JPH07500125A - Method for producing detergent composition containing alkyl sulfate particles and base granules - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

[Detailed description of the invention] Method for producing detergent composition containing alkyl sulfate particles and base granules Technical field The present invention involves separately preparing the spray-dried base granules and the alkyl sulfate particles. , and then on a method of manufacturing granular detergent compositions by mixing them. Ru.

Background technique The traditional method of manufacturing detergent granules is spray drying. Typically surfactants, building blocks Detergent ingredients such as detergent, silicates, and carbonates are mixed in a tank and the water is removed. Prepare a slurry of 35% to 50% target. This slurry is then transferred to a spray drying tower. to reduce moisture content. Dense detergent granules are obtained by compacting spray-dried particles. It is possible to prepare Moore et al., US Special Issue, December 29, 1987. See specification No. 4,715,979. However, the spray drying method generally Limited amounts (less than 40%) of organic ingredients such as surfactants are added for environmental and safety reasons. include.

Another method for preparing detergent particles is, for example, after continuous neutralization in a continuous neutralization loop. , U.S. Patent Application No. 364, filed June 9, 1989, which is a method of forming particles. ．． Mueller et al., filed on January 28, 1991, which is a partial continuation of Specification No. 721. Currently pending U.S. Patent Application No. 647,338 uses a continuous neutralization system. particles can be formed after forming highly active (active ingredients>50%) detergent granules. Are listed. polyethylene glycol and/or ethoxylated non-ionic The surfactant number, alkyl sulfates in concentrated sodium hydroxide (≧about 62%) and /or added during neutralization of alkylbenzenesulfonic acid. Adjustment method and particles prepared by this method. This case is 19 Published as EP No. 90306139.8 on December 12, 1990 .

Co-pending U.S. Patent Application Section 55 of Ojosu Asante et al., filed July 16, 1990 No. 2.663 (grant) states that anionic fields in acid form in continuous neutralization systems are By reacting a surfactant with an alkali metal hydroxide, glutamic acid, aspartic acid, Aminomalonic acid, aminoadipic acid, and 2-amino-2-methylpentanedi alpha-aminodicarboxylic acids selected from the group consisting of High activity involving the addition of alkali metal salts to the neutralization system during the production of the neutralized product The manufacturing process of active detergent particles is described. Highly active detergent particles are included.

Co-pending U.S. Patent Application Section 288 of Strauss et al., filed December 22, 1988. No. 759 (Permit) I; 6, highly active surfactant using finely dispersed cold granulation A method for producing concentrated surfactant granules from a paste is described. child This was published as specification EP 89306335.4 on January 3, 1990. It was.

U.S. Pat. No. 4.534.879 to Eiding et al., issued August 13, 1985. The specifications include sodium alkyl sulfate and sodium alkylbenzenesulfonate. Improved synthetic surfactant from roll drum dry paste containing water-soluble inorganic salts Discloses a method for producing flakes. Heat flakes are produced in low moisture environments with low dew points. It is cooled.

In all of the above, highly active alkyl sulfate particles are Granular cleaning by mixing with a spray-dried base granulate that contains little or no Detergent builder and soluble silicate A large amount of alkyl sulfate is Rusulfate and C1o-l-alkylbenzene sulfonate and/or The authors do not disclose compositions containing particles having C12-18 or C12-18 soaps.

Demonstration of invention The present invention (a) less than about 2% alkyl sulfate by weight of the spray-dried granulate; Anionic surfactant other than phate 0 to about 40%; Detergent builder about 10 to 80% %; and about 1-15% soluble silicate; (b) The alkyl sulfate particles are produced by a process including continuous highly active neutralization. The weight of the alkyl sulfate particles is 0 to 1 mole of alkyl sulfate. C alkyl sulfate 12-18 ethoxylated with about 4 moles of ethylene oxide Contains about 60-99% of esters); (c) said spray-dried granules and said alkyl sulfate particles each about 10: Mix in a ratio of 90 to 99:1 The present invention relates to a method for producing a granular detergent composition.

BEST MODE FOR CARRYING OUT THE INVENTION First, reduce feathering emissions from the spray drying tower and use a high surfactant spray dryer. In an effort to improve the physical properties of dried particles, alkyl sulfates have been removed from the spray drying process. were removed and incorporated into separately prepared "alkyl sulfate particles".

The removal of alkyl sulfates from the spray drying tower is Reduces the total amount of sticky organic matter in the product, thus reducing clumping and caking It was found that there was an improvement. Additionally, the alkyl sulfate can be dried outside the spray drying tower. Adding by a separate process reduces the total organic load in the column and This has been shown to reduce visible feathers and reduce the impact on the environment. Served.

Furthermore, the production rate of phosphorus-free (non-phosphate) particulates is higher than that of alkyl sulfates. Can be increased (up to about 30%; equivalent group dry load and (based on clarification and clarification moisture).

Other predominant and often used anionic surfactants, lines from spray drying towers Removal of alkylbenzene sulfonate (rLAsJ) alone It is thought that there is no reduction in the feathery appearance as in the case of feathers.

The production of alkyl sulfate particles by continuous neutralization is described in the aforementioned co-pending U.S. patent application. No. 647,338 and No. 552,663.

In this method, spray-dried granules are produced by conventional spray-drying means. . They contain less than about 2% alkyl sulfates, detergent builders, and soluble Contains silicates. Other detergent ingredients commonly added to spray-dried granules are also included here. It may be added with Alkyl sulfate particles are used in a continuous highly active neutralization system (hereinafter referred to as (see below) in a separate process. The spray-dried granules are then Mix with lukylsulfate particles. Other conventional detergent ingredients may also be mixed.

Manufactured with less feathering emissions, higher production rates and improved physical properties A highly consumer-acceptable product can be achieved using the present invention. Also, detergent set The amount of surfactant in the formulation adds more alkyl sulfate particles to the composition. It can be easily increased by Dense granular detergent compositions contain alkyl sulfates. It is easier to prepare due to the flexibility of mixing particles. Detergent builder, soluble Silicates, anionic surfactants, and other desired ingredients are spray dried in the granules. large amounts of alkyl salts that can be added through the Ruphate can be added via alkyl sulfate particles.

The term particle is used herein interchangeably with particulate.

■, alkyl sulfate particles Alkyl sulfate particles are produced by a process that includes continuous highly active neutralization. child These particles contain 1 mole of alkyl sulfate by weight of alkyl sulfate particles. C12-18 ethoxylated with 0 to about 4 moles of ethylene oxide per ethylene oxide, preferably or about 60 to 99% of the 014-1B alkyl sulfate, preferably about 70 to 99%. Contains 90%. The alkyl sulfate is preferably not ethoxylated (ethyl sulfate). 0 moles of ren oxide). Alkyl sulfate particles are particularly suitable for non-ethoxylated alkyl sulfate particles. If rusulfate is used, about 4 to 25 weights of alkyl sulfate particles %, preferably about 8-14% by weight of c1o-16, preferably 011-14 linear Preferably, it contains an alkylbenzene sulfonate. Alkyl sulfate Mixtures of alkyl ethoxy sulfates and alkyl ethoxy sulfates may also be used. Alkyrie If toxysulfate is used, approximately 0.5 to 2 moles of ethylene oxide are preferred. Alkyl sulfate fury is preferred.

Useful alkyl sulfate surfactants include 012-16 linear or branched alkyl sulfate surfactants. Water-soluble salts of sulfuric acid, especially alkali metal salts, ammonium salts and alkanol salts ammonium salts (e.g. monoethanol ammonium salt or triethanolammonium salt) ammonium salt).

The method for producing alkyl paste particles consists of the following steps.

A. Addition of acids and caustics The essential first step is the continuous neutralization system. sulfuric acid, and preferably C1o-16 alkylbenzenesulfonic acid or Reacting the mixture with a sodium hydroxide solution containing about 62% or more hydroxide by weight (preferably without kneading) to produce a neutralized product. neutralization generation The article preferably has less than about 12% water by weight.

Preferably, the ingredients of the detergent composition are not kneaded in a continuous neutralization system. continuous The neutralization system preferably does not include a hermetic mixer.

Continuous neutralization systems preferably do not substantially deposit additional crude materials in the detergent composition. stomach. In other words, other than surfactants, caustics and/or propylene glycol of crude material is preferably not fed to the system. For example, approximately 5% additional raw material less than about 1%, preferably less than about 1%, should be present in a continuous neutralization system. essentially Detergent builders or additional organic materials should also not be fed into the continuous neutralization system. is most preferable.

C alkyl (ethoxylated) sulfuric acid and C1o~1612~18 Alkylbenzene sulfonic acids can be produced by any sulfation/sulfonation method. Sulfonation can be carried out with SO3 in a falling film reactor, preferably in air. do. Synthetic Deterge nts), 7th edition, A. S. Davidson and B. Mirwidski, John. ・Willie & Sons Incorporated, 1987, pp. 15 See 1-168.

012-1B alkyl sulfate, and C linear 710-IB with it A mixture with alkylbenzenesulfonic acid is preferred for use herein. 2 types The mixture is an improvement of detergent particles prepared from the paste prepared using the mixture. Most preferred due to its dispersibility. The two acids are placed in separate streams in a continuous neutralization system. can be added or mixed before addition. Alternatively, prepared from each separate acid The paste can be mixed after neutralization.

In nature, sodium 012-18 alkyl sulfate versus C1o-16 linear alkyl sulfate The final ratio of sodium killbenzenesulfonate is from 75:25 to 96:4 , preferably from 80:20 to 95:5.

C alkyl sulfate is 14-1612-18 from C alkyl sulfate Also preferred for use in essential step (a). 014-15 alkyl sulfuric acid is the most is also preferable.

011-14 linear alkylbenzene sulfonic acid is C1o-IB alkylbenzene preferred over sulfonic acid.

012-13 linear alkylbenzene sulfonic acids are most preferred for use herein. Yes.

Steps to neutralize alkyl sulfates and/or alkylbenzenesulfonic acids The sodium hydroxide used in (a) is preferably about 62% by weight or more of hydroxide. 68% by weight or more, most preferably about 73% by weight. This highly concentrated caustic solution melts at high temperatures and therefore the caustic delivery system prevents "cold spots". must be carefully maintained at the required temperature to prevent "Cold spot" ” is the temperature at which the system is below the melting point of the caustic (e.g., 1 for 73% caustic). Feeding systems, pumps, and metering systems that reach 55″F or 68.3°C) , a point in a pipe or valve. Such "cold spots" are caused by caustic This may result in crystallization of the substance and blockage of the feeding system. Typically, the ``Hydrospot'' uses a hydrothermal jacket, electric tracing, and electric heating engine. Averted by Roger.

Sodium hydroxide is preferably used in a fraction of the stoichiometric amount needed to neutralize the acid. Exist in excess. Excess alkalinity (excess caustic) in the neutralization system If 2O- (where M is metal) exceeds about 1.5%, the paste will have a high viscosity. therefore, it is difficult to circulate through a continuous neutralization system. excess alkalinity If the It may not be stable over time. Therefore, the excess of melted paste in the neutralization system Alkalinity (measurable by acid titration) is about 0.1% to 1.5%, more preferably or about 0.2% to 1.0%, most preferably about 0.3% to 0.7%. is preferred.

The acid and caustic are preferably mixed together as quickly as possible using a high shear mixer. Kisser and separately into a continuous neutralization system. The high shear mixer preferably includes: Specifically designed for thorough mixing of viscous liquids.

Generally, in a continuous neutralization loop, the components are passed through a pump (typically centrifugal). The pump circulates the material through a heat exchanger in the loop and into the bottle. The material is then passed back through the tube where new material is introduced. Put in as much product as you emit. First, the material in the system recirculates without interruption. The product is usually placed after the pump. Exit through the control valve. The recirculation rate of the continuous neutralization loop is approximately 1:1 to 50:1. It is. The temperature of the neutralization reaction can be adjusted by adjusting the degree of cooling by a heat exchanger. It can be controlled to a certain degree. ``Processing amount'' refers to the amount of acid and caustic introduced. can be controlled by

The continuous neutralization loop should be modified as follows to implement its true nature.

(1) Insulate the loop.

(2) Positive displacement centrifugal pumps that can better handle very viscous materials Change to pump.

(3) Caustic supply system capable of handling concentrated caustic (over 50% solids) Install the system.

(4) Introducing the material through a high shear mixer placed in-line.

(5) Preferably after high shear mixer, polyethylene glycol and/or Install a metering system for ethoxylated nonionic surfactants.

(6) High shear mixer of acid and caustic inlet streams to produce the highest degree of mixing possible. Place it on the server.

(7) The temperature of the loop should be kept low for the paste to ensure proper recirculation and mixing. It should be high enough to maintain viscosity. However, the temperature Should not be so high as to cause hydrolysis of the kyl sulfate or alkyl sulfate. stomach. Typical paste temperatures in the loop are approximately 180 below (82,2°C) to 230°C. (110°C), preferably about 200″F (93,3°C) to 210″F (98,9°C) ℃).

An optional second step in nature is to add molecular weight 2 ．． 000 to 50,000 polyethylene glycol and/or about 120 pieces ( A formula with a melting point of 48,9℃ or higher R(OC2H4)nOH (wherein R is a 012-1B alkyl group or a C8-16 an ethoxylated nonionic alkylphenol group, n is about 9 to about 80 Adding a surfactant. The weight of the additive of step (b) versus the mixture of step (a) The quantitative ratio is about 1:5 to about 1:20.

Polyethylene glycol and/or ethoxylated nonionic surfactants They can also be added separately or as a mixture to a continuous neutralization system. neutralization loop , these one or more additives are preferably recirculated after the high shear mixer. Enter the loop before the ring pump. Additives must be melted before addition to the neutralization system. and therefore can be metered.

These two additives enhance cleaning performance and reduce temperatures below about 120"F (48.9C). Detergent particles that are full and solid and therefore hard at room temperature can be prepared from neutralized pastes. So, you will be selected. They also indicate that each additive increases the viscosity of the highly active paste during the neutralization loop. It is chosen because it also acts as a processing aid by reducing the viscosity. This viscosity reduction The start of the neutralizer loop is where the surfactant concentration is increased through the "interphase" region. sometimes especially important. Some alkyl sulfates It has a concentration of 40% to 60%.

Polyethylene glycol with a molecular weight of about 2,000 to 50,000 is an ethoxylated non- Preferred over ionic surfactants. Molecular weight about 3,000-20,000, preferably Kui! Polyethylene glycol strength of 7,000 to 12,000 (more preferably , polyethylene glycol (rPEG 8,000'') with a molecular weight of s,ooo Most preferred. In the present invention, polyethylene glycol versus acid/caustic acid in step (a) The preferred weight ratio of the mixture is from about 1:8 to about 1=12. Molecular weight s, o In the case of polyethylene glycol with oo, the preferred weight ratio is PE08 , 0,001 parts to 10 parts of acid/caustic mixture.

Polyethylene glycol is a compound with a molecular weight of about 2,090 to 50,000 produced from the polymerization of ethylene oxide and ethylene glycol in sufficient quantities to give to be accomplished. It is obtained from Union Carbide (Danbury, CT). can be done.

Preferred ethoxylated nonionic surfactant materials have the formula R(QC　H　)OH(formula Middle, R ha 012-18 alkyl 4n and n is about 12 to about 30). 18 per mole of alcohol Tallow alcohol ethoxylated with mol of ethylene oxide (rTAE 1 8J) is most preferred. The preferred melting point of the ethoxylated nonionic surfactant is Greater than about 140″F (60°C).

Examples of other ethoxylated nonionic surfactants of the invention include 1 mole of decylphenol and Condensation product with 9 moles of ethylene oxide, 1 mole of dodecylphenol and ethylene oxide Condensation product with 16 moles of tetradecylphenol and 2 moles of ethylene oxide Condensation product with 0 mol or 1 mol of hexadecylphenol and 3 ethylene oxide It is a condensate with 0 mol.

Continuous neutralization is (a) In a highly active continuous neutralization loop, the alkyl sulfate in acid form is about 30 to 75% by weight of oxide and from stoichiometric to slightly stoichiometric excess React with the sodium hydroxide solution present to produce a neutralized product: (b) The particles formed from the product of step (b) contain about 0.0% α-aminodicarboxylic acid. The neutralized product is added to the continuous high activity neutralization loop so as to contain 2 to 15% by weight of the neutralized product. When grown, glutamic acid, aspartic acid, aminomalonic acid, aminoadipic acid, and α- selected from the group consisting of 2-amino-2-methyl-bentanedioic acid. Add aminodicarboxylic acids or their alkali metal salts This can be done by a method characterized by:

The alkali metal salts of glutamic acid or aspartic acid are preferably Add to pool. Preferably monosodium glutamate and/or glutamate Approximately 1-10% by weight of disodium phosphate is added to the neutralization loop.

The alkali metal hydroxide solution is preferably about 62-73% hydroxide by weight. . Sodium hydroxide is preferred.

The neutralization product preferably has less than about 12% water by weight. The third step in the particle manufacturing process is to form detergent particles. Detergent particles are continuously It can be formed in a variety of ways from the neutralized products exiting the neutralization system.

The desired detergent particle size distribution is about 100-1200μ, preferably about 150-600μ. It has a range of μ, with an average of 300μ.

The molten paste from the continuous neutralization loop can be atomized into droplets in a prilling (cooling) tower. Wear. To avoid any prilling, the molten paste is simultaneously cooled and pressed. It can be strained, cut, or ground to the desired particle size.

The third option is to chill-roll the molten paste until it reaches a dough-like consistency. cooling on a heat exchanger unit, at which point other detergent ingredients are removed. Can be kneaded. The resulting dough can then be granulated by mechanical means.

A fourth preferred option is to cool the molten paste on a chill roll into flakes; The next step is to grind the flakes to the desired particle size. additional drying is required If the It can be dried with

■, Spray-dried granules Spray-dried granules for use in nature can be prepared by conventional spray-drying methods. . They contain less than about 2% alkyl sulfate by weight of the spray-dried granules; Anionic surfactant other than rusulfate 0 to about 40%; Detergent builder about 10% ~80%; and about 1-15% soluble silicate (as structuring agent), preferably Prepared by a spray drying method consisting of spray drying a slurry containing 2-5% Ru.

About 5-30% anionic surfactant is preferred. Anionic surfactants are preferred is C linear alkyl 10-16 It is a salt of benzenesulfonic acid. C linear alkyl 11-14 About 10-20% sodium benzenesulfonate is most preferred.

Phosphorus-free granules are preferred. The spray-dried granules are preferably carbonate, saline, etc. selected from the group consisting of itrates, aluminosilicates, and mixtures thereof. Contains about 30-60% by weight of detergent building blocks. Most preferably sodium carbonate and/or a water-soluble inorganic salt, preferably about 5-60% by weight of sodium sulfate. Included.

In version 1B, the spray-dried granules contain about 5-50% sodium aluminosilicate. Including amount%.

An applicable spray drying method is described in US Pat. No. 4,715,979, Chamberline, issued October 16, 1990 No. 4,963,226, issued Aug. 17, 1982; U.S. Pat. No. 4,344,871 to All Away et al., incorporated herein by reference. (incorporated).

■, mixed The spray-dried granules and alkyl sulfate particles are each from about 10:90 to 99=1, more preferably about 50:50 to 99:1, more preferably about 7 Mix in a ratio of 0:30 to 90:10, most preferably about 85:15. Ru. Mixing can be done by conventional means. Preferably, the finished composition Approximately 2-40% by weight of detersive builder is mixed with the (finished) granules.

The alkyl sulfate particles and said spray-dried granules are preferably used in the finished composition. About 3-10% by weight of citric acid and effective amounts of flavoring and enzymes are mixed.

■1 Scope of composition claims 2 inventions, methods of making the compositions, and the compositions themselves are considered to be included herein. the latter about 4-20% C1o-1-alkyl for enhanced solubility in cold water Contains benzene sulfonate and/or 012-1g (coconut) soap Contains alkyl sulfate particles. Alkyl sulfate is the same as above For this reason, it is incorporated into highly active particles rather than base granules.

By weight of finished composition (a) Weight of alkyl sulfate particles, per mole of alkyl sulfate C12-18 alkyl sal ethoxylated with O to about 4 moles of ethylene oxide Phate about 60-99%; C1o-ta linear alkylbenzene sulfonate and and/or alkyl sulfate particles containing about 4-20% of C1°-18 soap. ~90%; and (b) less than about 2% alkyl sulfate by weight of the granulate; alkyl sulfate; 0 to about 40% of anionic surfactants other than; about 10 to 80% of detergency builders; and 10-99% base granular material containing about 1-15% soluble silicates Particulate detergent compositions are included.

Preferred granular detergent compositions of the present invention have a (a) Weight of alkyl sulfate particles, essentially 012-18 alkyl sulfate about 60-99%; C1o-16 linear alkylbenzene sulfonates and / or C1□~18 soap approximately 4~20%; molecular weight approximately 2,000~50,000 Polyethylene glycol approximately 5-20%; glutamic acid, aspartic acid, amino Malonic acid, aminoadipic acid, and 2-amino-2-methyl-pentanedione α-aminodicarboxylic acids selected from the group consisting of acids, or their alkali metal about 0.2-15% of metal salts; and 1-15% of water and/or unreacted materials. 1-90% of alkyl sulfate particles; and (b) 10-99% of the base particulate material containing less than about 2% phosphorus; including.

The spray-dried granules preferably contain anionic surfactants other than alkyl sulfates. detergent builder 0 to about 40%, preferably about 2 to 40%; detergent builder about 10 to 80%; and about 1-15% soluble silicates.

The spray-dried granules preferably contain 010-16 linear alkylbenzene sulfones. and about 2-5% soluble sodium silicate. spray dried grains Preferably, carbonates, citrates, aluminosilicates, and and about 30 to 60% by weight of a detersive builder selected from the group consisting of include. They are more preferably sodium carbonate and/or sodium sulfate. about 5 to 60% by weight.

The spray-dried granules preferably have an average molecular weight of about 1.000 to 10.000. further comprises about 1 to 10% of a homopolymer or copolymer of acrylic acid or a salt thereof. . The granular detergent composition of the present invention preferably has a phosphorus content of less than 2.0, preferably or have no phosphorus content.

The following are separately preferred two lines for the alkyl sulfate particles in (a). The alkylbenzene sulfonate range is approximately 6-12% CLAS; 1-14 Rusulfate range is approximately 14-1B C alkyl sulfate 65-90%; polyethylene glycol ranges from molecular weight approximately 4,000 to 12 ,000 is about 5-15%; α-aminodicarboxylate range is about 1-3%. and most preferably monosodium glutamate and/or glutamine and the water and/or unreacted material range is about 2-8%. Ru.

Preferably, the ratio of LAS to alkyl sulfate is about 60:40 to 80. :20, most preferably 70:30.

The composition preferably comprises (c) about 2-40% by weight of the finished composition, preferably 5-40% by weight of the finished composition; 15% by weight detergent builder; or (C) about 3-10% detergent builder by weight of the finished composition. Also contains enoic acid and effective amounts of flavoring and enzymes (mixed on both types of granules) ). Enzymes, preferably proteases, lipases and/or cellulases, are Like perfume, it accounts for less than about 3% by weight of the composition.

The ratio of (a) to (b), respectively, is preferably about 50:50 to 1=99, and so on. The ratio is preferably about 30:70 to 1190.

■, Optional ingredients An example of a detergent surfactant that can be used here is Collie, published May 18, 1971. U.S. Pat. No. 3,579.454 (incorporated herein by reference), No. It is described in column 11, line 45 to column 13, line 64. A broader discussion of surfactants , U.S. Pat. No. 3,936,537 (incorporated herein by reference), inter alia It is included in column 11, line 39 to column 13, line 52. Anionic synthetic surfactant is particularly preferred.

Cationic surfactants can also be included in such finished detergent compositions. useful here A more complete disclosure of these and other cationic surfactants is available at , Camber U.S. Pat. No. 4,228,044, issued October 14, 1980. Specification (herein incorporated by reference).

Other optional ingredients that may be incorporated into the detergent composition of the present invention include Baskerville's special U.S. Pat. No. 3,936.537, column 19, line 53 to column 21, line 2. Detergent builders, chelating agents, bleaches listed on line 1 (incorporated herein by reference) Whitening agents, anti-fog and anti-corrosion agents, fragrance and color additives, and other optional ingredients Can be mentioned.

Chelating agents are described in Bush et al., U.S. Pat. No. 4,663,071, No. 17 It is also stated in Column line 54 to Column 18, Line 68 (incorporated here as a reference). Ru. Foam control agents are also optional ingredients and are described in Bartoletta et al. U.S. Pat. No. 4,136.045, issued January 23, 1979 to Rudo et al. Both are incorporated herein by reference). Cleanability builder Scarville Patent, Col. 13, Line 54 to Col. 16, Line 16 and May 5, 1987 No. 4,663,071 to Bush et al. (incorporated as a reference). Examples of such builders include , phosphate, aluminosilicate, silicate, carbonate, C~018 Alkyl monocarboxylates, polycarboxylates, polyphosphonates, and mixtures thereof.

All parts, percentages and ratios used herein are by weight unless otherwise specified. Ru.

Example I Alkyl sulfate particles are prepared according to the following recipe.

weight% C14-15 alkyl sodium sulfate 72.8 linear C alkylbenzene sulfo acid 1o, 612.3 Sodium sulfate L, S Polyethylene glycol (MW-8000) 11.3 glutamic acid monosodium um/disodium 2.1 Miscellaneous components 2.8 The detergent composition is prepared by first spray-drying an aqueous slurry having the following formulation. Prepare.

Product A Product B (Control) (Test) Linear C12,3 alkylbenzenesulfonate sodium 14.88 15.3 90 Sodium alkyl sulfate 8JII O, 0014-15 Sodium carbonate 10.98 12.02 Sodium polyacrylate (MW-4 500) 3.51 3.85 Sodium aluminosilicate 29.48 324 4 Sodium silicate (S i02: Na 201.6) 2.41 2.8 4 Fluorescent brightener OJG O,32 Sodium sulfate 21.58 22.79 Polyethylene glycol (MW-80 00) 1.62 0.99 Deaerator★ 0.11 0.12 Moisture 8.77 9.54 ★Dow Corning D C-544 spray drying is Single nozzle at 740 bonds/hr, inlet air temperature of about 390 and about 200 The drying process was carried out in a 10 foot diameter countercurrent spray drying tower with an exhaust temperature of 100 ft.

The final detergent composition is then prepared by mixing according to the following formulation: .

Spray-dried granules 91.2483.18 Citric acid 5.5 5.5 Fragrance OJO0,34 Protease/amylase 0.9 0.9 Ammonium sulfate 22 Alkyl sulfate particles 0 8.01 Foam inhibitor 0.0B 0.08 ★★Alcalase/Rapidase (Novo) Product A is a control prepared as described above. Represents a detergent composition. Product B is the same except for the formulation of mixed alkyl sulfate particles. Prepare as desired. It is a control and chemically equivalent washing product of the above two types in a home washing machine. When evaluated for two weeks by consumers (single product blind test), they Evaluated as equivalent.

conclusion Alkyl sulfate particles/spray-dried granules blends without any change in consumer perception. Enables the production of laundry detergents that are chemically equivalent to current detergent compositions. The mixture is Processing benefits of increased capacity and reduced organic emissions from spray drying towers give.

Example ■ Alkyl sulfate particles such as those described in Example I can be used in the detergent formulations described below. Ru.

weight% (Control) (Test) Linear Cl2J Sodium Alkylbenzenesulfonate 9.70 L29C Al Sodium kill sulfate 9.70 0.0014-15 Sodium carbonate 10 10 Sodium polyacrylate (MW4500) 3.2 3.2 Sodium aluminosilicate Thorium 26.9 28.9 Sodium silicate (SiO:Na O1,6) 2.2 2.2 Fluorescent brightener 0.27 0.27 Sodium sulfate 19.69 18.82 Polyethylene glycol (MW-80 00) 1.48 0.37 Deaerator★ 0.1 0.1 Moisture 8 7.73 mixture Citric acid 5.5 5.5 Fragrance 0.30 0.34 Protease/amylase 0.9 0.9 Ammonium sulfate 22 Alkyl sulfate particles 0 13.32 Foam inhibitor o, oe o, oe ★Dow Corning DC-544 ★★ Alcalase/Rapidase (Novo) These formulations are again chemically linked to each other. is equal to

Product C1 control is surfactant alkyl sulfate versus linear alkyl benzene sulfate. The product in Example I except that the ratio of honate was changed from 30:70 to 50:50. Product C was sprayed with additional alkyl sulfate. Spray drying also It can no longer be manufactured.

However, products, even Product A, can be manufactured with lower environmental impact. product The role is better when alkyl sulfates are the preferred surfactants. It is expected that this will be achieved.

Example ■ Alkyl sulfate particles such as those described in Example ■ can be used in the following detergent formulations: Ru.

weight% (Control) (Test) Linear CL2J sodium alkylbenzenesulfonate 'lJ'7mu 19.09 I7 ．． 90C Sodium alkyl sulfate 8.18 014-15 Sodium carbonate 1010 Sodium polyacrylate (MW4500) 3.2 L2 sodium aluminosilicate Lium 26.9 26.9 Sodium silicate (SLO: Na2O1,6) 2 ．． 2 2-2 Fluorescent brightener 0.27 0.27 Sodium sulfate 11.82 11.06 Polyethylene glycol (MW-80 00) t-+g (1,55 deaerator” 0.1 0.1 Citric acid 5.5 5.5 Fragrance 0.30 044 Protease/amylase 0.9 0.9 Ammonium sulfate 22 Alkyl sulfate particles 0 11.24 Foam inhibitor 0.0B 0.06 ★Dow Corning DC-544 ★★ Alcalase/Rapidase (Novo) These formulations are chemically equivalent to each other. It is. Product E, the control, contains all surfactants (linear alkylbenzene sulfur) in the formulation. Honate plus alkyl sulfate) increased from 19.40% to 27.27%. Same as Product A1 control in Example I except that. Product E is for safety and the environment. The reason for the effect of , agglomeration and caking) can no longer be produced by spray drying. However However, product F is a combination of spray drying and mixing of alkyl sulfate particles. Therefore, it can be manufactured. This product is better than product A for surfactant-sensitive soils. It is expected that this will be achieved.

Example ■ The detergent compositions described below are prepared in a 10 foot diameter countercurrent qI fog drying tower.

Control test Sodium C alkylbenzenesulfonate 11.45 11.2712.3 CI4.5 Sodium alkyl sulfate 11.45 0 Sodium aluminosilicate (Hydration, water 20%) 28.90 28.90 Sodium carbonate 17.0G 17 ．． 00 Sodium silicate (SI O2: N a 20 ratio 1.6) 5.35 5.35 Sodium polyacrylate (MW■4500) 3.5 8.5 Poly Ethylene glycol (MW-8000) 1.2 0 Fluorescent brightener 0.22 0 ．． 22 Tallow fatty acid 1.28 1.28 Water, sodium sulfate, balance, balance Cake grade results Force to break cake under 20 lbs load 5.2 2J (bond/sq. ) Water by analysis 11.4 11.1 The improved physical properties (lower cake grade) of the test racks are due to the surface activity of the spray-dried granules. Demonstrates the benefit of minimizing sex agent content. This means that the burr imparting aid , polyethylene glycol (MW-8000) is the most widely used surfactant, This is true even if it is removed together with lukylsulfate.

Example V The preparation of highly active detergent materials suitable for granulation into free-flowing granules is as follows.

Device 014-1. in acid form using a falling film type S03 reactor. alkyl sulfate generate. The acid was supplied by Chemiton Medium Corporation of Seattle, Washington. Supplies the highly active neutralization system provided. This custom made neutralization system introduces a cooling heat exchanger, a recirculation pump suitable for highly viscous fluids, and reactants. It consists of a recirculation loop containing a high shear mixer.

To achieve the very low water content required for free-flowing highly active particles, neutralizing 70% hydroxyl rather than the 38-50% commonly used in neutralization loops. modified to handle sodium chloride melts. This modification reduces the 70% caustic to approximately Hot water jacket to maintain above caustic melting point of 155″F (68,3°C) and electrical heating of the caustic feed system.

Another necessary modification is to neutralize the polyethylene glycol at the discharge side of the high shear mixer. It is equipped with a metering system for injecting into the pipe. Presence of polyethylene glycol facilitates pumping into the base recirculation loop and reduces stickiness of the finished material. Decrease. Polyethylene glycol having a molecular weight of about 8000 is polyethylene Approximately 1 part glycol 8000 to 10 parts sodium 014-15 alkyl sulfate active ingredient part as a melt (approximately 160 parts or 71.1°C).

operation At startup, the neutralization loop is filled with water and the hot water is passed through the heat exchanger and into the recirculation loop. By using the system in a double-walled vibrator consisting of Maintain at 82.2-110°C. Start recirculation pump and high shear mixer. move.

70% sodium hydroxide and C alkyl sulfate 14-15 are introduced into a high shear mixer and allowed to react. Sodium hydroxide and C alkyl sulfur Metering the acid, just 14 to 15 minutes or allow excess sodium hydroxide. Back the material displaced from the recirculation loop. Discharge through pressure control valve.

As operation continues, water is displaced from the loop and the 014-15 alkyl sulfate sodium The concentration of um increases to over 70% of the active ingredient. The desired amount of highly active, low moisture material is produced. Continue the operation until it is completed. The reactant feed is then stopped and the reaction loop is flushed with hot water. Wash with

result The prepared molten paste was cooled and manually ground to form a free-flowing product with the following composition: As a granular product.

014-15 Sodium alkyl sulfate 74.9% polyethylene glycol 80 00 8.5 Wed 9.1 Sodium hydroxide 0.6 Unreacted substances/miscellaneous components 6.9 Example■ Alkyl sulfate particles are prepared according to the following recipe.

Nominal weight% C14-15 alkyl sodium sulfate 75.0 Water 11.0 Sodium sulfate 2.5 Polyethylene glycol (MW-8000) 7.5 Miscellaneous components 4.0 The detergent composition is prepared by first spray-drying an aqueous slurry having the following formulation. Prepare.

Village! gloss (Control) (Test) Linear Cl2J sodium alkylbenzene sulfonate 11.90 13.25 Sodium C alkyl sulfate 11.02 0.0014-15 Sodium carbonate 18.2L 18.87 Sodium polyacrylate (MW-4 500) 3.34 4.12 Sodium aluminosilicate 2349 31.4 0 Sodium silicate (Sio: Na2O1,6) 1.82 1.90 Fluorescence increase Whitening agent OJI O, 2g Sodium sulfate 15.08 2G, 94 polyethylene glycol (MW-80 00) 0.94 042 Sodium tallow soap 1.03 1.3B Moisture - 7,967,56 Spray drying with a single nozzle at 740 posid/hr, inlet air temperature below about 390 and in a 10-foot diameter countercurrent spray drying tower with an exhaust temperature of about 200 mm. cormorant.

The final detergent composition is then prepared by mixing according to the following formulation: .

Spray-dried granules 100.00 B4.37 alkyl sulfate particles 0 1 5.63 Product A represents a control detergent composition prepared as described above. Product B is , prepared in the same manner except for the amount of mixed alkyl sulfate particles. It is a contrast Chemically equivalent alkyl sulfate particles/spray-dried granulate blends are It enables the production of laundry detergents that are chemically equivalent to synthetic products. Mixing increased volume provides processing advantages in quantity and reduced organic emissions from the spray drying tower.

international search report PCT/US 92105659 Continuation of front page (81) Specified interval EP (AT, BE, CH, DE.

DK, ES, FR, GB, GR, IT, LU, MC, NL, SE), 0A (BF , BJ, CF, CG, CI, CM, GA, GN, ML, MR, SN, TD, TG. ), AU, BB, BG, BR, CA, C3, FI, HU, JP.

KP, KR, LK, MG, MN, MW, No, PL, RO, RU , S.D.

Claims (22)

[Claims] 1. (a) less than 2% alkyl sulfate by weight of the spray-dried granulate; Anionic surfactant other than rusulfate 0-40%; detergency builder 10-8 0%, preferably 2-40%; and 1-15% soluble silicate. -spray dry; (b) The alkyl sulfate particles are produced by a process including highly active continuous neutralization ( Here, the particles contain 1 alkyl sulfate by weight of the alkyl sulfate particles. C12-18 als ethoxylated with 0 to 4 moles of ethylene oxide per mole (contains 60-99% kill sulfate); (c) combining said spray-dried granules with said alkyl sulfate particles from 10;90 to 9; Mix in a 9:1 ratio A method for producing a granular detergent composition, characterized by: 2. The anionic surfactant in the spray-dried granules is a C10-16 linear alkali 2. The method according to claim 1, wherein the salt is a salt of killbenzenesulfonic acid. 3. The spray-dried granules are carbonate, citrate, aluminosilicate. 30-60 weight detergency builder selected from the group consisting of , and mixtures thereof. %. 4. The spray-dried granules contain 5-50% by weight of sodium aluminosilicate and charcoal. Claims 1 to 3 containing 5 to 60% by weight of sodium acid and/or water-soluble inorganic salt. The method according to any one of the above. 5. Claims 1 to 3, wherein the slurry further comprises 2-5% soluble sodium silicate. 4. The method according to any one of 4. 6. The highly active continuous neutralization (a) In a continuous neutralization system, C12-18 alkyl sulfuric acid is converted into 62% hydroxide. % or more of a sodium hydroxide solution to produce a neutralized product; (b) the continuous neutralization system has a molecular weight of 2,000 to 5 when producing the neutralized product; 0,000 polyethylene glycol, melting point greater than 120°F (48.9°C) has the formula R(OC2H4)nOH, where R is a C12-18 alkyl group or C 8-16 alkylphenol group, n is 9-80). on surfactants, or mixtures thereof (where the additives of step (b) The weight ratio of the product of step (a) to the product of step (a) is from 1:5 to 1:20) 6. The method according to any one of claims 1 to 5, carried out by a method comprising: 7. The alkyl sulfate particles are C10-16 linear alkylbenzene sulfonate. Cl0-16 linear alkylbenzene sulfone containing 4-25% A method according to any one of claims 1 to 6, wherein an acid is also added to the continuous neutralization system. . 8. The ingredients of the detergent composition are not kneaded into the continuous neutralization system; Claims 1 to 7, wherein the system is substantially free of additional coarse material and does not include an airtight kneader. The method according to any one of the above. 9. Essentially no detersive builders or additional organic substances are present in the continuous neutralization system. 9. The method according to any one of claims 1 to 8, wherein the method is not supplied to a. 10. the neutralization product has 12% by weight or less of water; and the continuous neutralization system a continuous neutralization loop; and the additive in step (b) has a molecular weight of 3,000 to 20 ,000 polyethylene glycol; and the additive of step (b) versus step (a ) is 1:10. the method of. 11. The additive of step (b) is molten polyethylene having a molecular weight of 8,000. 11. The method according to any one of claims 1 to 10, wherein the glycol is a glycol. 12. Claims 1 to 3, wherein R is a C12-18 alkyl group and n is 12-30. 12. The method according to any one of 11. 13. The highly active continuous neutralization (a) In a highly active continuous neutralization loop, the alkyl sulfate in acid form is 30 to 75% by weight and present in a stoichiometric amount or a slight stoichiometric excess. reacting with a sodium hydroxide solution present to form a neutralized product; (b) The particles formed from the product of step (b) have an α-aminodicarboxylic acid salt of 0. The continuous high activity neutralization loop contains 2 to 15% by weight of the neutralization product. During production, glutamic acid, aspartic acid, aminomalonic acid, aminoadipic acid , and α- selected from the group consisting of 2-amino-2-methylpentanedioic acid. A method consisting of adding aminodicarboxylic acids, or their alkali metal salts 13. The method according to any one of claims 1 to 12, carried out by. 14. Adding an alkali metal salt of glutamic acid or aspartic acid to the neutralization loop and the alkali metal hydroxide solution contains 62 to 73% by weight of hydroxide; 14. A method according to any one of claims 1 to 13. 15. Monosodium glutamate or disodium glutamate 1 to 10 times % of sodium hydroxide into the neutralization loop; and the alkali metal hydroxide solution 15. The method according to any one of claims 1 to 14. 16. When the neutralization product is produced in the neutralization loop, a molecular weight of 2,000 to 50,000 is added. Polyethylene glycol of formula R ( OC2H4)nOH (wherein R is a C12-18 alkyl group or a C8-16 alkyl group) (kylphenol group, n is 9 to 80) ethoxylated nonionic surfactant or mixtures thereof in a weight ratio of 1:5 to 1:20 with the components of step (a). 16. A method according to any one of claims 1 to 15, comprising the additional step of adding. 17. The polyethylene glycol has a molecular weight of 8000, and the polyethylene glycol has a molecular weight of 8000, and 17. The weight ratio of glycol to component of step (a) is 1:10. The method described in any one of the above. 18. The molten neutralized product is simultaneously cooled, extruded and cut or crushed to form detergent granules. 18. The method of any one of claims 1-17, further comprising filiation. 19. Cooling the product of step (b) on a chill roll until solidification; The product is separated from the chill roll and flaked into detergent flakes with a moisture content of 5%. Claims 1-1 further comprising drying the detergent particles to less than 100 ml and mechanically grinding the detergent particles into detergent particles. 8. The method according to any one of 8. 20. The alkyl sulfate particles are sodium C14-16 alkyl sulfate. 20. A method according to any one of claims 1 to 19, comprising 70-90%. 21. Claims 1 to 20, wherein the phosphorus content of the granular detergent composition is less than 2.0%. The method according to any one of the above. 22. 3-10% citric acid and effective amounts of fragrances and enzymes by weight of the finished composition. mixing the alkyl sulfate particles and the spray-dried granules; said ratio of rusulfate to spray-dried granules is from 30:70 to 10:9, respectively; 22. The method according to any one of claims 1 to 21, wherein 0.