, citric acid and mixtures thereof.

11. A method according to claim 1, further characterized in that said ratio of said surfactant paste to said dry detergent material is from about 1: 4 to about 4: 1.

12. A method according to claim 1, further characterized in that said surfactant paste has a viscosity of about 5,000 cps to about 10,000 cps.

13. A process according to claim 1, further characterized in that said surfactant paste comprises water and a surfactant selected from the group consisting of ammonium, nonionic, z itteponic, ampholytic and cation ionic surfactants. and mixtures thereof.

14. A method according to claim 1, further characterized in that said moderate speed mixer / densifier imparts from about 5 x 10 ° erg / 1 to about 2 x 1012 erg / kg of energy at a speed of about 3 x 108 erg / kg-sec to approximately 3 x 10? erg / kg-sec.

15. A method according to claim 1, further characterized in that it comprises the step of adding a coating agent in said moderate speed mixer / densifier.

16. A process for continuously preparing a high density detergent composition comprising the steps of: (a) continuously charging a detergent surfactant paste and dry starting detergent material into a high speed mixer / densifier to obtain agglomerated; (b) mixing said agglomerates in a moderate speed mixer- / densitator to further densify, agglomerate and agglomerate said agglomerates so that said agglomerates have an average particle size of from about 300 microns to about 900 microns; (c) sieving said agglomerates to thereby form a first agglomeration mixture having substantially a particle size of at least about 6 nm and a second agglomeration mixture having substantially a particle size less than 6 nm; (d) feeding said first agglomeration mixture into a grinding apparatus and said second agglomeration mixture in a conditioning apparatus and for separating said second agglomeration mixture into a third agglomeration mixture and a fourth agglomeration mixture, wherein said third agglomeration mixture has substantially a particle size of less than about 150 microns and said fourth agglomeration mixture has substantially a particle size of at least about 150 microns; (e) recirculating said third agglomeration mixture in said high speed densifier / densifier for further agglomeration; (f) separating said fourth agglomeration mixture into a fifth agglomeration mixture and a sixth agglomeration mixture, wherein said fifth agglomeration mixture has a particle size of at least about 900 microns and said sixth agglomeration mixture has? n average particle size around - from 50 microns to approximately 1400 microns; (g) introducing said fifth agglomeration mixture into said grinding apparatus for milling with said first agglomeration mixture to form a base agglomeration mixture which is recirculated in said conditioning apparatus; and (h) mixing the adjunct detergent ingredients in said sixth agglomeration mixture to thereby form said high density detergent composition.

17. A process according to claim 16, further characterized in that it comprises the step of adding a coating agent to said sixth agglomeration mixture between said separation step and said mixing step, wherein said coating agent is selected from the group consisting of aluminosi licatos, carbonatoe, silicates and mixtures thereof.

18. A method according to claim 16, further characterized in that said conditioning apparatus comprises a fluid bed dryer and a fluid bed cooler.

19. A high density detergent composition made in accordance with the process of claim 1.

20. A high density detergent composition made in accordance with the method of claim 1.