MXPA97009168A - Procedure for manufacturing detergent highly active and high densi granules - Google Patents

Abstract

The present invention includes a continuous process for producing highly active and high density detergent granules, consisting essentially of the following steps: preparing a mixture in a high speed mixer, the mixture being prepared from components fed into the mixer consisting of essentially from the following: from about 15% to about 35% of an anionic surfactant acid selected from alkylbenzenesulfonic acid and alkylsulfuric acid and mixtures thereof, from about 5% to about 65% of a phosphate builder selected from of polyphosphates and pyrophosphates and mixtures thereof, and from about 10% to about 65% of particulate carbonate selected from sodium carbon and potassium carbon and mixtures thereof, the amount of carbonate being at least 2 times the amount theoretically necessary to neutralize agent-based antacid anionic surfactant, agglomerating the first pass mixture in a moderate speed mixer, whereby the anionic surfactant acid selected from alkylbenzenesulfonic acid and alkylsulfuric acid and mixtures thereof, from about 5% to about 65% of a detergent improver of phosphate selected from polyphosphates and pyrophosphates and mixtures thereof, and from about 10% to about 65% particulate carbonate selected from sodium carbon and potassium carbon and mixtures of the mimes, the amount of carbonate being At least 2 times the amount theoretically necessary to neutralize the anionic surfactant agent, agglomerate the mixture from the first step in a moderate speed mixer, whereby the anionic surfactant acid is neutralized by the carbonate, and the resulting detergent granules have a global density of more than about 550% g / l and a content of ag ua of less than approximately

Description

PRQCEDIRING TO MANUFACTURE HIGHLY ACTIVE AND HIGH DENSITY DETERGENT GR.

TECHNICAL FIELD The present invention includes a process for making highly active and high density phosphate-containing detergent granules, which are then typically combined with other ingredients to form a detergent product.

BACKGROUND OF THE INVENTION The granules of detergents containing an anionic surfactant are typically produced by neutralizing the acid form of the surfactant in the presence of a builder. Low density granules are commonly produced by making an aqueous paste of neutralized surfactant and builder, and by spray drying the paste to form granules. The higher density detergent granules were manufactured by carrying out the neutralization of the surfactant and the incorporation of a builder in a mixer.

Typically, the water, added alone or with another raw material, and / or a flow aid, is used to obtain complete neutralization and desired granule formation in said mixing process. The granules must then be dried to remove the excess water. It is an object of the present invention to provide a process for making highly active, high density detergent granules containing an ammonium surfactant and a phosphate detergent improver. It is a further object of the present invention to provide said process with minimal incorporation of water, so that the drying of the produced detergent granules is unnecessary. It is also a further object of the present invention to provide such a method in which the incorporation of a flow aid into the process is unnecessary. It is also an object of the present invention to provide said process which produces small granules.

BRIEF DESCRIPTION OF THE INVENTION The present invention includes a continuous process for producing highly active and high density detergent granules consisting essentially of the following steps: (a) preparing a mixture in a high speed mixer, the mixture being prepared from components fed into the mixer which consist essentially of the following: (1) from about 15% to about 35% of an ammonium surfactant acid selected from alkylbenzenesulfonic acid and alkylsulfupic acid and mixtures thereof; (2) from about 5% to about 65% of a phosphate detergent builder selected from polyphosphates and pyrophosphates and mixtures thereof; and (3) from about 10% to about 65% particulate carbonate selected from sodium carbonate and potassium carbonate and mixtures thereof, the amount of carbonate being at least 2 times the amount theoretically necessary to neutralize the ammonium surfactant acid; (b) agglomerating the mixture of step (a) in a moderate speed mixer; whereby the ammonium surfactant acid is neutralized by the carbonate, and the resulting detergent granules have an overall density of more than about 550 g / 1 and a water content of less than about 7%.

DETAILED DESCRIPTION OF THE INVENTION The present invention includes a two step mixing process for producing highly active and high density detergent granules by dry neutralizing the acidic form of an anionic detergent with a particulate inorganic carbonate compound and in the presence of a phosphate builder. Typically, said detergent granules are subsequently mixed with other ingredients to produce a granular detergent product, especially suitable for cleaning clothes. The process of the present invention produces a mixture from raw material, the raw material preferably consisting essentially of an anionic surfactant acid, a phosphate builder and sources of alkali metal carbonate feedstock.

Raw material The process of the present invention includes the neutralization of an anionic surfactant acid. The anionic surfactant acid raw material that is useful in the process of the present invention consists essentially of alkylbenzenesulfonic acid or alkylsulfuric acid or a mixture thereof. The anionic surfactant acid raw material preferably has a moisture content of less than about 0.3%, most preferably less than about 0.1%. Based on the total weight of the raw material added during the process of the present invention, the amount of anionic surfactant acid is from about 15 to about 35%, preferably from about 20% to about 30%, and preferably from about 25% to approximately 28%. The preferred alkylbenzene-phonic acid useful in the present process includes that with an alkyl portion which is straight chain or branched chain, preferably having from about Q to about 18 carbon atoms, most preferably from about 10 to about 16 carbon atoms. The alkyl chains of the alkylbenzenesulonic acid have preferably an average chain length of from about 11 to about 14 carbon atoms. The alkylbenzene sulphide acid which includes branched chain alkyl is called HP.BS (ABS when neutralized). Alkylbenzenesulfonic acid, which is straight chain, is preferred because it is biodegraded more easily; and it is called HLAS (LAS when neutralized). The preferred alkylsulfuric acid useful in the present process includes that with an alkyl portion which is straight chain or branched chain, preferably having from about 9 to about 24 carbon atoms, most preferably from about 10 to about 20 carbon atoms, more preferably still from about 12 to about IB carbon atoms. The alkyl chains of the alkylsulfuric acids preferably have an average chain length of from about 14 to about 16 carbon atoms. The alkyl chains are preferably linear. Alkisulfuric acids (HAS, AS when neutralized) are typically obtained by sulfating fatty alcohols produced by reducing the glycerides of fats and / or oils from natural sources, especially from tallow or coconut oil. The anionic surfactant acids useful in the process of the present invention can also be combinations of alkylbenzenesulonic acid and alkylsulfuric acid, either mixed together or added during the process separately. Combinations having an alkylbenzenesulfonic acid to alkylsulfuric acid ratio of from about 20:80 to about 80:20 are preferred, and those having a ratio of from about 40:60 to about 60:40 are preferred. The raw material of phosphate builders useful in the process of the present invention is in the form of particles and consists essentially of the water-soluble salts of polyphosphates or pyro or mixtures thereof. The raw material of phosphate builders preferably has a moisture content of less than about 2%, most preferably less than about 1%. Based on the total weight of the raw material added during the process of the present invention, the amount of phosphate builder is from about 5% to about 65%, preferably from about 15% to about 55%, most preferably about 25% to approximately 45%. The raw material of phosphate detergent builders is preferably obtained in powder form with an average particle size of about 10 microns to about 50 microns, and preferably about 20 microns to about 30 microns. If coarse raw material is obtained, a conventional pre-rolling step can be used to obtain a desired distribution of the particle size. A preferred detergency builder useful in the present process is sodium t-ripolyphophosphate (STPP); STPP can be obtained commercially from, for example, FMC Corp. Another preferred phosphate detergent builder is tetrasodium pyrophosphate (TSPP); TSPP can be obtained commercially from, for example, FC Corp. The process of the present invention utilizes particulate alkali metal carbonate feedstock, preferably consisting essentially of sodium carbonate or potassium carbonate or a mixture thereof, for the neutralization of ammonium surfactant acids. The alkali metal carbonate is preferably fed in the present process as a powder having an average particle size of about 1 miter to about 40 microns, most preferably from about 5 microns to about 15 microns. If a thicker raw material is obtained, a conventional pre-rolling step can be used to obtain a desired particle size distribution. The alkali metal carbonate feedstock preferably has a moisture content of less than about 2%, rnuy preferably less than about 1%. Based on the total weight of the raw material added to the process of the present invention, the amount of alkali metal carbonate is from about 10% to about 65%, preferably about 2 (3% to about 55%, most preferably from about 30% to about 45% .To neutralize the ammonium surfactant acid, each carbonate ion (CO3 *) reacts with two acid hydrogens (H +) .From this reaction the amount of carbonate raw material required can be determined to theoretically neutralize all the acidic material The amount of carbonate fed in the present process is at least about 2 times that which is theoretically necessary to neutralize the acid, preferably about 4 times to about 20 times, most preferably about 5 times to about 15 times , more preferably still about 6 times to about 12 times. According to the present invention, substantially the only water present in the materials while passing through the process are the minor amounts of moisture present in the raw material and the water generated by the neutralization reaction. Throughout the process, the maximum amount of water in the materials being processed is preferably about 8%, most preferably about 6%, more preferably still about 5%, and still more preferably about 3%. The loss of water (which is due to evaporation) during the present process, based on the weight of the granules produced, is less than about 2%, preferably from about 0.5% to about 1.5%. The amount of moisture in the detergent granules produced by the present process is from about 0% to about 7%, preferably from about 0.5% to about 5%, most preferably from about 1% to about 3%. The detergent granules produced in this way can be somewhat hygroscopic and collect moisture from the atmosphere. The detergent granules made by the process of the present invention preferably have an overall density of about 550 g / 1, most preferably from about 600 g / 1 to about 900 g / 1, more preferably even about 650 g / 1. 1 to about 850 g / 1, still more preferably from about 700 g / 1 to about 800 g / 1. The detergent granules of the process of the present invention preferably have an average particle size of from about 200 microns to about 600 microns, most preferably from about 300 microns to about 500 microns, more preferably even from about 350 microns to about 450 microns. In the processes of the present invention, the materials that are processed and the detergent granules produced are kept substantially free of flow aids such as silicas, clays, diatornaceous earth, aluminosilicates, pearlite and calcite.

Process Steps The continuous process of the present invention comprises two mixing steps; preferably, the method essentially consists of two steps, very preferably consists of two steps. The first step of the process of the present invention is carried out in a high speed, high shear mixer. Suitable mixers for this step include, for example, the Loedige CB *, the? Hugí Granulator *, and the Drais K-TTP *. The preferred mixer for the first step of the process of the present invention is Loedige CB *. Typically, the high-speed mixer has a substantially cylindrical mixing chamber having from about 0.3 rn to about 1 m in diameter and from about 1 m to about 3.5 m in length. For the mixers used in the first step of the process of the present invention, the preferred mixers have a central arrow with mixing paddles attached to it, which preferably rotates at a speed of from about 300 rpm to about 1800 rpm, most preferably from about 350 rpm to about 1250 rprn, still more preferably from about 400 rprn to about 600 rprn, the rate being generally lower for large rne mixers. The high speed mixer is preferably covered with water to allow cooling water to flow through the mixer cover and thus remove the heat generated by the neutralization reaction. For the first step of the present method, the above three materials are typically fed to the high-speed mixer near one end of the cylindrical chamber and intimately mixed as they pass through the chamber; the mixture is discharged near the other end of the cylindrical chamber. The typical average production rate is from about 0.2 kg / sec to about 17 kg / sec, especially from about 9 kg / sec to about 13 kg / sec, generally achieving higher production speeds using larger mixers. The average residence time of the materials in the mixer of the first step is preferably from about 2 seconds to about 30 seconds, most preferably from about 5 seconds to about 20 seconds, more preferably still from about 10 seconds to about 15 seconds. The cooling water at a temperature < From about 5 ° C to about 25 ° C, it is preferably fed into the water cover of the high speed mixer. The temperature of the mixture in the discharge from the high-speed mixer is typically from about 35 ° C to about 70 ° C, preferably from about 45 ° C to about 55 ° C. Most of the neutralization of the ammonium surfactant acid by the carbonate occurs in the first step of the process of the present invention. Preferably, substantially all neutralization takes place in the first step. The neutralization reaction can be completed after the mixture is discharged from the mixer of the first step. The ammonium surfactant acid is substantially completely neutralized during the process of the present invention. The materials discharged from the mixer of the first step are typically fed substantially immediately into the mixer of the second step. The average residence time for the materials between the mixers is preferably less than about 5 minutes, most preferably less than about 1 minute. The second step of the process of the present invention is carried out in a moderate speed mixer. Suitable mixers for this step include grate mixers, for example, the Loedige KMR and the Drais K-TR. The Loedige KM "is the preferred mixer for the second step of the process of the invention., the moderate speed mixer has a substantially cylindrical mixing chamber having from about 0.6 rn to about 2 n diameter and from about 2 in to about 5 rn in length. Preferred mixers have a central arrow with mixing paddles attached thereto, preferably rotating at a rate of from about 40 rprn to about 160 rprn, most preferably from about rprn to about 140 rpm, still more preferably from about 50 rprn to about 80 rprn, the speed being generally lower for larger mixers. The moderate speed mixer preferably has a water cover to allow lukewarm water to flow through the mixer cover and thus maintain the temperature of the product in the moderate speed mixer at approximately its inlet temperature. For the second step of the present method, the mixture of materials discharged from the mixer of the first step is typically fed to the moderate speed mixer near one end of the cylindrical chamber, mixed while passing through the chamber, and discharged near the other end. of the cylindrical chamber. Typically, the production rate for the second step is the same as that of the first step. The average residence time of the materials in the mixer of the second step is preferably from about 20 seconds to about 300 seconds, most preferably from about 30 seconds to about 90 seconds, still more preferably from about 40 seconds to about 55 seconds. Water at a temperature of from about 25 ° C to about 50 ° C is preferably fed to the water cover of the moderate speed mixer. The temperature of the mixture in the discharge of the moderate speed mixer is typically from about 35 ° C to about 70 ° C, preferably from about 45 ° C to about 55 ° C.

EXAMPLES The following non-limiting examples exemplify the methods of the present invention.

EXAMPLES 1-18 Examples 1-7 are carried out using a Loedige CB-30 * with water cover as the high speed mixer and a Loedige KM-60QR mixer with water cover as the moderate speed mixer. The product passes immediately from the high speed mixer to the moderate speed mixer. Table 1 shows the production rate for each of the examples 1-8, and indicates the speed of the mixer and the temperature of the water cover of each mixer. Table 1 also shows the amount of carbonate fed to the mixer in terms of the multiple of that amount necessary to neutralize all the ammonium surfactant acids fed to the process for each example.

TABLE 1 In each of the examples 1-7 three materials are continuously fed to the high speed mixer: an ammonium surfactant acid material, a phosphate builder material and a particulate carbonate material. The amount of each material fed in each of Examples 1-7 is the amount needed to produce the products shown in Table 2 below. The HLAS material obtained from P lot Chemical Co. under the tradename Calsoft LAS-99R has an average of about 12 carbons in the alkyl chain and has a minimum purity of 96%. The HABS material, obtained from Pilot Chernical Co. under the trade name Ernulsifier 99R, has an average of about 12 carbons in the alkyl chain and has a minimum purity of 96%. The alkylsul-upco acid material is derived from coconut oil, and has an average of about 13-14 carbon atoms in the alkyl chain, and has a minimum purity of 96%. The STPP and TSPP materials are obtained from FMC Corp., and have a minimum purity of 94%, the impurities being mainly other phosphates. The sodium carbonate material, obtained from FHC Corp., has a minimum purity of 98%.

TABLE 2 The water in the products of Examples 1-8 is produced in the neutralization reaction or comes with the materials. Sodium sulfate is a by-product of the neutralization reaction, due to the presence of a small amount of impurities in the sulfuric acid in the ammonium surfactant acid. The other materials are impurities that come with the materials.

EXAMPLE 9 Example 8 is similar to the procedures in examples 1-8, except that mixers use "Jos" are larger: a Loedige CB-100R with water cover as the high-speed mixer and a Loedige KM-15,000R with cover for water as the speed mixer rnotjerada. The product is produced at a speed of 8.3 kg / sec. The high speed mixer operates at a speed of 450 rpm with water at 5 ° C fed into the water cover. The "Jad moderate" speed mixer operates at 60 rpm with water at 25 ° C fed into the water cover. The amount of sodium carbonate fed to the process is 10.3 times the amount necessary to neutralize the ammonium surfactant acid. The product made in Example 9 is shown in Table 3 below.

TABLE 3 The material and sources of the product component are the same as for examples 1-8.

Although particular embodiments of the present invention have been described, it will be obvious to those skilled in the art that various changes and modifications can be made to the present invention without departing from the spirit and scope of the invention. It is intended to cover, in the appended claims, all those modifications that are within the scope of this invention.

Claims (18)

NOVELTY OF THE INVENTION CLAIMS

1. - A continuous process for producing highly active and high density detergent granules consisting essentially of the following steps: (a) preparing a mixture in a high-speed mixer, the mixture being prepared from components fed into the mixer consisting of essentially of the following: (1) from about 15% to about 35% of an ammonium surfactant acid selected from alkylbenzenesulonic acid and alkylsulfoxide acid and mixtures thereof; (2) from about 5% to about 65% of an improved phosphate detergency selected from polyphosphates and pyrophosphates and mixtures thereof; and (3) from about 10% to about 65% of particulate carbonate selected from sodium carbonate and potassium carbonate and mixtures thereof, with the amount of carbonate being at least 2 times the amount theoretically necessary. to neutralize the ammonium surfactant acid; (b) agglomerating the mixture of step (a) in a moderate speed mixer; whereby the ammonium surfactant acid is neutralized by the carbonate, and the resulting detergent granules have an overall density of more than about 550 g / 1 and a water content of less than about 7%.

2. The process according to claim 1, wherein the average particle size of the detergent granules produced by the process is approximately 200 microns to about 600 microns.

3. The process according to claim 2, wherein the amount of carbonate fed to the mixer is at least about 4 times the amount theoretically necessary to neutralize the acid of ammonium surfactant, and wherein the content of Water of the granules produced by the process is less than about 5%.

4. The method according to claim 3, wherein the average residence time of the material in the high-speed mixer is from about 2 seconds to about 30 seconds; and wherein the average residence time of the material in the moderate speed mixer is from about 20 seconds to about 300 seconds.

5. The process according to claim 4, wherein the alkyl portion of the alkylbenzenesulfonic acid is straight chain or branched chain having from about 8 to about 18 carbon atoms, and the alkyl portion of the alkyl sulfuric acid is straight chain or branched chain having about 8 to about 24 carbon atoms. 6.- The procedure in accordance with the? : > claim 5, wherein the overall density of the granules produced in the process is from about 650 g / 1 to about 850 g / 1, and in which the average particle size of the detergent granules produced by the process is from approximately 300 microns to approximately 500 microns. 7. The process according to claim 6, wherein the average residence time of the materials in the high-speed mixer is from about 5 seconds to about 15 seconds, and the average residence time of the materials in the Moderate speed mixer is about 30 seconds to about 55 seconds. 8. The method according to claim 7, wherein both mixers have chambers substantially mixed cylindrical with a central arrow; wherein the arrow of the high-speed mixer rotates at a speed of about 300 rpm at about "1,800 rpm; and wherein the arrow of the moderate speed mixer rotates at a speed of about 40 rpm at about 160 rpm. 9. The process according to claim 5, wherein the amount of anionic surfactant acid fed into the process is from about 20% to about 30%. 10. The process according to claim 0, wherein the amount of acid (ammonium surfactant) fed into the process is approx.from about 20% to about 30%, and the amount of carbonate is about 5 times to about 15 times the amount theoretically necessary to neutralize the ammonium surfactant acid. 11. The process according to the indications 1, 5, 7 or 10, in which the water content of the granules produced by the process is less than about 3%. 12. The process according to claim 10, wherein the speed of the high speed mixer is from about 400 rpm to about 600 rprn, and the speed of the moderate speed mixer is from about 50 rprn to about 80 rprn. 13. The process according to claim 10, wherein the phosphate detorgent enhancer is STPP, and the carbonate fed into the process is sodium carbonate. 14. The process according to claim 10, wherein the phosphate detergent builder is TSPP, and the carbonate fed into the process is sodium carbonate. 15. The process according to claim 14, wherein the acid fed into the process is alkylsulphuric acid having an average chain length of about 14 to about 16 carbon atoms. 1

6. The process according to claim 14, wherein the acid fed in the process is HABS having an average chain length of about 11 to about 14 carbon atoms. 1

7. The process according to claim 14, wherein the acid fed in the process is HLAS having an average chain length of about 11 to about 14 carbon atoms. 1

8. The process according to claim 14, wherein the acid fed in the process is a mixture of alkylsulfuric acid and alkylbenzene sulfonic acid having a ratio of about 20:80 to approx. .