MXPA98008660A - Procedure for the preparation of high density detergent using a highly surfacing paste that has better stability - Google Patents

Abstract

The present invention relates to: A process is provided for preparing detergent agglomerates in which a highly surfactant paste and a detergency builder are agglomerated together. The process includes keeping the highly surfactant paste in a highly stable, pumpable and transportable form over a prolonged period, thus, the process facilitates the large-scale manufacture in multiple locations of modern compact detergent products, in particular the highly surfactant paste. can be manufactured in a facility and then stored and transported to a separate facility for further treatment to form the finished detergent agglomerates

Description

PROCEDURE FOR PREPARATION OF HIGH DENSITY DETERGENT. USING A HIGHLY SURFACTATING PASTE THAT HAS IMPROVED STABILITY FIELD OF THE INVENTION In general terms, the present invention is directed to a process for preparing high density detergent compositions from a highly surfactant paste and other detergent ingredients. More particularly, the invention is directed to a process for producing a high density detergent composition in the form of agglomerates, with which the stability and storage life of a highly surfactant paste is unexpectedly improved. This method is especially useful in the production of modern compact granular detergent compositions that typically require higher levels of detersive surfactants.

BACKGROUND OF THE INVENTION Within the detergent industry, there has recently been considerable interest in laundry detergents that are "compact" and therefore have low dosage volumes. To facilitate the production of these so-called low dosage detergents, they have been many attempts to produce high density global detergents, for example with a density of 650 g / 1 or higher. Currently, low dosage detergents are in high demand because they conserve resources and can be sold in small packages that are more convenient for consumers. In general, there are two main types of processes by which granules or detergent powders can be prepared. The first type of process includes spray drying an aqueous detergent suspension in a spray drying tower to produce highly porous detergent granules. In the second type of process, various detergent components are mixed, and then agglomerated with a nonionic or anionic detergent paste which also serves as a binder for the agglomerated particles. In both processes, the most important factors that govern the density of the resulting detergent granules are the density, porosity and surface area of the different starting materials and their respective chemical composition. However, these parameters 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 treatment steps leading to the densification of the detergent granules or by agglomeration-forming processes.

The technique is replete with methods directed to the agglomeration to produce detergent compositions. For example, attempts have been made to agglomerate builders by mixing zeolite and / or layered silicates in a mixer to form free flowing agglomerates. Another example includes a starting detergent material in the form of highly viscoelastic surfactant paste, which is agglomerated with dry powders, such as aluminosilicates and carbonates, to form highly dense, free-flowing, brittle, detergent agglomerates. However, a variety of problems have been encountered with the handling of highly viscoelastic surfactant pastes of higher activity which are used to produce high density, high activity detergent agglomerates, suitable for modern low dosage detergent products. Specifically, these highly surfactant pastes are extremely sensitive to parameters of the environment and the operation equipment, all of which makes it difficult to transport, store and process the pastes during the production of the detergent agglomerates. Typically, the surfactant pastes are manufactured by a process in which a fatty alcohol is sulfated and then neutralized with an alkaline material (e.g., sodium hydroxide). This is an extremely delicate process, especially when it is used to produce predominantly (more than 60% by weight) highly surfactant pulps containing the surfactant and only a relatively smaller amount of water and auxiliary ingredients. The resulting highly surfactant pastes are extremely sensitive to their environment, for example, to the high temperature zones or "hot spots" of the equipment (pipes, valves, storage tanks and the like) to which it is exposed, as well as to any contaminant that is in the paste that has a pH of less than 7. In the case in which the highly surfactant paste is exposed to one or more of these factors of the environment, these highly active pastes tend to undergo a hydrolysis reaction , where the surfactant is reverted to its alcohol form. This hydrolysis reaction is an autocatalytic reaction, since a by-product is an acid that continues to react with any remaining surfactant. This threat of hydrolysis particularly exacerbates the sensitivity to the environment of highly active surfactant pastes and makes it difficult to keep them stable for the periods necessary for the large-scale commercial manufacture of modern compact laundry detergents (for example 2 to 7 days). It should be understood that even hydrolysis of 1% by weight of the surfactant paste can have major financial consequences in the large-scale commercial manufacture of detergent products. Typical attempts of the prior art in this area included the immediate formation of surfactant particles after making the pulp. However, for This requires that the particle formation equipment be "in the same place", or that the surfactant manufacturing equipment be located in or near the detergent manufacturing facilities. Currently, the detergent manufacturing and surfactant manufacturing industries have separated physically and commercially, a trend that is only growing. Thus, it would be convenient to have a highly surfactant paste that remains stable for longer periods, to be able to locate the surfactant preparation operation apart from the detergent manufacturing facilities, which is more representative of the current commercial environment. Another challenge with the use of these highly surfactant pastes includes their rheological properties, since they must have a sufficiently low viscosity to be pumped to and from trucks and transport trains, and to storage tanks and out of them, in the facilities of detergent manufacture. Any significant change in temperature can lead to undesirable gelification or solidification of the surfactant paste, resulting in increased costs and manufacturing time. Note, however, that different rheological properties of the surfactant paste may arise after reheating. Also in that regard, additional ingredients such as carbonates are included to maintain the Storage stability and transport of the surfactant paste before being treated, have the effect of increasing the viscoelasticity of the highly surfactant paste, thus making its treatment very difficult. The difficulty in the treatment arises due to a change in the viscoelasticity of the surfactant paste, which requires the implementation of relatively expensive high-pressure pumps, more pipeline and shorter transport distances in the detergent preparation process. As a consequence, it would be convenient to have a process with which the stability of the stored dough is maintained without sacrificing its treatment capacity. Accordingly, despite the above-mentioned disclosures in the art, there remains a need for a process for producing an agglomerated detergent composition from a highly surfactant paste which is sufficiently stable during transport and storage for sufficient periods to allow commercial manufacture to large scale of modern compact detergent compositions. There also remains a need for such a process that is not expensive and can be easily incorporated into large-scale production facilities of low-dosage or compact detergents.

TECHNICAL BACKGROUND The following references are directed to surfactant pastes: Aouad et al., WO 93/18123 (Procter &Gamble); Aouad et al., WO 92/18602 (Procter &Gamble); Aouad et al., EP 508,543 (Procter &Gamble); Mueller et al., Patent of E.U.A. No.5, 152, 32; Strauss et al., Patent of E.U-. No. 5,080,848 (Procter &Gamble); Ofosu-Asante et al., Patent of E.U.A. No. 5,066,425 (Procter &Gamble); Jolicoeur et al., U.S. Patent No. 5,045,238 (Procter &Gamble); and Van Zorn et al., EP 504,986 (Shell). The following references are directed to the densification of spray-dried granules: Appel et al., Patent of E.U.A. No. 5,133,924 (Lever); Bortolotti 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 No. 451,894. The following references are directed to the production of detergents by agglomeration: Beerse et al., U.S. Pat. No. 5,108,646 (Procter &Gamble); Capeci et al., Patent of E.U.A. No. 5,366,652 (Procter &Gamble); Capeci et al., Patent of E.U.A. No. 5,486,303 (Procter &Gamble); Capeci et al., Patent of E.U.A. No. 5,489,392 (Procter &Gamble); Hollingsworth et al., European Patent Application No. 351,937 (Unilever); and S atling et al., U.S. Patent. No. 5,205,958.

BRIEF DESCRIPTION OF THE INVENTION The present invention covers the needs identified above, providing a process for preparing detergent agglomerates from a highly surfactant paste and a builder. There is a significant advantage with this process, since the surfactant paste is stable, pumpable and transportable over a prolonged period, in such a way that it facilitates the large-scale manufacture and in multiple locations of modern compact detergent products. In particular, highly active surfactant paste can be manufactured in one facility and then stored and transported to another remote facility to convert it later into finished detergent agglomerates. As used herein, the term "contaminant" means any foreign substance with which the surfactant paste makes contact while it is stored and transported before the introduction and agglomeration steps of the process. Examples of these contaminants include, but are not limited to, multiple colored residues of sulfuric acid, sodium sulfate, fatty alcohol, iron, chromium and nickel. As used herein with respect to the surfactant paste, the term "stable" means that the surfactant paste substantially retains its formulation containing a neutralized surfactant and is not significantly reverted by hydrolysis to its alcohol form. As used herein with respect to the surfactant paste, the term "treatable" means that the surfactant paste retains its convenient rheological properties to allow its use in the current process, which typically means that it will have a viscosity as detailed below. regarding the Power Law Model. As used herein, the term "agglomerate" refers to particles formed by agglomeration of granules or detergent particles that typically have a smaller average particle size than the agglomerates formed. All percentages and ratios used herein are expressed as percentages by weight (on anhydrous basis), unless otherwise indicated. All documents are incorporated here by reference. All viscosities referred to herein are measured at 70 ° C (± 5 ° C), and at cutting speeds of about 10 to 100 sec-1, unless otherwise indicated. In accordance with an aspect of the invention, a process for producing detergent agglomerates is provided. The method comprises the steps of: (a) providing a non-linear viscoelastic surfactant paste including, by weight of the surfactant paste, from about 70% to 95% of a detersive surfactant, from about 5% to about 30% water, and an excess amount of an alkali metal hydroxide so that the pH of the surfactant paste is at least about 10; (b) regulate the temperature of the surfactant paste within a scale of approximately 50 ° C at about 80 ° C, so that the surfactant paste is treatable and stable for at least 48 hours; (c) charging the surfactant paste in a high speed mixer / densifier; (d) introducing from about 1% to about 70% by weight of a builder in the high speed mixer / densifier; and (e) agglomerating the surfactant paste with the improver, treating the surfactant paste and the improver initially in the high speed mixer / densifier and subsequently in a moderate speed mixer / densifier to form the detergent agglomerates. In accordance with a highly preferred aspect of the invention, another method for producing detergent agglomerates is provided. The method comprises the steps of: (a) providing a non-linear viscoelastic surfactant paste including, by weight of the surfactant paste, about 70% to 80% of a mixture of C14-15 alkyl sulfate surfactant and linear alkylbenzene sulfonate surfactant of Ci2-13, from about 15% to about 20% water, from about 2% to about 8% polyethylene glycol and from about 0.5% to about 1% sodium hydroxide so that the pH of the surfactant paste is at least approximately 11; (b) regulating the temperature of the surfactant paste within a range of about 65 ° C to about 70 ° C such that the surfactant paste is treatable and stable for at least 120 hours; (c) charging from about 1% to about 50% by weight of the surfactant paste in a high speed mixer / densifier; (d) introducing from about 1% to about 70% by weight of a detergency builder in the high speed densifier / densifier; (e) agglomerating the surfactant paste and the improver by treating the surfactant paste and the improver initially in the high speed mixer / densifier, and subsequently in a moderate speed mixer / densifier to form the detergent agglomerates; and (f) drying the detergent agglomerates. The present invention also provides detergent compositions comprising detergent agglomerates made in accordance with any of the methods described herein. Accordingly, an object of the invention is to provide a process for producing an agglomerated detergent composition from a highly surfactant paste which is sufficiently stable during transport and storage for sufficiently long periods, in such a manner as to allow large-scale commercial manufacture of compositions. modern compact detergents. Also, an object of the invention is to provide such a process that is cheap and can be easily incorporated in large-scale production facilities of low-dosage or compact detergents. These and other concomitant objects, features and advantages of the present invention will become apparent to the person skilled in the art of reading the following detailed description of the preferred embodiment and the appended claims.

DETAILED DESCRIPTION OF THE PREFERRED MODALITY In general, the present process is used in the production of low dosage detergents, whereby the resulting detergent agglomerates can be used as a detergent or as a detergent additive. In particular, the process can be used to form "high activity" (ie, high level surfactant) detergent agglomerates that are used as a mixture for the purpose of increasing activity levels in low dosage granular detergents, and thereby have more compact detergents.

Procedure The process produces high density, free-flowing detergent agglomerates, preferably with a density of at least 650 g / 1. The process produces high density detergent agglomerates from a highly viscoelastic surfactant paste having a relatively low water content. In the past, the treatment and storage of certain highly surfactant, highly viscoelastic pastes has been a problem, especially in light of their sensitivity to temperature variations and pollutants of acid nature. Although not intended to be limited by theory, it is believed that these temperature variations, and acidic contaminants, cause the autocatalytic hydrolysis reaction of the surfactant paste that effectively reverts the surfactant paste to an aqueous solution of alcohol that can not be treated. Therefore, it has been found that optimally selected temperature scales and contaminant pH scales must be regulated to produce the desired detergent agglomerates that are used in modern compact detergent products. In the first step of the process, a non-linear viscoelastic surfactant paste is provided which is characteristic of many highly viscoelastic, highly active pastes used in the production of high density detergent agglomerates. The phrase "non-linear viscoelastic" means that the pulp has a non-linear fluid velocity profile and exhibits viscoelastic fluid behavior, i.e., it can be extended during its flow such as a chewing gum or the like. Until now, it has been very difficult to treat and maintain these non-linear viscoelastic surfactant pastes stable. Preferably, the surfactant paste comprises, by weight of the surfactant paste, from about 70% to about 95%, preferably from about 70% to about 85%, and preferably from about 70% to about 75%, of a surfactant detersive.

In a preferred embodiment, the surfactant paste is a mixture of alkyl sulfate surfactants ("AS") of C14-15 and linear alkylbenzene sulfonate ("LAS") of C12-13, in a weight ratio of about 1: 1 to about 5. : 1 (AS: LAS). Another preferred embodiment herein contemplates a surfactant paste blend having a weight ratio of C14-15 alkyl sulfate to linear Ciais alkylbenzenesulfonate of about 3: 1. Other optional surfactant systems include pure AS or pure LAS surfactants in the pastes, as well as alkyl ethoxy sulfate systems ("AES") in which the AES is the only surfactant in the pulp or one of them. The surfactant paste also includes from about 5% to about 30%, preferably from about 15% to about 25%, preferably from 15% to about 20% by weight of the paste, of water. In addition, the pulp includes from 0.1 to about 10%, preferably from about 1% to about 8%, preferably from about 2% to about 8% by weight of the pulp, of polyethylene glycol- The surfactant paste also contains about 0.01% to about 5%, preferably from about 0.1% to about 1%, and preferably from about 0.5% to about 1% by weight of the paste, of an alkali metal hydroxide which is preferably sodium hydroxide. Also included in the surfactant paste are minor ingredients such as unreacted alcohols, sulfates and the like, although it is preferable to keep these amounts to a minimum. In the subsequent step of the process, the surfactant paste is regulated within a temperature range from about 50 ° C to about 80 ° C, preferably from about 60 ° C to about 75 ° C, preferably about 65 ° C to approximately 70 ° C. Preferably, the regulation step maintains or makes the surfactant paste stable for at least 48 hours, preferably for at least 72 hours and preferably for at least 170 hours. In this way, the likelihood that the surfactant paste undergoes the undesirable hydrolysis reaction and / or the difficulty in transporting and treating it due to intolerable rheological properties such as high viscosity is eliminated. In addition, it is preferred that the surfactant paste be substantially free of gas producing materials when reacting with an acid. These materials include carbonates, perchonates, perborates or any other material that produces gas after its contact with an acidic material. Although not intended to be limited by theory, it is considered that if the surfactant paste includes said gas producing material, it will react with any acidic contaminating material to produce a gas that propagates through the remaining surfactant paste, thereby creating a "channel" or "route" through which the acid pollutant can pass through the paste. This it facilitates the hydrolysis reaction of all the surfactant paste, unlike only a small isolated hydrolysis incident which otherwise would not affect the total composition of the surfactant paste. Also in this regard, it is preferable in the current process to keep the surfactant paste substantially free of contaminating materials having a pH of less than about 7. In the next step of the process, the surfactant paste is loaded in a high speed mixer / densifier (eg Lódige Recycler CB 30) which typically operates on a scale from 300 rpm to approximately 2500 rpm. In this step, in the process from about 25% to about 65%, preferably 30% to about 60%, and preferably from 35% to about 55% by weight, of the surfactant paste is used to prepare the agglomerates. Also, they are introduced into the high speed mixer / densifier from about 1% to about 70%, preferably from about 5% to about 70%, and preferably from about 50% to about 70% by weight, of a slurry improver. detergency Although other builders can be used in the process as described below, the aluminosilicate builder is preferred. The surfactant paste and builder are agglomerated by treating the paste and the improver initially in the high speed mixer / densifier and subsequently in a moderate speed mixer / densifier (see Lódige Recycler KM 300"Ploughshare" which has a large central arrow operating on the scale from 100 rpm to 300 rm), to form detergent agglomerates. Other suitable equipment for use as the high speed mixer / densifier or moderate speed mixer / densifier is described in the U.S. Patent. No. 5,366,652, the description of which is incorporated herein by reference. Optionally, other conventional detergent ingredients can also be introduced as described below in the high speed mixer / densifier and / or the moderate speed mixer / densifier to make a fully formulated detergent agglomerate. The surfactant paste, builder and other optional starting detergent materials are sent to a moderate speed mixer / densifier for the subsequent formation of agglomerates having a density of at least 650 g / 1, and preferably of approximately 700. g / 1 to approximately 900 g / 1. Preferably, the average residence time of the surfactant paste and other starting detergent materials in the high-speed mixer / densifier (eg, the Lódige Recycler CB 30 mixer / densifier) is from about 1 to 30 seconds, whereas the time of residence in the low or moderate speed mixer / densifier (eg, Lódige Recycler KM 300"Ploughshare" mixer / densifier) is approximately 0.25 to 10 minutes.

Inevitably, a certain amount of the agglomerates leaving the moderate speed densifier / densifier will be below the predetermined particle size scale and optionally, they can be separated and recirculated back to the high speed mixer / densifier for the subsequent formation of agglomerates. . In this regard, these agglomerates, referred to as "smaller" or "thin", will comprise from about 5% to about 30% by weight of the detergent agglomerates. The particle porosity of the resultant detergent agglomerates produced in accordance with the process of the invention is preferably in the range of about 5% to about 20%, preferably about 10%. The combination of the porosity referred to above and the particle size, results in agglomerates having density values of 650 g / 1 and higher. Such a feature is especially useful in the production of low dosage laundry detergents as well as in other granular compositions such as dishwashing compositions. The process may comprise the steps of sprinkling an additional binder in the mixer / densifier used in the agglomeration step to facilitate the production of the desired detergent agglomerates. A binder is added in order to increase the agglomeration by providing a "binding" or "adhesion" agent for the detergent components. The binder is preferably selected from the group consisting of water, anionic surfactants, nonionic surfactants, polyethylene glycol, polyacrylates, citric acid and mixtures thereof. Other suitable binding materials, including those listed herein, are described in Beerse et al., U.S. Pat. No. 5,108,646 (Procter &Ga Co.), the disclosure of which is incorporated herein by reference. Another optional step contemplated by the present method includes conditioning the detergent agglomerates by drying the detergent agglomerates after passing through the moderate speed mixer / densifier. Another optional step includes adding a coating agent (eg aluminosilicates, carbonates, sulfates or any other dry powder material) to the detergent agglomerate before or after leaving the moderate speed mixer / densifier, in order to increase the flowability of agglomerates (that is, reduce cake formation). This further increases the condition of the detergent agglomerates to be used as an additive or to place them in dispensable or packable form. Those skilled in the art will appreciate that a wide variety of methods can be used to dry and cool the resulting detergent agglomerates without departing from the scope of the invention. By way of example, apparatuses such as a fluidized bed can be used for dry, while an air siphon can be used to cool if necessary.

Tensioactive Paste The viscoelastic surfactant paste used herein has viscoelastic fluid properties that can be described by means of a commonly used mathematical model that takes into account the shear thinning nature of the pulp. The mathematical model is called the Power Law Model and is described by means of the following relationship: where s = shear stress (dynes / cm2), K = Consistency (oise * sec "-1), t = Cut-off regime (sec-1), and n = regime index (dimensionless) The rate index n varies from 0 to 1. The closer to 0 is n, it will be The shear thinning of the fluid is greater, the closer n is to 1, the closer it will be to a simple Newtonian behavior, ie constant viscosity behavior, K can be interpreted as the apparent viscosity at a cutting rate of 1 sec. 1. In this context, the viscoelastic surfactant paste used in the process has a K consistency, at 70 ° C, from about 50,000 to about 250,000 cPoise * sec -1 (500 to 2,500 Poise * sec-1), preferably from approximately 100,000 to approximately 195,000 cPoise ^ sec "-1 (1,000 to 1,950 Poise * sec" -1), and is highly preferred from approximately 120,000 to approximately 180,000 cPoise »sec "- (1,200 to 1,800 Poise" according to?) Preferably, the surfactant paste has a shear rate n of about 0.05 to about 0.25, preferably about 0.08 to about 0.20, and about 0.10 is most preferred. at about 0.15 The surfactant can be selected from the anionic, nonionic, zwitterionic, ampholytic and cationic classes and compatible mixtures thereof Detergent surfactants useful herein are described in US Patent No. 3,664,961, orris. , issued May 23, 1972, and in U.S. Patent No. 3,919,678, Laughlin et al., issued December 30, 1975, both of which are incorporated herein by reference. Useful ionics also include those described in U.S. Patent No. 4,222,905, Cockrell, issued September 16, 1980, and in U.S. Pat. No. 4,239,659, Murphy, issued December 16, 1980, both are incorporated herein by reference as well. Of the surfactants, anionics and nonionics are preferred, and anionics are highly preferred. The following are representative examples of detergent surfactants useful in the present dough surfactant. The water-soluble salts of the higher fatty acids, ie the "soaps" are useful anionic surfactants in the compositions herein. These include alkali metal soaps such as sodium, potassium, ammonium and alkylolammonium, of higher fatty acids containing from about 8 to about 24 carbon atoms, preferably from about 12 to about 18 carbon atoms. The soaps can be made by direct saponification of fats and oils or by neutralization of free fatty acids. Particularly useful are the sodium and potassium salts of the fatty acid mixtures of coconut oil and tallow, ie tallow and coconut soap of sodium or potassium. Additional anionic surfactants suitable for use herein include the water soluble salts, preferably the alkali metal, ammonium and alkylammonium salts, of organic sulfuric reaction products having in their molecular structure an alkyl group containing from about 10 to about 20 carbon atoms and a sulfonic acid or sulfuric acid ester group (the alkyl portion of acyl groups is included in the term "alkyl"). Examples of this group of synthetic surfactants are the sodium and potassium alkyl sulfates, especially those obtained by sulfating the higher alcohols (8 to 18 carbon atoms) such as those produced by reducing the glycerides of tallow or coconut oil; and the sodium and potassium alkylphennesulfonates, in which the alkyl group contains from about 9 to about 15 carbon atoms, in branched or straight chain configuration, for example, those of the type described in the patents of E.U.A. Nos. 2,220,099 and 2,477,383. Particularly valuable are linear straight-chain alkylbenzene sulphonates in which the average number of carbon atoms in the alkyl group is from about 11 to 13, abbreviated as LAS Cn-13. Other suitable anionic surfactants for use herein are alkyl glyceryl ether sulfonates. sodium, especially those ethers of higher alcohols derived from tallow and coconut oil; monoglyceridesulfonates and fatty acid sulfates of sodium coconut oil; sodium or potassium of ethylene oxide per molecule and wherein the alkyl groups contain from about 8 to about 12 carbon atoms; and sodium and potassium salts of ethylene oxide alkyl ether sulphates containing from about 1 to about 10 ethylene oxide units per molecule, and wherein the alkyl group contains from about 10 to about 20 carbon atoms. In addition, suitable anionic surfactants include the water-soluble salts of alpha-sulfonated fatty acid esters containing from about 6 to 20 carbon atoms in the fatty acid group, and from about 1 to 10 carbon atoms in the ester group; water-soluble salts of 2-acyloxyalkane-1-sulfonic acids containing about 2 to 9 carbon atoms in the acyl group and from about 9 to about 23 carbon atoms in the alkane portion; alkyl ether sulphates containing from about 10 to 20 carbon atoms in the alkyl group and from about 1 to 30 moles of ethylene oxide; water-soluble salts of olefin and paraffinsulfonates containing from about 12 to 20 carbon atoms; and beta-alkyloxy alkane sulfonates containing from about 1 to 3 carbon atoms in the alkyl group and from about 8 to 20 carbon atoms in the alkane portion. Preferred anionic surfactants are linear C 1 -i β alkyl benzene sulphonate and C?-ß-ß alkyl sulfate If desired, low moisture content alkylsulfate pulp (less than about 25% water) may be the only ingredient in the surfactant paste. Preferred are Cis-alkylsulfates, linear or branched, and any of primary, secondary or tertiary. A preferred embodiment of the present invention is wherein the surfactant paste comprises from about 20% to about 40% of a mixture of linear sodium alkylbenzenesulfonate of C10-13 and sodium alkyl sulfate of C12-16, in a weight ratio of about 1: 1 to 1: 2. Another preferred embodiment of the detergent composition includes a mixture of C?-18 alkyl sulfate and C al--al alkylethoxysulfate in a weight ratio of about 80:20.

Water-soluble nonionic surfactants are also useful in the present invention. These nonionic materials include compounds produced by the condensation of alkylene oxide groups (hydrophilic in nature) with an organic hydrophobic compound which may be aliphatic or alkylaromatic in nature. The length of the polyoxyalkylene group that condenses with any particular hydrophobic group can be easily adjusted to produce a water-soluble compound having the desired degree of balance between hydrophilic and hydrophobic elements. Suitable nonionic surfactants include the polyethylene oxide condensates of alkylphenols, for example, the condensation products of alkylphenols having an alkyl group containing from about 6 to 15 carbon atoms, in either straight chain or branched chain configuration , with about 3 to 12 moles of ethylene oxide per mole of alkylphenol. The water-soluble and water-dispersible condensation products of aliphatic alcohols containing from 8 to 22 carbon atoms, in either straight chain or branched chain configuration, with from 3 to 12 moles of ethylene oxide per mole are included of alcohol. A further group of nonionic surfactants suitable for use herein, are non-ionic surfactants are polar which include water-soluble amine oxides containing an alkyl portion of about 10 to 18 carbon atoms and two portions selected from the group of alkyl and hydroxyalkyl portions of from about 1 to about 3 carbon atoms; water-soluble phosphine oxides containing an alkyl portion of about 10 to 18 carbon atoms and two portions selected from the group consisting of alkyl groups and hydroxyalkyl groups containing from about 1 to 3 carbon atoms; and water soluble sulfoxides containing an alkyl portion of about 10 to 18 carbon atoms and a portion selected from the group consisting of alkyl and hydroxyalkyl portions of about 1 to 3 carbon atoms. Nonionic surfactants of the formula R1 (OC2 H4) nOH are preferred, in which Ri is a C10-Ci6 alkyl group or a C8-C12 alkylphenyl group, and n is from 3 to about 80. Particularly preferred are the products of condensation of C12-C15 alcohols with from about 5 to about 20 moles of ethylene oxide per mole of alcohol, for example, C12-C13 alcohol condensed with about 6.5 moles of ethylene oxide per mole of alcohol. Additional suitable nonionic surfactants include polyhydroxy fatty acid amides of the formula 0 Ri R--! C - N 1 - Z wherein R is a C9-17 alkyl or alkenyl, Ri is a methyl group and Z is glycityl derived from a reduced sugar, or alkoxylated derivative thereof. Examples are N-methyl-N-1-deoxyglucitylcocoamide and N-1-deoxyglucityl-amide. Methods for making polyhydroxy fatty acid amides are known, and can be found in the U.S. Patent. No. 2,965,576, for Wilson, the U.S. Patent. No. No. 2,703,798, for Schwartz, the descriptions of which are incorporated herein by reference. Ampholytic surfactants include aliphatic derivatives of heterocyclic secondary and tertiary amines in which the aliphatic portion can be straight or branched chain and wherein one of the aliphatic substituents contains from about 8 to 18 carbon atoms, and at least one aliphatic substituent contains an anionic water solubilization group. Zwitterionic surfactants include quaternary ammonium, phosphonium and sulfonium aliphatic derivatives, in which one of the aliphatic substituents contains about 8 to 18 carbon atoms. Cationic surfactants may also be included in the present invention. Cationic surfactants comprise a wide variety of compounds characterized by one or more organic hydrophobic groups in the cation and generally by a quaternary nitrogen associated with an acid radical. The pentavalent nitrogen ring compounds are also consider quaternary nitrogen compounds. Suitable anions are halides, methylsulfate and hydroxide. The tertiary amines may have characteristics similar to cationic surfactants at pH values of the wash solution of less than about 8.5. A more complete description of these and other cationic surfactants useful herein can be found in the U.S. Patent. No. 4,228,044, Cambre, issued October 14, 1980, incorporated herein by reference. Frequently, cationic surfactants are used in detergent compositions to provide fabric softening and / or antistatic benefits. The antistatic agents that provide some softening benefit and which are preferred herein are the quaternary ammonium salts described in the USA No. 3,936,537, Baskerville, Jr., et al., Issued February 3, 1976, the description of which is incorporated herein by reference.

Detergent Enhancer The present method includes the step of introducing a builder into the high speed mixer / densifier for coagglomeration with the surfactant paste. The detergency builder also helps control the mineral hardness, especially Ca and / or Mg in the wash water, or to assist in the removal of particulate soils from the surfaces.

The enhancers can operate through a variety of mechanisms, including the formation of soluble or insoluble complexes with hardness ions, by ion exchange, and offering a more favorable surface for the precipitation of hardness ions than the surfaces of the articles to be cleaned. The level of builder can vary widely depending on the final use and the physical form of the composition. The improved detergents typically comprise at least about 1% builder. Liquid formulations typically comprise about 5% to about 50%, typically 5% to 35%, of builder. Granular formulations typically comprise from about 10% to about 80%, typically 15% to 50%, of detergent builder by weight of the detergent composition. Lower or higher levels of builders are not excluded. For example, certain detergent additives or highly surfactant formulations may be without an improver. Suitable improvers herein can be selected from the group consisting of phosphates and polyphosphates, especially the sodium salts; the silicates include the water soluble and hydrated solid types and include those having chain, layer or ridging structure as well as types of amorphous solid or unstructured liquid; carbonates, dicarbonates, sesquic rbonatos and carbonate minerals, apart from sodium carbonate or sesquicarbonate; aluminosilicates; mono-, di-, tri-, and tet-organic carboxylates especially water-soluble non-surfactant carboxylates in the form of acid, sodium, potassium or alkanolammonium salt, as well as water-soluble low molecular weight polymeric or oligomeric carboxylates, including aliphatic and aromatic types; and phytic acid. These may be supplemented with borates, for example, for pH regulation purposes or with sulfates, especially sodium sulfate and other fillers or vehicles which may be important for designing the stable surfactant and / or the detergent-containing detergent compositions. Mixtures of builder, sometimes referred to as "builder systems", can be used and typically comprise two or more conventional builders, optionally supplemented with chelators, pH buffers or fillers, although the latter materials are generally considered separately when they are described. quantities of materials herein. In terms of relative amounts of surfactant and builder in the detergents present, preferred builder systems are typically formulated at a weight ratio of surfactant to builder from about 60: 1 to about 1:80. Certain preferred laundry detergents have said ratio in the range of 0.90: 1.0 to 4.0: 1.0, preferably 0.95: 1.0 to 3.0: 1.0.

Phosphorus-containing detergency builders, often preferred when permitted by law, include, but are not limited to, the alkali metal, ammonium and alkanolammonium salts of polyphosphates, exemplified by the tripolyphosphates, pyrophosphates, crystalline polymeric metaphosphates; and phosphonates. Suitable silicate builders include alkali metal silicates, particularly liquids and solids that have a Si 2 to 2 ratio. in the scale from 1.6: 1 to 3.2: 1, including particularly for purposes of automatic dishwashing, solid dihydrate silicates marketed by PQ Corp., under the brand name BRITESIL *, e.g., BRITESIL H20; and layered silicates, for example those described in the U.S. Patent. No. 4,664,839, of May 12, 1987, H. P. Rieck. NaSKS-6, abbreviated some. sometimes as "SKS-6", it is an aluminum-free crystalline layered silicate of d-Na2Si? 5 morphology, sold by Hoechst, and is especially preferred in granular laundry compositions. See the preparative methods in German Patent DE-A-3,417,649 and DE-A-3,742,043. Also, other layered silicates such as those having the general formula NaMSix Q2x +? And H2 ?, where M is sodium or hydrogen, x is a number from 1.9 to 4, and "y" can be used in the present or alternatively. number from 0 to 20, preferably 0. The stratified silicates from Hoechst also include NaSKS-5, NaSKS-7 and NaSKS-11, such as stratified silicate forms a, & and r. Other silicates such as magnesium silicate, which serve as a crispening agent in granules, as a stabilizing agent for bleaches, and as a component for foam control systems may also be useful. Also suitable for use herein are synthesized crystalline ion exchange materials or hydrates thereof having chain structure and a composition represented by the following general formula in an anhydrous form: xM2? And Si? 2zM'0, wherein M is Na and / or K, M 'is Ca and / or Mg; y / x is 0.5 to 2.0 and z / x is 0.005 to 1.0, as taught in the U.S. Patent. No. 5,427,711, Sakaguchi et al., June 27, 1995. Suitable carbonate builders include alkali metal and alkaline earth metal carbonates as described in German Patent Application No. 2,321,001, published November 15, 1973, although Sodium dicarbonate, sodium carbonate, sodium sesquicarbonate and other carbonate minerals such as rona or any convenient multiple salt of sodium carbonate and calcium carbonate such as those having the composition 2Na2C? 3CaC? 3 when anhydrous may be useful , and even calcium carbonates including calcite, aragonite and vaterin, especially forms having high surface areas relative to compact calcite, for example as seeds for use in synthetic detergent bars.

The aluminosilicate builders are especially useful in granular detergents, but can also be incorporated in liquids, pastes or gels. Those with the empirical formula are suitable for the present purposes: [M? (AIO2)? (SÍO2) v] * xH2 ?, where z and v are integers of at least 6, the molar ratio of zav is on the scale from 1.0 to 0.5, and x is an integer from 15 to 264. Aluminosilicates can be crystalline or amorphous , of natural origin or synthetically derived. A method of producing aluminosilicate is found in the U.S. Patent. No. 3,985,669, Krummel, et al., Oct. 12, 1976. Preferred synthetic crystalline aluminosilicate ion exchange materials are available as zeolite A, zeolite P (B), zeolite X and, to any extent this differs from zeolite P, the so-called MAP zeolite. Natural types can be used, including clinoptilolite. Zeolite A has the formula: Nai2 [(AIO2) i2 (SIO2) i] xH2 ?, where x is from 20 to 30, especially 27. Dehydrated zeolites (x = 0-10) can also be used. Preferably, the aluminosilicate has a particle size of 0.1 to 10 microns in diameter. Suitable organic builders include polycarboxylate compounds, including dicarboxylates and water-soluble non-surfactant ricarboxylates. The builder polycarboxylates typically have a plurality of carboxylate groups, preferably at least 3 carboxylates. The breeders Carboxylate detergency can be formulated in acid, partially neutral, neutral or very alkaline form. When they are in salt form, alkali metal salts such as sodium, potassium and lithium, or alkanolammonium salts are preferred. Polycarboxylate builders include ester polycarboxylates such as oxydisuccinate, see Berg, U.S. 3,128,287, of April 7, 1964, and Lamberti et al., Patent of E.U.A. No. 3,635,830, of January 18, 1972; detergent builders "TMS / TDS" of the U.S. Patent. No. 4,663,071, Bush et al., May 5, 1987; and other ethercarboxylate including cyclic and alicyclic compounds, such as those described in US Pat.

E.U.A. Nos. 3,923,679; 3,835,163; 4,158,635; 4,120,874 and 4,102,903 - Other suitable detergency builders are the ether hydroxypolycarboxylates, copolymers of maleic anhydride with ethylene or ethyl vinyl ether; 1,2,5-trihydroxybenzene-2,4,6-trisulfonic acid; carboxymethyloxysuccinic acid; the various alkali metal, ammonium and substituted ammonium salts of polyacetic acids such as ethylenediaminetetraacetic acid and nitrilotriacetic acid; as well as mellitic acid, succinic acid, polymaleic acid, benzene-1,3,5-tricarboxylic acid, carboxymethyloxysuccinic acid, and soluble salts thereof. Citrates, for example, citric acid and soluble salts thereof, are important carboxylate builders for example for heavy-duty liquid detergents, due to their availability from renewable resources and their biodegradability. The citrates can also be used in granular compositions, especially in combination with zeolite and / or silicates is ratified. The oxydisuccinates are especially useful in these compositions and combinations. When permitted, and especially in the formulation of bars for manual laundry operations, alkali metal phosphates such as sodium ripolyphosphate, sodium pyrophosphate and sodium orthophosphate can be used. Phosphonate builders such as ethane-1-hydroxy-1, 1-diphosphonate and other known phosphonates can also be used, for example those of U.S. Pat. Nos. 3,159,581; 3,213,030; 3,422,021; 3,400,148 and 3,422,137, and may have convenient properties against scab formation. Certain detersive surfactants or their short chain homologs also have a detergency builder action. For purposes of non-ambiguous consideration of the formula, when they have surfactant capacity, these materials are added as detersive surfactants. The preferred types of detergency builder functionality are illustrated by: 3,3-dicarboxy-4-oxa-l, 6-hexanedioates and the related compounds described in the U.S. Patent. No. 4,566,984, Bush, January 28, 1986. The succinic acid builders include alkyl and C5-C2G alkenyl succinic acids and the salts thereof. Succinate builders also include: lauryl succinate, myristylsuccinate, palmityleuccinate, 2-dodecenylsuccinate (preferred), 2-pentadecenylsuccinate, and the like. Lauryl succinates are described in European Patent Application No. 86200690.5 / 0,200,263, published November 5, 1986. Fatty acids, for example C12-C18 monocarboxylic acids, can also be incorporated into the compositions as surfactants / builders, alone or in combination with the aforementioned improvers, especially citrate and / or succinate improvers, to provide additional detergency builder activity. Other suitable polycarboxylates are described in Patent of E.U.A. No. Crutchfiel et al., March 13, 1979 and in the U.S. Patent. No. 3,308,067, Diehl, March 7, 1967. See also the U.S. Patent. Diehl, 3,723,322. Optionally, inorganic builder materials having the formula (Mx)? Cay (CO3) z, where x and y are integers of 15, and is an integer from 1 to 10, z is an integer from 2 to 25, can be used My are cations, at least one of which is soluble in water, and the equation is satisfied? =? -? S (XÍ multiplied by the valence of Mi) + 2y = 2z, in such a way that the formula has a neutral or "balanced" load. Hydration water or other anions other than carbonate may be added, provided that the total charge is balanced or neutral. The charge or valence effects of these anions must be added to the correct side of the previous equation. Preferably, a water-soluble cation selected from the group consisting of hydrogen, water-soluble metals, hydrogen, boron, ammonium, silicon, and mixtures thereof, preferably sodium, potassium, hydrogen, lithium, ammonium and mixtures thereof, with sodium and potassium being preferred. Non-limiting examples of non-carbonate anions include those selected from the group consisting of chloride, sulfate, fluoride, oxygen, hydroxide, silicon dioxide, chromate, nitrate, borate and mixtures thereof. Preferred builders of this type in their simplest forms are selected from the group consisting of Na2Ca (C03 2, 2C (C03) 2, Na2Ca (C03) 3, NaKCa (C03) 2, NaKCa2Ca (C03) 3, K2Ca2 (C03) 3, and combinations thereof An especially preferred builder material described herein is Na2Ca (C0s) 2, in any of its crystalline modifications Suitable builders of the type defined above are exemplified by , and include, the natural or synthetic forms of any of the following minerals or combinations of them: Afghanite, Andersonite, Ashcroftine Y, Beyerite, Borcarite, Burbankite, Butschliite, Cancrinite, Carboneernaite, Carletonite, Davyne, Donnayta Y, Fai rchildita, Ferrisurita , Franzinita, Gaudefroyita, Gaylussita, Girvasita, Gregoryita, Jouravskita, Kamphaugita Y, Kettnerita, Khanneshita, Lepersonnita Gd, Liottita, Mckelveyita Y, Microsommita, Mroseita, Natrofairchildita, Nyerereita, Remondita Ce, Sacrofanita, Schrockingerita, Shortita, Surita, Tunisita, Tuscanita, Tyrolita, Vishnevita, and Ze korita. Preferred mineral forms include Nyererite, Fairchildite and Shortite.

Optional detergent components The detergent components starting or being introduced into the present treatment may also include any number of additional ingredients. These include other detergency builders, bleaches, bleach activators, foam enhancers or foam suppressors, anti-galling and corrosion agents, soil suspending agents, soil removal agents, germicides, pH adjusting agents, alkalinity sources, non-soil improvers. detergency, chelating agents, smectite clays, enzymes, enzyme stabilizing agents and perfumes. See the patent of E.U.A. No. 3,936,537, issued February 3, 1976 to Baskerville, Jr., et al., Incorporated herein by reference. Bleaches and activators are described in the U.S.A. No. 4,412,934, Chung et al., Issued November 1, 1983, and in the U.S. patent. No. 4,483,781, Hartman, issued November 20, 1984, both of which are incorporated herein by reference. I also know describe chelating agents in the U.S. patent. No. 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 and are described in the U.S. Patents. No. 3,933,672, issued January 20, 1976 to Bartoletta et al., And No. 4,136,045, issued January 23, 1979 to Gault and others, both incorporated herein by reference. Smectite clays suitable for use herein are described in the U.S.A. No. 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 the Baskerville patent, in column 13, line 54 to column 16, line 16, and in the US patent. No. 4,663,071, Bush et al., Issued May 5, 1987, both incorporated herein by reference. In order to make the present invention more easily understandable, reference is made to the following examples which are intended to be illustrative only and not limiting in scope.

EXAMPLE This example illustrates the procedure of the invention described and claimed in the present. The percentages are in base to the weight in the mixtures, before any subsequent drying step, unless otherwise specified. The terms "LAS" and "AS" as used herein mean, respectively, "linear sodium alkylbenzene sulfonate" and "sodium alkyl sulphate". Various surfactant pastes consisting of AS C14-15 and LAS C12.3 are made by sulfating C14-15 alcohol with SO3 and co-neutralizing with HLAS C12.3 using 50% caustic soda (sodium hydroxide). The specific compositions of the surfactant pastes are indicated in Table 1.

TABLE I Components A B C D E Alkylsulfate 55-0 55.0 44-0 64.5 55.0 C14-15 Alkylbenzenesulfonate 18.3 18.3 29.3 8.8 Linear 18.3 C12.3 Polyethylene glycol 4000 3. 7 3. 7 3. 7 3. 7 0.0 Sodium hydroxide 0.75 0. 5 0.75 0.75 0.75 Water .9.5 19.5 19.5 19 - 5 23.2 Minors (sulfate without 2.75 3.0 2.75 2. 75 2.75 react, etc.) Total 100 100 100 100 100 A downstream film SO3 reactor is used to prepare the acid form of C14-15 alkyl sulfate and linear C12.3 alkyl benzene sulfonate. The acid is fed to a highly active neutralization system consisting of a recirculation circuit containing a heat exchanger for cooling, a recirculation pump suitable for highly viscous fluids, and a high shear mixer to which the reagents are introduced. The surfactant paste that leaves the highly active neutralization system is transported and stored in 316 1 stainless steel storage vessels lined with temperature controlled at 75 ° C. The surfactant paste remains stable and maintains a pH above 10 for at least five days (120 hours). The temperature of the pulp is maintained between 65 ° C and about 70 ° C by the circulation of glycol solution through the jacket of the container. Two feed streams of various detergent starting ingredients are fed continuously, at a speed of 2800 kg / hr, into a L? Dige CB-30 mixer / densifier, one of which comprises the surfactant paste and the other stream contains the improver of detergency that is aluminosilicate. The surfactant paste, the aluminosilicate and optionally associated sodium carbonate improver, agglomerate to form detergent agglomerates. The detergent agglomerates of the Lódige mixer / densifier CB-30 are continuously fed to a mixer / densifier Lódige KM-600 for subsequent agglomeration. The resulting detergent agglomerates are then fed to optional conditioning apparatuses including a bed dryer 4- »fluid and a fluid bed cooler. The detergent agglomerates emerging from the fluid bed cooler are screened, after which they are mixed with the same auxiliary detergent ingredients to result in a fully formulated detergent product having a uniform particle size distribution. The composition of the detergent agglomerates that come out of the fluid bed cooler is indicated in Table II below: TABLE II Components% by weight C14-15 alkyl sulfate and 30.0 linear C12.3 alkylbenzenesulfonate Aluminosilicate 36.0 Sodium carbonate 21.0 Miscellaneous (water, perfume, etc.) 13.0 Total 100.0 Having thus described the invention in detail, it will be clear to the person skilled in the art that various changes can be made without departing from the scope of the invention, and this is not limited to what is described in the specification.

Claims (10)

V NOVELTY OF THE INVENTION CLAIMS

1. - A process for preparing detergent agglomerates, characterized by the steps of: (a) providing a non-linear viscoelastic surfactant paste including, by weight of said surfactant paste, from 70% to 95% of a detersive surfactant, from 5% to 30% % water, and an excess amount of an alkali metal hydroxide so that the pH of said surfactant paste is at least 10; (b) regulate the temperature of said surfactant paste within a range of 50 ° C to 80 ° C, so that said surfactant paste is treatable and stable for at least 48 hours; (c) loading said surfactant paste into a high speed mixer / densifier, (d) introducing from 1% to 70% by weight of a builder into said high speed mixer / densifier; and (e) agglomerating said tenactive paste and said improver, treating said surfactant paste and said improver initially in said high speed mixer / densifier, and subsequently in a moderate speed mixer / densifier, to form said detergent agglomerates.

2. The process according to claim 1, characterized in that said surfactant paste is substantially free of materials that produce a gae when they react with an acid.

3. The process according to claims 1 and 2, characterized in that said alkali metal hydroxide in said surfactant paste is sodium hydroxide.

4. The process according to claims 1 and 3, characterized in that said detersive surfactant is a mixture of alkyl sulfate surfactants and linear alkylbenzenesulfonate in a weight ratio of 1: 1 to 5: 1.

5. The process according to claims 1 and 4, further characterized by the step of drying said detergent agglomerates.

6. The process according to claims 1 and 5, characterized in that said detergency builder is aluminosilicate.

7. The method according to claims 1 and 6, characterized in that said step of regulation makes said surfactant paste stable for at least 72 hours.

8. The method according to claims 1-7, characterized in that said step of regulation includes the step of maintaining said surfactant paste stable for at least 170 hours.

9. The method according to claims 1-8, characterized in that said step of The V regulation includes the step of maintaining said surfactant paste within a temperature of 60 ° C to 75 ° C.

10. The method according to claims 1-9, further characterized in that it comprises the step of maintaining said surfactant paste substantially free of contaminating materials having a pH of less than 7.