WO1997042300A1

WO1997042300A1 - Process for making agglomerated detergent compositions having improved flowability

Info

Publication number: WO1997042300A1
Application number: PCT/US1996/006472
Authority: WO
Inventors: Fukuji Ebihara; Takashi Kazuta
Original assignee: The Procter & Gamble Company
Priority date: 1996-05-07
Filing date: 1996-05-07
Publication date: 1997-11-13
Also published as: CA2252881A1; JPH11509263A; CZ356398A3; EP0912716A1

Abstract

Zeolite X is used in the process for manufacture of detergent agglomerates to improve flowability of the finished product.

Description

PROCESS FOR MAKING AGGLOMERATED DETERGENT COMPOSITIONS HAVING IMPROVED FLOWABILITY

TECHNICAL FIELD The invention relates to the manufacture of high density, free flowing agglomerated detergent granules, using a liquid binding agent and zeolite X as a flow aid.

BACKGROUND OF THE INVENTION Recently there has been considerable interest within the detergent industry in the production of detergent granules having relatively high bulk density, e.g. 600 g/liter and above. Typically, detergent granules, which comprise organic surfactant and inorganic or organic builders are prepared by spray drying an aqueous slurry of the components. The granules thus obtained typically have a density of from about 300 to about 500 g/liter. To meet the requirement for higher density detergent products various processes have been developed for providing such products. U.S. Pat 5,133,924, Appel et al, issued July 28 1992 discloses a process wherein a spray-dried detergent composition or a mixture of particulate components of a detergent composition is subjected to a two-stage mixing process in order to reduce the porosity of the particles, thereby increasing density. Liquids, such as water or nonionic surfactants are optionally added to the second stage mixer. U.S. Pat. No. 5,164,108, Appel et al., issued November 17, 1992, discloses a process for making high density detergent powder wherein a liquid acid precursor of an anionic surfactant, a solid, water-soluble alkaline builder and optionally other detergent materials are fed to a high speed mixer/densifier in which the liquid acid precursor is neutralized, thereby producing a powder and then mixing the powder in a moderate speed mixer to reduce the porosity of the powder particles, the patent states that complications can arise with respect to particle size distribution in cases where high active (i.e., 20% or more surfactant) compositions are processed. It is disclosed that these problems can be obviated by adding a powdered material such as Zeolite A to the second mixer. Jap. Pat. Application 61-69897, published April 10, 1986 discloses a process for producing a dense agglomerated detergent product from spray dried detergent granules comprising a surfactant and builder, wherein the granules are pulverized by vigorous stirring in a blade mixer, followed by mixing with a binder (e.g., nonionic surfactant) and a "surface improving agent", which can be an aluminosilicate.

U.S. Pat. No. 4,652,391 (Balk), issued March 24, 1987, discloses spray dried detergent granules in which the surfactant is a nonionic. The patent indicates that the granules coming from the spray tower should be cooled rapidly to prevent nonionic from diffusing to the surface of the granules. Such diffusion of nonionic reduces the fluidity and density of the granular product. It is stated that if warm weather prevents rapid cooling, the granules can be "dusted" with a "fluidizing agent" (also referred to as an "anti caking agent"). Synthetic Zeolites (Zeolite A and Zeolite X) are disclosed for this purpose.

BACKGROUND ART See U.S. Pats. 5,133,924, 5, 164, 108, 4,656,391 and Japanese Pat. Appln. 61- 69897, discussed supra, and Perry's Chemical Engineers' Handbook 6th Edition (1984) at Page 16-9.

SUMMARY OF THE INVENTION The present invention is directed to a process of forming agglomerated detergent compositions comprising the steps of;

(a) forming a homogeneous mixture of a granular detergent composition and a liquid binder material, wherein the granular detergent composition comprises a detersive surfactant, and the amount of said liquid binder material is from about 1% to about 6% by weight of said granular detergent composition, and

(b) contacting the mixture formed in Step (a) with Zeolite X, wherein the amount of Zeolite X is at least equal to, and preferably from 1 to about 2.5 times, the weight amount of liquid binder in Step (a).

The present invention also encompasses the composition of the above process.

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to the preparation of agglomerated detergent granules wherein granular detergent material is mixed with a limited amount of a liquid binder material, thereby resulting in agglomerates having an increased particle size compared to the original detergent granules.. Experience has shown that agglomerates formed in this manner often tend to be sticky, and therefore have poor free-flow properties. In accordance with the present invention it has been found that for detergent agglomerates which utilize liquid binders, Zeolite X is a particularly effective free-flow aid when applied as a surface coating to said agglomerates. Although Zeolite A is also effective as a free-flow aid and has generally been preferred over Zeolite X for most detergent uses because of its better sequestering power, it has now been found that Zeolite X is a more effective free-flow aid than Zeolite A for detergent agglomerates utilizing liquid binders. Additionally it has been found that the use of Zeolite X as free-flow aid in said agglomerates results in a higher density product than obtained when using Zeolite A. Typically, the products produced by the process herein have a bulk density of greater than 600 grams/liter. Granular Detergent Compositions

The granular detergent composition in Step (a) of the process of the present invention comprises a detersive surfactant. The surfactant and any other components of the granular compositions can be introduced into Step (a) as separate ingredients or as a pre-formed composition, such as a spray dried detergent composition or as a mixture of one or more separate granular ingredients and a spray dried detergent composition. Anionic surfactants are the preferred surfactants for use herein and are well known in the art. The following are representative examples of such surfactants.

Anionic surfactants suitable for use herein include the water-soluble salts, preferably the alkali metal, ammonium and alkylolammonium 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. (Included in the term "alkyl" is the alkyl portion of acyl groups.) Examples of this group of synthetic surfactants are the sodium and potassium alkyl sulfates, especially those obtained by sulfating the higher (Cβ.jg carbon atoms) primary or secondary alcohols such as those produced by reducing the glycerides of tallow or coconut oil or by the oxo process; and the sodium and potassium alkylbenzene sulfonates in which the alkyl group contains from about 9 to about 15 carbon atoms, in straight chain or branched chain configuration, e.g., those of the type described in U.S. Patents 2,220,099 and 2,477,383, incorporated herein by reference. Especially valuable are linear straight chain alkylbenzene sulfonates in which the average number of carbon atoms in the alkyl group is from about 1 1 to 13. Other anionic surfactants suitable for use herein are the sodium alkyl glyceryl ether sulfonates, especially those ethers of higher alcohols derived from tallow and coconut oil; sodium coconut oil fatty acid monoglyceride sulfonates and sulfates; sodium or potassium salts of sulfuric acid esters of the reaction product of one mole of a fatty alcohol (e.g. coconut or tallow alcohol) with 1 to 6 moles of ethylene oxide; sodium or potassium salts of alkyl phenol ethylene oxide ether sulfates having about 1 to 10 units of ethylene oxide per molecule and in which the alkyl radicals contain about 8 to 12 carbon atoms. In addition, suitable anionic surfactants include the water-soluble salts of esters of alpha-sulfonated fatty acids 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 from about 2 to 9 carbon atoms in the acyl group and from 9 to about 23 carbon atoms in the alkane moiety; water-soluble salts of olefin and paraffin sulfonates 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 moiety.

Preferred anionic surfactants are the alkali metal salts of C JO-18 »ⁿear alkylbenzene sulfonate and C i o- 18 ^a M sulfate. A preferred embodiment of the present invention is wherein the anionic surfactant comprises from about 20% to about 40% of a mixture of sodium C IQ- B linear alkylbenzene sulfonate and sodium C12-I6 alkyl sulfate in a weight ratio of about 2: 1 to 1 :2.

Water-soluble salts of the higher fatty acids, i.e., "soaps", are also useful anionic surfactants in the compositions herein. This includes alkali metal soaps such as the sodium, potassium, ammonium, and alkylolammonium salts of higher fatty acids containing from about 8 to about 24 carbon atoms, and preferably from about 12 to about 18 carbon atoms. Soaps can be made by direct saponification of fats and oils or by the neutralization of free fatty acids. Particularly useful are the sodium and potassium salts of the mixtures of fatty acids derived from coconut oil and tallow, i.e., sodium or potassium tallow and coconut soap.

Other types of surfactants suitable for use in the granular detergent compositions of step (a) includes nonionic, cationic ampholytic, and zwitterionic types.

Typical nonionic surfactants include the alkylene oxide condensates of hydrocarbyl groups (e.g. alkyl or alkyl phenyl) wherein the hydrocarbyl groups contain from about 8 to about 22 carbon atoms. Nonionics also include semi polar compounds such as C8-C22 amine oxides. An extensive discussion of nonionic surfactants is found in U.S. Pat. 5,338,491 Conner, et al issued August 16, 1994. Nonionics also include fatty acid amide surfactants of the formula O Rj

II I

R₂ - C - N - Z wherein: K\ is H, Cj-Cg hydrocarbyl, 2-hydroxyethyl, 2-hydroxypropyl, or a mixture thereof, preferably C1-C4 alkyl, more preferably C\ or C₂ alkyl, most preferably C\ alkyl (i.e., methyl); and R^ is a C5-C32 hydrocarbyl moiety, preferably straight chain C7-C19 alkyl or alkenyl, more preferably straight chain C9-C17 alkyl or alkenyl, most preferably straight chain C1 1-C19 alkyl or alkenyl, or mixture thereof; and Z is a polyhydroxyhydrocarbyl moiety having a linear hydrocarbyl chain with at least 2 (in the case of glyceraldehyde) or at least 3 hydroxyls (in the case of other reducing sugars) directly connected to the chain, or an alkoxylated derivative (preferably ethoxylated or propoxylated) thereof. Z preferably will be derived from a reducing sugar in a reductive amination reaction; more preferably Z is a glycityl moiety. Suitable reducing sugars include glucose, fructose, maltose, lactose, galactose, mannose, and xylose, as well as glyceraldehyde. As raw materials, high dextrose corn syrup, high fructose corn syrup, and high maltose corn syrup can be utilized as well as the individual sugars listed above. These corn syrups may yield a mix of sugar components for Z. It should be understood that it is by no means intended to exclude other suitable raw materials. Z preferably will be selected from the group consisting of -CH₂-(CHOH)_n-CH₂-OH, -CH(-CH₂-OH)-(CHOH)_n.₁-CH₂-OH, - CH₂- (CHOH)₂(CHOR*)(CHOH)-CH₂-OH, where n is an integer from 1 to 5, inclusive, and R' is H or a cyclic mono- or poly- saccharide, and alkoxylated derivatives thereof. Most preferred are glycityls wherein n is 4, particularly -CH2-(CHOH)4-CH₂-OH.

In the above formulas, R\ can be, for example, methyl, ethyl, propyl, isopropyl, butyl, isobutyl, 2-hydroxy ethyl, or 2-hydroxy propyl. For highest sudsing, Rj is preferably methyl or hydroxyalkyl. If low sudsing is desired, R\ is preferably C₂-Cg alkyl, especially n-propyl, iso-propyl, n-propyl, iso-propyl, n-butyl, iso-butyl, pentyl, hexyl and 2-ethyl hexyl.

Specific examples of this type of amide surfactant include Cι₂-N-(3- methyxypropyl) glucamide and coconut n-methyl glucamide. Further disclosure of this type of amide surfactant can be found in U.S. Pat. 5,376,310, Cripe, issued December 27, 1994. Cationic detersive surfactants include the ammonium surfactants such as alkyldimethylammonium halogenides, and those surfactants having the formula:

[R2(OR³)_y[R⁴(OR³)_y]2R⁵N⁺X ^~ wherein R^ is an alkyl or alkyl benzyl group having from about 8 to about 18 carbon atoms in the alkyl chain, each R³ is selected from the group consisting of -CH₂CH₂-, -CH₂CH(CH₃)-, -CH₂CH(CH₂OH)-, -CH₂CH₂CH₂-, and mixtures thereof; each R4 is selected from the group consisting of C1-C4 alkyl, C1-C4 hydroxyaJkyl, benzyl, ring structures formed by joining the two R4 groups, CH2CHOHCHOHCOR6CHOHCH2OH wherein R6 is any hexose or hexose polymer having a molecular weight less than about 1000, and hydrogen when y is not 0; R5 is the same as R4 or is an alkyl chain wherein the total number of carbon atoms of R2 plus R5 is not more than about 18; each y is from 0 to about 10 and the sume of the y values is from 0 to about 15; and X is any compatible anion. Other cationic surfactants useful herein are also described in U.S Pat No 4,228,044, Cambre, issued Oct 14, 1980 Ampholytic surfactants can be broadly described as aliphatic derivatives of secondary or tertiary amines, or aliphatic derivatives of heterocyclic secondary and tertiary amines in which the aliphatic radical can be straight chain or branched. One of the aliphatic substituents contains at least about 8 carbon atoms, typically from about 8 to about 18 carbon atoms, and at least one contains an anionic water-solubilizing group, e g , carboxy, sulfonate, sulfate See U.S Pat. No. 3,929,678 to Laughlin et al , issued December 30, 1975 at column 19, lines 18-35 for examples of ampholytic surfactants Zwitterionic surfactants can be broadly described as derivatives of secondary and tertiary amines, derivatives of heterocyclic secondary and tertiary amines, or derivatives of quaternary ammonium, quaternary phosphonium or tertiary sulfonium compounds. See U.S. Pat No 3,929,678 to Laughlin et al., issued December 30, 1975 at column 19, line 38 through column 22, line 48 for examples of zwitterionic surfactants A further extensive disclosure of various types of surfactants can be found in

US Pat. 3,664,961, Norris, issued May 23, 1972.

Surfactant will generally comprise from about 20% to about 95%, preferably from about 30% to about 60%, of the granular detergent composition of Step (a) prepared by the process herein. Typically detergent compositions made by the present process will contain builders. Builders useful in the present invention are generally selected from the various water-soluble, alkali metal, ammonium or substituted ammonium phosphates, polyphosphates, phosphonates, polyphosphonates, carbonates, borates, polyhydroxy sulfonates, polyacetates, carboxylates, and polycarboxylates Preferred are the alkali metal, especially sodium, salts of the above Preferred for use herein are the phosphates, carbonates, silicates, polycarboxylates, and mixtures thereof. More preferred are sodium tripolyphosphate, tetrasodium pyrophosphate, sodium citrate, sodium tartrate sodium mono- and di-succinates, and mixtures thereof. .

Specific examples of inorganic phosphate builders are sodium and potassium tripolyphosphate, pyrophosphate, polymeric metaphosphate having a degree of polymerization of from about 6 to 21, and orthophosphates Other phosphorus builder compounds are disclosed in U.S. Patents 3,159,581; 3,213,030, 3,422,137, 3,400,176 and 3,400,148, all of which are incorporated herein by reference.

Examples of nonphosphorus, inorganic builders are sodium and potassium carbonate, bicarbonate, sesquicarbonate, tetraborate decahydrate, and Zeolites such as Zeolite A. Water-soluble, nonphosphorus organic builders useful herein include the various alkali metal, ammonium and substituted ammonium polyacetates, carboxylates, polycarboxylates and polyhydroxy sulfonates. Examples of polyacetate and polycarboxylate builders are the sodium, potassium, lithium, ammonium and substituted ammonium salts of ethylene diamine tetraacetic acid, nitrilotriacetic acid, oxydisuccinic acid, mellitic acid, benzene polycarboxylic acids, and citric acid. Polymeric polycarboxylate builders are set forth in U.S. Patent 3,308,067,

Diehl, issued March 7, 1967. Such materials include the water-soluble salts of homo- and copolymers of aliphatic carboxylic acids such as maleic acid, itaconic acid, mesεconic acid, fumaric acid, aconitic acid, citraconic acid and methylenemalonic acid.

Other suitable polycarboxylates for use herein are the polyacetal carboxylates described in U.S. Patent 4,144,226, issued March 13, 1979 to Crutchfield et al., and U.S. Patent 4,246,495, issued March 27, 1979 to Crutchfield et al.

Builders generally comprise from about 5% to about 50%, preferably from about 20% to about 40% of compositions prepared by the process herein. Builders can be included in the granular detergent composition of Step (a) or they can be added to the agglomerates after they have been mixed with the Zeolite X.

Filler materials such as sodium sulfate or sodium chloride are typically present in the detergent compositions of Step (a) at levels up to about 40%.

Binder A wide variety of liquids can be used as the binder for the granular detergent components in Step (a) of the process of the invention.

Water is a suitable binder. Likewise aqueous solutions containing up to about 65%, preferably up to about 55%, more preferably up to about 35% of inorganic or organic materials such as sodium silicate (2.0 ratio Na₂O:SiO₂) or polyacrylate polymer can be used. Generally solute levels above about 65% result in aqueous dispersions or solutions which are too viscous to be conviently worked into a homogeneous mixture with the granular detergent of Step (a) of the process herein. Also, the preferred way of introducing the liquid binder into the process is by spraying it onto the granular detergent. Highly viscous solutions are difficult to spray. Nonionic organic liquids (melting point below about 7 degrees C) are preferred binders for use in the process of the invention. Preferred materials are the nonionic surfactants since they will contribute to the cleaning performance of the compositions. See the discussion of nonionic surfactants supra. The most common types of these materials are alkoxylated long chain organic compounds. Alkoxylated nonionic materials suitable for use as binders herein include condensation products of Cj2-18 f^attv alcohols with an average of 3 to 20, preferably 4 to 16, alkoxy moieties. The alcohol radicals may be saturated or monounsaturated, linear or methyl-branched in the 2-position (oxo radical), and may be derived from naturally occurring or hydrogenated fatty residues and/or synthetic residues. Ethoxylates derived from cetyl, stearyl and oleyl alcohol and mixtures thereof are particularly suitable. Examples are tallow fatty alcohols containing on average from 4 to 8 ethylene oxide (EO) moieties, tallow fatty alcohol containing on average from 10 to 18 EO and oleyl alcohol containing on average from 6 to 12 EO and also mixtures thereof.

Other nonionic materials are alkoxylated C i2-24_> preferably Ci4_ιg alcohols in the production of which 1 to 3 mols of propylene oxide and then 4 to 20, preferably 4 to 7, mols of ethylene oxide are added onto the alcohol. Ethoxylated Cg_ι₂- alkyl- phenols containing 4 to 14 EO are also suitable.

Nonionic organic liquids which are not surfactants can also be used as binders herein. Examples of such materials are polyethylene glycols and polypropylene glycols. Binders are used in an amount of from about 1% to about 6%, preferably from about 2.5% to about 6%, most preferably from about 3% to about 4.5%, based on the total weight of detergent components in Step (a) of the process.

Zeolite X In Step (b) of the process herein the agglomerated particles which have been formed from the essential detergent components and binder in Step (a) are contacted and intimately mixed with Zeolite X in an amount which is at least equal to the amount of liquid binder used in Step (a) of the process. Preferably the amount of Zeolite X is from 1 to 2.5 times the weight amount of liquid binder used in Step (a). Zeolite X is a synthetic aluminosilicate, readily available commercially from, for example, Union Carbide Company and Philadelphia Quartz Company. The sodium salt form ( Zeolite 13X) has a pore size of about 8 Angstroms and the calcium form (Zeolite 10X) a pore size of about 7 Angstroms. For use herein, the sodium form is preferred. The Zeolite X should be in powdered form having particle size of less than about 20 millimicrons, Preferred particle sizes are in the range of from about 5 to about 10 millimicrons.

It has been found that further improvement in the free flow properties and increased density of compositions made by the process herein can be achieved if hydrophobic precipitated silica is included along with Zeolite X in Step (b) of the process. Hydrophobic precipitated silicas suitable for use herein are commercially available, for example Supernat D 10 and D 17 from Degussa AG, Frankfurt/Main, Germany.

When used in Step (b) of the process , the amount of hydrophobic precipated silica is from about 0.1% to about 1%, preferably from about 0.2% to about 0.4%, based on the weight of the mixture in Step (a).

Optional Materials

Optionally, other materials useful in detergent compositions can be included as detergent components in Step (a) of the process herein. Alternatively, such materials can be added to the agglomerates after they have been mixed with Zeolite X, or Zeolite X and precipitated silica. Optional materials include additional types of surfactants such as ampholytics , zwitterionics and cationics. Examples of such surfactants are disclosed in U.S. Patents 3,664,961, Norris, issued May 23, 1972, and 4,228,044, Cambre, issued October 14, 1980, incorporated by reference herein. Other optional ingredients include bleaches, brighteners, bleach activators, suds boosters, suds suppressors, anti-tarnish and anti-corrosion agents, soil suspending agents, dye transfer inhibition agents, soil release agents, dye transfer inhibiting agents, germicides, pH adjusting agents, chelating agents, clays and enzymes.

Processing

A particulate composition comprising surfactant is used in Step (a) of the process. This composition can consist of granules from a spray drying tower or one or more particulate materials which have not been spray dried. Alternatively, the composition can be a mixture of spray dried granules and other particulate detergent components such as additional surfactant and/or builder, bleach, etc..

Prior to mixing with binder, the particulate composition can be densified. For example it can subjected to mixing in a high speed mixer such as a Loedige CB, Shugi Granulator, or Drais K-TTP, followed by mixing in a moderate speed mixer such as the Loedige KM or Drais K-T. See for example; U.S. Pats. 5,133,924 and 5, 164,108. The mixing of densified detergent particles and binder and the contacting of said mixture with Zeolite X (or Zeolite X plus precipitated silica) is accomplished in the moderate speed mixer.

In a preferred way of carrying out the process to produce free flowing, densified agglomerates, a spray dried granular product comprising anionic surfactant and, optionally, additional dry particulate detergent components is subjected to compaction to remove air, for example by passing the particulate composition through a compactor such as the BCS25 type compactor from Shinto Industrial Company, thereby forming chips. These chips then can be ground (e.g. in a Fitz Mill ), and screened to produce the desired particle size. The densified particles are then mixed with nonionic binder and contacted with Zeolite X (or Zeolite X plus precipitated silica). Preferably, the liquid binder is added to the granular detergent composition by spraying it onto the detergent composition during the mixing, but prior to adding Zeolite X. The mixing of particulate detergent (whether densified or not) with binder, and the contact with Zeolite X can be accomplished in any suitable mixer. Examples of suitable mixers are the Fukae Vertical High Speed Mixer from Fukae Industrial Company, Hogyo prefecture, Kobe Japan, and the Ribbon Mixer from Powerex Company, Osaka prefecture, Osaka Japan

All percentages and ratios described herein are by weight unless otherwise stated. All documents mentioned herein are incorporated by reference.

The invention will be illustrated by the following example, which is not to be construed in any manner as a limitation of the invention.

EXAMPLE I

A spray dried surfactant granule having of 290 grams/liter is densified as described t

Fatty Alcohol Sulfate 9.0%

Linear Alkylbenzene 30.0

Sulfonate

Sodium Carbonate 21

Sodium Silicate 16

Sodium Sulfate 8

Polyethylene Glycol 0.3

Brighteners 0.4

Moisture 4

Other conventional ingredients 11.3

TOTAL 100%

The spray dried detergent granule is continuously loaded onto the top of a roll- type compactor unit via a force feeder that is located at the top of the compactor rolls, to produce chips. Pilot compactor unit operation condition is: the rotation rate of rolls is 3.60 φm, ammeter of roll is 5.5 A, roll pressure is 1.7 ~2.1 tons and rotation rate of force feeder is -16.8 φm, ammeter of force feeder is 3.0A. Compaction rate is -56 kgs/hr as chips. Chip density that comes out rolls, is 1.3-1.6 g/cc. The surfactant level in the chips remains at 39%.

The surfactant chips are constantly fed into a pilot grinder (Fitz mill). Pilot grinder operation condition is: the rotation rate of shaft is ~4726φm, ammeter of shaft is 6.0-7.2 A and 2.0 mm punch out size of screen is used. % on 850 m of the ground chips is 4.0-10.0%. % under 150 m is 19-22%. The bulk density of the ground chips is -660 g/L as ground. The surfactant level in this ground granule remains-39%.

9.85 kgs of the densified ground granules and 1.58 kgs of sodium C_jg secondary alkyl sulfate (95% sodium alkyl sulfate, 2% sodium sulfate, 3% moisture and misc.) powder are loaded into a pilot Lόdige KM mixer (50 liter capacity). Fill level is 37% in accordance with the assumed the bulk density of finished product of 700 g/L. The blade speed is set at 35 φm while keeping chopper speed at 3000 φm. The ground surfactant granule and alkyl sulfate powder are well mixed in the Lόdige mixer during 70 sec. 30 g of polypyrrolidone (dye transfer inhibition agent) is then sprayed into Lόdige mixer during 25-30 sec. 440 g of C14-C15 EO9 alkyl ethoxylate nonionic which has been heated to 70°C is then sprayed onto the material in the Lόdige mixer.during a time period of 50 to 60 seconds. Then 810g of Zeolite 13X, 50 g of hydrophobic precipitated silica and 100 g of soil release polymers are added/mixed into Lόdige mixer during 200 sec. Then, 40 g of perfume is sprayed into mixer during 30-40 sec. The surfactant level of the resulting product is -45%. The product is sieved through an 1 180 m screen. The sieved product has a total surfactant level of- 45%. The product is a free flowing granule having a bulk density of 781 g/L.

Claims

WHAT IS CLAIMED IS:

1. A process of forming agglomerated detergent compositions comprising the steps of;

(a) forming a mixture of a granular detergent composition and a liquid binder material wherein the granular detergent composition comprises a detersive surfactant, and the amount of said liquid binder is from about 1% to about 6% by weight of said granular detergent composition, and

(b) forming a mixture of the composition produced in Step (a) with Zeolite X, wherein the amount of Zeolite X is at least equal to the weight amount of liquid binder in the composition produced in Step (a).

2. The process of Claim 1 wherein the amount of Zeolite X is from about 1 to about 2.5 times the weight amount of liquid binder in the composition produced in Step (a).

3. The process of claim 2 wherein the binder is an organic liquid.

4. The process of claim 2 wherein the binder is an alkoxylated C12 to Cig alcohol having an average of 3 to 16 alkoxy groups.

5. The process of Claim 2 wherein hydrophobic precipitated silica is included in the mixture formed in Step (b) in an amount which is from about 0.1% to about 1% of said mixture.

6. The process of Claim 2 wherein the granular detergent of Step (a) is a spray dried granule which has been subjected to compaction to remove entrapped air prior to use in Step (a).

7. The process of any one of Claims 1 through 6 wherein the granulated detergent composition of Step (a) comprises from about 20% to about 95% detersive surfactant and from about 5% to about 50% detergency builder.

8. The process of Claim 7 wherein the detersive surfactant is an anionic synthetic surfactant.

9. The process of Claim 8 wherein the detergency builder is selected from the group consisting of phosphates, polyphosphates, phosphonates, polyphosphonates carbonates, borates, polyhydroxy sulfonates, polyacetates, carboxylates, and polycarboxylates.

10. An agglomerated detergent composition prepared by the process of;

11. The product of Claim 10 wherein the amount of Zeolite X is from about 1 to about 2.5 times the weight amount of liquid binder in the composition produced inStep (a).

12. The product of Claim 1 1 wherein hydrophobic precipitated silica is included in the mixture formed in Step (b) in an amount which is from about 0.1% to about 1% of said mixture.

13. The product of Claim 1 1 wherein the binder is an organic liquid.

14. The product of claim 11 wherein the binder is an alkoxylated Cι₂ to Cig alcohol having an average of from 3 to 16 alkoxy groups.

15. The product of any one of Claims 10 through 13 wherein the granular detergent composition of Step (a) comprises from about 20% to about 95% detersive surfactant and from about 5% to about 50% detergency builder.

16. The product of Claim 15 wherein the detersive surfactant is an anionic synthetic surfactant.

17. The product of Claim 16 wherein the detergency builder is selected from the group consisting of phosphates, polyphosphates, phosphonates, polyphosphonates carbonates, borates, polyhydroxy sulfonates, polyacetates, carboxylates, and polycarboxylates.