JP2020097664A - Manufacturing method of powdered detergent - Google Patents

Abstract

PROBLEM TO BE SOLVED: To produce a powder detergent having excellent fluidity, solubility and rinsability. SOLUTION: (A) α-sulfofatty acid ester salt: 0.1 to 5% by mass (B) Surfactant other than the component (A): 0.1 to less than 25% by mass (C) Water-insoluble component: 0 A method for producing a powder detergent containing 1 to less than 20% by mass, wherein a solid α-sulfofatty acid ester salt is added during stirring granulation. [Selection diagram] None

Description

The present invention relates to a method for producing a powder detergent having excellent fluidity, solubility and rinsability.

Generally, as a method for producing a detergent containing an α-sulfofatty acid ester salt, a detergent composition containing an α-sulfofatty acid ester salt is kneaded, mixed, ground, and then coated with a water-insoluble powder. (See, for example, Patent Documents 1 to 4). However, there is no description about the improvement of solubility when a surfactant other than the α-sulfofatty acid ester salt is mainly used, and the content of a water-insoluble component such as aluminosilicate is 20% by mass or more. The water-insoluble component may remain in the clothes after washing and may cause turbidity during rinsing, which may increase the amount of water required for rinsing, increase the number of rinses, and make rinsing complicated. Not preferable. On the other hand, if the content of the water-insoluble component is reduced in order to reduce turbidity during rinsing and facilitate rinsing (improving rinsing properties), the fluidity of the powder detergent will deteriorate. Therefore, a powder detergent having excellent solubility, rinseability and fluidity is desired.

JP, 9-87700, A JP, 2010-248382, A JP, 2003-105378, A International Publication No. 2004/111166

The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a method for producing a powder detergent excellent in solubility, rinseability, and fluidity.

As a result of intensive studies, the present inventors have found that the following method for producing a powder detergent can solve the above problems.
That is, the present invention has the following aspects.
[1] (A) α-sulfofatty acid ester salt: 0.1 to 5% by mass
A method for producing a powder detergent containing (B) a surfactant other than (A) component: 0.1 to less than 25% by mass (C) a water-insoluble component: 0.1 to less than 20% by mass,
Characterized in that a solid α-sulfo fatty acid ester salt is added during stirring granulation,
Powder detergent manufacturing method.
[2] The method for producing a powder detergent according to [1], wherein the component (C) is zeolite.
[3] The method for producing a powder detergent according to [1] or [2], wherein the component (B) is at least one selected from LAS, soap, and nonionic surfactant.

ADVANTAGE OF THE INVENTION According to this invention, the manufacturing method of the powder detergent excellent in detergency, fluidity, solubility, and rinseability can be provided.

[Powder detergent]
The powder detergent produced by the present invention contains the following components (A) to (C).

≪(A) ingredient≫
The component (A) is an α-sulfofatty acid ester salt.

The α-sulfo fatty acid ester salt is a kind of anionic surfactant and functions as a cleaning component. The α-sulfo fatty acid ester salt is represented by the following general formula (a1).

[In the formula (a1), R ¹ is a hydrocarbon group having 8 to 18 carbon atoms, R ² is a hydrocarbon group having 1 to 6 carbon atoms, and M is a counter ion. ]
In the formula (a1), the hydrocarbon group for R ¹ may be linear or branched, or may have a cyclic structure. Among them, the hydrocarbon group of R ¹ is preferably an aliphatic hydrocarbon group, more preferably a linear or branched alkyl group, or a linear or branched alkenyl group, and a linear alkyl group or a linear alkenyl group. More preferred are groups.
The carbon number of R ¹ is 8 to 18, preferably 10 to 18, more preferably 10 to 16, and further preferably 14 to 16. It is preferable in terms of detergency that the carbon number of R ¹ is in the range of the lower limit value or more and the upper limit value or less.
In the formula (a1), the hydrocarbon group represented by R ² may be linear or branched, and may have a cyclic structure. Among them, the hydrocarbon group of R ² is preferably an aliphatic hydrocarbon group, more preferably a linear or branched alkyl group or a linear or branched alkenyl group, and a linear alkyl group or a linear alkenyl group. More preferred are groups.
The carbon number of R ² is 1 to 6, and preferably 1 to 3.
Examples of the hydrocarbon group for R ² include a methyl group, an ethyl group, an n-propyl group, and an isopropyl group. From the viewpoint of further enhancing the detergency, a methyl group, an ethyl group, and an n-propyl group are preferable, and a methyl group. Is more preferable.
In the formula (a1), M is a counter ion as long as it can form a water-soluble salt with R ¹ CH(COOR ² )SO ₃ ⁻ . Examples of the counter ion include alkali metal ions, protonated amines, ammonium and the like.
Examples of the alkali metal that can be the counter ion include sodium and potassium. The amine that can be the counterion may be any of primary to tertiary, and the total carbon number is preferably 1 to 6. The amine may have a hydroxy group, and preferably has a hydroxy group because the solubility of the detergent in water is increased under low temperature conditions (5°C or lower). Examples of such amines include alkanolamines, and the alkanol group preferably has 1 to 3 carbon atoms. Examples of the alkanolamine include monoethanolamine, diethanolamine, triethanolamine and the like. Among them, M is preferably an alkali metal ion.

The content of the α-sulfofatty acid ester salt of the powder detergent produced in the present invention is 0.1 to 5% by mass, preferably 0.5 to 4% by mass, and more preferably 1 to 3% by mass.
When the content of the α-sulfo fatty acid ester salt is not more than the above upper limit, the fluidity of the powder detergent and the dispersibility in water are easily improved.
When the content of the α-sulfo fatty acid ester salt is at least the above lower limit, the detergency is likely to be improved.
The α-sulfo fatty acid ester salt is produced by a conventionally known production method. Examples of the method for producing the α-sulfo fatty acid ester salt include the production method described in JP2011-121996A.

≪(B) ingredient≫
The component (B) is a surfactant excluding the α-sulfofatty acid ester salt which is the component (A), and includes an anionic surfactant (B1), a nonionic surfactant (B2), and a cationic surfactant (B3). , At least one component selected from an amphoteric surfactant (B4) and a semipolar surfactant (B5), among which an anionic surfactant (B1) and a nonionic surfactant (B2) are selected. At least one component is preferred.
The content of the component (B) in the powder detergent produced in the present invention is 0.1 to less than 25% by mass, preferably 2 to 20% by mass, more preferably 5 to 18% by mass.

(B1) Anionic Surfactant Examples of the anionic surfactant include the following.
(1) A straight-chain or branched-chain alkylbenzene sulfonate (LAS or ABS) having an alkyl group having 8 to 18 carbon atoms.
(2) Alkane sulfonate having 10 to 20 carbon atoms.
(3) α-Olefin sulfonate (AOS) having 10 to 20 carbon atoms.
(4) Alkyl sulfate or alkenyl sulfate (AS) having 10 to 20 carbon atoms.
(5) Any of alkylene oxides having 2 to 4 carbon atoms, or ethylene oxide and propylene oxide (molar ratio EO/PO=0.1/9.9 to 9.9/0.1), an average of 0.5 to An alkyl (or alkenyl) ether sulfate (AES) having a linear or branched alkyl (or alkenyl) group having 10 to 20 carbon atoms added with 10 mol.
(6) Any of alkylene oxides having 2 to 4 carbon atoms, or ethylene oxide and propylene oxide (molar ratio EO/PO=0.1/9.9 to 9.9/0.1), on average 3 to 30 mol An alkyl (or alkenyl) phenyl ether sulfate having an added linear or branched alkyl (or alkenyl) group having 10 to 20 carbon atoms.
(7) Any of alkylene oxides having 2 to 4 carbon atoms, or ethylene oxide and propylene oxide (molar ratio EO/PO=0.1/9.9 to 9.9/0.1), an average of 0.5 to An alkyl (or alkenyl) ether carboxylate having a linear or branched alkyl (or alkenyl) group having 10 to 20 carbon atoms added with 10 mol.
(8) Alkyl polyhydric alcohol ether sulfate such as alkyl glyceryl ether sulfonic acid having 10 to 20 carbon atoms.
(9) Long chain monoalkyl, dialkyl or sesquialkyl phosphates.
(10) Polyoxyethylene monoalkyl, dialkyl or sesquialkyl phosphate.
(11) Soap.
Examples of the soap include alkali metal salts of higher fatty acids having an average carbon number of fatty acids of 10 to 20, preferably 12 to 18 carbons, and more preferably sodium or potassium salts. The alkyl group of the fatty acid is preferably primary. The soap may have a single chain length or a mixture of two or more chain lengths.
Examples of the salt in the anionic surfactant include alkali metal salts such as sodium and potassium, amine salts and ammonium salts.
The anionic surfactants may be used alone or in combination of two or more.
The content of the component (B1) is determined in consideration of the dosage form of the powder detergent, the type of surfactant and the like.
For example, the content of the anionic surfactant excluding the component (A) is preferably 1 to less than 20 mass% and more preferably 10 to 19 mass% with respect to the total mass of the powder detergent.
When the content of the anionic surfactant is not more than the above upper limit, the fluidity of the powder detergent and the dispersibility in water are likely to be improved.
When the content of the anionic surfactant is at least the above lower limit value, the detergency will be easily improved.

(B2) Nonionic Surfactant The nonionic surfactant is not particularly limited as long as it has been conventionally used for detergents, and examples thereof include the following.
(1) An alkylene oxide having 2 to 4 carbon atoms is added to an aliphatic alcohol having 6 to 22 carbon atoms, preferably 8 to 18 carbon atoms, on average 3 to 30 mol, preferably 3 to 20 mol, more preferably 5 to 20 mol. Polyoxyalkylene alkyl (or alkenyl) ether. Among these, polyoxyethylene alkyl (or alkenyl) ether and polyoxyethylene polyoxypropylene alkyl (or alkenyl) ether are preferable. Examples of the aliphatic alcohol used here include primary alcohols and secondary alcohols. Moreover, the alkyl group may have a branched chain. The aliphatic alcohol is preferably a primary alcohol.
(2) Polyoxyethylene alkyl (or alkenyl) phenyl ether.
(3) A fatty acid alkyl ester alkoxylate in which an alkylene oxide is added between ester bonds of a long-chain fatty acid alkyl ester.
(4) Polyoxyethylene sorbitan fatty acid ester.
(5) Polyoxyethylene sorbit fatty acid ester.
(6) Polyoxyethylene fatty acid ester.
(7) Polyoxyethylene hydrogenated castor oil.
(8) Glycerin fatty acid ester.
As the nonionic surfactant, any one kind may be used alone, or two or more kinds may be used in combination.
The content of the nonionic surfactant is determined in consideration of the dosage form of the detergent, the type of nonionic surfactant, and the like.
For example, the content of the nonionic surfactant is preferably 0.1 to 3% by mass, more preferably 0.5 to 2% by mass, based on the total mass of the powder detergent.
When the content of the nonionic surfactant is not more than the above upper limit value, the fluidity of the powder detergent and the dispersibility in water are likely to be improved. When the content of the nonionic surfactant is at least the above lower limit value, the detergency is easily improved.
The component (B) is preferably at least one selected from LAS, soap and nonionic surfactants.

≪(C) ingredient≫
The component (C) is a water-insoluble component.
In the present specification, the “water-insoluble component” means a component having a solubility of 0.1 g or less in 100 mL of ion-exchanged water at 25°C.
As the component (C), aluminosilicates such as zeolite, natural or synthetic montmorillonite, beidellite, nontronite, saponite, sauconite, hectorite, clay minerals of the smectite group such as stevensite, vermiculite, synthetic fluoromica (for example, , Na-type synthetic mica, Li-type synthetic mica) and the like can be used. Further, it is possible to use a high metal ion substituted clay mineral in which the above clay mineral is ion-exchanged to improve the swelling power. Of these, zeolite and bentonite are preferable, and zeolite is more preferable, because they have a chelating effect and the like.

The aluminosilicate may be crystalline or amorphous (amorphous). From the viewpoint of cation exchange ability, crystalline aluminosilicate is preferable. Examples of the crystalline aluminosilicate include A-type, X-type, Y-type, P-type zeolite and the like, and any of them can be used.
Bentonite has montmorillonite as a main component.
As the component (C), any one type may be used alone, or two or more types may be used in combination.
In the powder detergent, a part of the component (A) is mixed with water and, if necessary, other components to form a slurry, which is spray-dried into spray-dried particles. The spray-dried particles are kneaded and pulverized as they are or with the addition of water and, if necessary, other components, and the resulting particles are blended into a powder detergent.
The content of the component (C) is 0.1 to less than 20% by mass, preferably 1 to 16% by mass, and more preferably 2 to 12% by mass, based on the total mass of the powder detergent.
When the content of the component (C) is at most the above upper limit value, the rinsability will be easily improved.
When the content of the component (C) is at least the above lower limit, it becomes easy to improve the detergency.
The average particle size of the component (C) is preferably 0.1 to 200 μm, more preferably 1 to 10 μm. The average particle diameter can be measured by a laser light scattering method (for example, a particle size distribution measuring device (LDSA-3400A (17ch), manufactured by Tohnichi Computer Applications Co., Ltd.)).

<Arbitrary ingredients>
The powder detergent produced by the present invention, in addition to the components (A) to (C), a bleaching agent such as sodium percarbonate, a bleaching activator such as NOBS, an alkali builder, and the like in addition to the components (A) to (C). Inorganic salts, solvents, preservatives, optical brighteners, anti-staining agents, foam control agents, viscosity reducing agents, solubilizers, enzymes, flavoring agents, coloring agents, emulsifying agents, extracts, pH adjusting agents. Ingredients such as fragrances and the like may be included in the conventional cleaning agents.
Examples of the pH adjuster include acidic compounds such as sulfuric acid and hydrochloric acid; alkanolamines such as monoethanolamine, diethanolamine and triethanolamine, and alkaline compounds such as sodium hydroxide and potassium hydroxide. Among them, as the pH adjuster, sulfuric acid, sodium hydroxide, potassium hydroxide, and alkanolamine are preferable, because sulfuric acid, sodium hydroxide, potassium hydroxide, and alkanolamine are preferable, because it is easy to maintain the pH of the cleaning liquid before and after the immersion of the object to be washed. Is more preferable. The pH adjusters may be used alone or in combination of two or more.

As the alkali builder, conventionally known ones can be used, and examples thereof include alkali metal carbonates or hydrogen carbonates, alkali metal silicates, and amines.
Examples of the alkali metal carbonate include sodium carbonate, potassium carbonate, sodium potassium carbonate, sodium sesquicarbonate and the like.
Examples of the alkali metal hydrogencarbonate include sodium hydrogencarbonate and potassium hydrogencarbonate.
Examples of the alkali metal silicate include sodium silicate, layered sodium silicate, sodium metasilicate, sodium orthosilicate and the like.
Examples of amines include monoethanolamine, diethanolamine, triethanolamine and the like.
Silicates generally have a higher pH than carbonates, and carbonates generally have a higher pH buffering capacity than silicates. Therefore, it is preferable that the cleaning agent contains both carbonate and silicate.
The total content of the components (A) to (C) and the optional components does not exceed 100% by mass.

The powdered detergent produced by the present invention may be processed into a solid detergent in the form of sheet, tablet, flake, granule or the like by subjecting it to known processing techniques.
Although the average particle diameter of the powder detergent is not particularly limited, for example, 200 to 1500 μm is preferable, 250 to 1000 μm is more preferable, and 300 to 700 μm is further preferable.
When the average particle diameter is not more than the above upper limit value, it is easily dissolved in water.
If the average particle diameter is not less than the above lower limit value, it is difficult to cause dusting during use.
The average particle size of the powder detergent produced in the present invention is a mass-based median size (particle size at which the cumulative value of mass frequency is 50% by mass). For example, it can be measured by [Method of measuring average particle diameter by sieving method] described in paragraph 0008 of JP-A-2018-30925.

The bulk density of the powder detergent produced in the present invention is preferably 0.5 to 1.3 g/cm ^{3, and} more preferably 0.6 to 1.1 g/cm ³ .

[Method of manufacturing powder detergent]
The method for producing a powder detergent of the present invention is characterized in that a solid α-sulfofatty acid ester salt is added at the time of granulation with stirring. The solid α-sulfofatty acid ester salt added during the stirring granulation may be the whole or a part of the component (A). The solid state can be used without particular limitation as long as it is in a solid state such as powder, granules, flakes, sheets, tablets and the like.
In addition, in other steps, it is manufactured by a conventionally known manufacturing method such as a powder detergent.
As a method for producing a powder detergent, a dry blending method in which each raw material is powder-mixed, a dry granulation method in which the powder raw material is granulated while flowing, and a liquid binder is sprayed and granulated while flowing the powder raw material Agitation granulation method, extrusion granulation method of kneading the raw material and extruding it with an extruder, pulverization granulation method of kneading the raw material and crushing it, spray drying method of spray drying a slurry containing the raw material, etc. Are listed.
As a preferred manufacturing method, a slurry containing raw materials is spray-dried to prepare a spray-dried powder (spray-drying step), and then a nonionic surfactant among the components (A) and (B) is added to the spray-dried powder. And a method of stirring granulation by adding (stir granulation step). Then, if necessary, the powder raw materials may be mixed (powder mixing step).
The mass ratio (A/B) of the component (A) and the component (B) added during the stirring granulation is preferably 10/1 to 1/10.

The stirring granulator used in the present invention includes, for example, a Loedige mixer, a high speed mixer, a Henschel mixer, a Nauta mixer, a Nugra machine, a Shugi mixer, a plowshare mixer, a Spartan mixer, a pug mixer, a turbulator, Examples thereof include a horizontal cylindrical mixer, a kneading extruder, a horizontal continuous kneader, and a closed consolidation apparatus.
As the granulation conditions, after adding components (A) to (C) and other optional components to the mixer while sequentially stirring, further stirring is performed at 100 to 4000 rpm for 5 to 30 minutes. Thus, the powder detergent of the present invention can be prepared.

The stirring Froude number in the stirring granulation of the present invention may be, for example, 0.5 to 25, or 1 to 20. The stirring Froude number (Fr) is defined by the following formula (1), for example.

Fr=V/[(R×g) ^0.5 ] (1)
V: peripheral speed (m/s) of the tip of the stirring blade
R: Radius of rotation of stirring blade (m)
g: Gravitational acceleration (m/s ² )

[How to use powder detergent]
The method of using the powder detergent (that is, the washing method) is the same as the conventionally known washing method (laundry method) for clothing.
As a cleaning method, for example, a powder detergent is dispersed in water so as to have an arbitrary concentration to form a cleaning liquid, and the object to be cleaned is immersed in the cleaning solution for an arbitrary time, and then the object to be cleaned is rinsed with water (immersion). Washing method).
The content of the powder detergent in the cleaning liquid is appropriately determined according to the composition and dosage form of the powder detergent. For example, the content of the powder detergent in the cleaning liquid is preferably 0.1 to 0.6% by mass, more preferably 0.4 to 0.6% by mass, and further preferably 0.5% by mass.
If it is less than the above lower limit, the cleaning effect may be lowered, and if it exceeds the above upper limit, undissolved residue may occur in the cleaning liquid or rinsing may be complicated.
The pH (25° C.) of the cleaning liquid is not particularly limited, but is preferably 8 to 10.5. When it is at least the above lower limit value, the rinsability is easily improved, and when it is at most the above upper limit value, the detergency is easily improved.

As a cleaning method, a method of manually rubbing the object to be cleaned while immersing the object to be cleaned in the cleaning liquid can be mentioned. In this cleaning method, the content of the powder detergent in the cleaning liquid is the same as the content of the powder detergent in the cleaning liquid in the immersion cleaning method.
Alternatively, as a cleaning method, a method in which a cleaning liquid and an object to be cleaned are put into a washing machine and the cleaning liquid is stirred can be mentioned. In this cleaning method, the content of the powder detergent in the cleaning liquid is preferably 0.05 to 0.2% by mass, more preferably 0.1 to 0.2% by mass. If it is at least the above lower limit value, the detergency will be easily improved, and if it is at most the above upper limit value, the rinsability will be easily improved.
The material to be washed is not particularly limited, but for example, clothing, cloth, sheets, curtains and other fiber products are preferable. This is because the cleaning agent of the present invention can exert excellent cleaning power on textile products.

As described above, the powder detergent produced by the present invention contains the component (A) in a specific content, the component (B), and the component (C) in a specific content. Therefore, it is excellent in powder fluidity, solubility, rinseability, and detergency.

Hereinafter, the present invention will be described in more detail with reference to examples, but the present invention is not limited to these examples.
The composition (content (% by mass)) of the powder detergent of each example is shown in Tables 1 to 3.
In the table, when there is a blank compounding ingredient, the compounding ingredient is not compounded.
In the table, "balance" means the balance that is added so that the total amount of all the components included in the powder detergent is 100% by mass.
The raw materials used in this example are as follows.

≪(A) ingredient≫
A-1: α-sulfofatty acid methyl ester salt (in the formula (a1), R ¹ is an alkyl group having 14 carbon atoms, and R ² is a methyl group: an α-sulfofatty acid ester salt: R in the formula (a1) A mixture of α-sulfo fatty acid ester salt in which ¹ is an alkyl group having 16 carbon atoms and R ² is a methyl group = 85:15 (mass ratio)) (trade name: MIZULAN P-82, Global Ecochemicals Malaysia Co., Ltd. Made).

≪(B) ingredient≫
B-1: sodium linear alkylbenzene sulfonate (LAS-Na) (alkyl group carbon number: 10 to 14) (trade name: Ripon LS-250, Lion Corporation).
B-2: soap: fatty acid sodium having 12 to 18 carbon atoms (manufactured by Lion Corporation, pure content: 67%, titer: 40 to 45° C., fatty acid composition: carbon number C12: 11.7%, carbon number C14: 0.4%, carbon number C16: 29.2%, carbon number C18F0* (stearic acid): 0.7%, C18F1* (oleic acid): 56.8%, carbon number 18F2* (linoleic acid): 1 .2%, molecular weight: 289). *F0, F1 and F2 are the number of double bonds in the fatty acid.
B-3: Alcohol having an alkyl group having 12 to 16 carbon atoms (C12 to 16 alcohol manufactured by P&G Chemicals, trade name: CO-1214) having an average ethylene oxide content of 15 mol (90% pure, manufactured by Lion Corporation) )
B-4: Leox CL-90 (manufactured by Lion Specialty Chemicals Co., Ltd.)
B-5: Leox CL-70 (manufactured by Lion Specialty Chemicals Co., Ltd.)
≪(C) ingredient≫
C-1: A-type zeolite (trade name: Shilton B (containing 20% by mass of water in the powder), manufactured by Mizusawa Chemical Co., Ltd.).
C-2: Bentonite (trade name: bentonite, manufactured by AMCOL).

≪Arbitrary ingredients≫
-PAS: polyacrylic acid sodium salt (molecular weight: 2000) (trade name: Acusol 420N, manufactured by Dow Chemical).
-HIDS: Hydroxyiminodisuccinate 4 sodium (brand name: HIDS, manufactured by Nippon Shokubai Co., Ltd.).
-Na carbonate: sodium carbonate (trade name: soda ash (grain ash), manufactured by Tosoh Corporation).
-Na silicate: sodium silicate (trade name: powdered sodium silicate No. 2, manufactured by Nippon Kagaku Kogyo Co., Ltd.).
-Na sulphate: sodium sulphate (trade name: Glauber's salt, manufactured by Nippon Chemical Industry Co., Ltd.).
-Na sulfite: sodium sulfite (trade name: sodium sulfite, manufactured by Nippon Chemical Industry Co., Ltd.).
CMC: sodium carboxymethyl cellulose (trade name: CMC Daicel, product number: 1105 manufactured by Daicel Chemical Industries, Ltd.).
Enzyme A: Proteolytic enzyme (trade name: Deozyme, manufactured by Novozymes).
Enzyme B: Complex enzyme (trade name: SuperioR, manufactured by Novozymes).
Enzyme C: complex enzyme (trade name: SmartR, manufactured by Novozymes).
Enzyme D: Complex enzyme (trade name: CleanR, manufactured by Novozymes).
-Fluorescent brightening agent: Chinopearl CBS-X (trade name, manufactured by BASF Japan Ltd., distyryl biphenyl derivative, water-soluble fluorescent agent).
-Fragrance: The fragrance composition A shown in [Table 11] to [Table 18] of JP-A-2002-146399.

<Examples 1 to 24, Comparative Examples 1 to 3>
In Examples 1 to 24 and Comparative Example 3, among the components of the powder detergents listed in Tables 1 to 3, (B) component (B-1 or B-2 of (B) component), (C) component, A detergent slurry was prepared using sodium silicate and sodium sulfate so that the solid content was 60% by mass at a temperature of about 70°C. The order of adding the raw materials was not particularly limited. The slurry was stirred at 70° C. for about 2 hours, and dried using a countercurrent spray drying tower at a hot air temperature of 260° C. to a water content of about 6% by mass to obtain a spray-dried powder (spray drying step).
The component (A) and the component (B) (B-3 or B-4 or B-5 of the component (B)) are added to the spray-dried powder, and the mixture is stirred and granulated to form an α-sulfofatty acid methyl ester salt. Content particles were obtained (stir granulation step).
(C) Component and the remaining components other than the perfume components shown in Tables 1 to 3 are dry-mixed with the α-sulfofatty acid methyl ester salt-containing particles, and then the perfume is spray-mixed to prepare a powdered powder detergent. (Powder mixing step).
In Comparative Example 1, a powder detergent of powder was prepared in the same manner as above except that the component (A) was added after the stir-casting (powder mixing step).
In Comparative Example 2, a powder detergent of powder was prepared in the same manner as above except that the amount of the component (B) was changed.
In Comparative Example 3, a powder detergent of powder was prepared in the same manner as above except that the amount of the component (C) was changed.

[Evaluation of detergency]
Using a color difference meter (manufactured by Nippon Denshoku Industries Co., Ltd., product name: SE-2000), measure the reflectance of 5 sheets of artificially contaminated cloth (product name: wfk10TE, manufactured by wfk) before washing (hereinafter referred to as dirty cloth). The reflectance was calculated from the Hunter whiteness Z as R=Z/100. The same applies hereinafter. Terg-O-Tometer (manufactured by US Testing) is used as a cleaning tester, and 5 pieces of dirt cloth and a charge cloth (the cloth which has been finely cut, thoroughly washed and rinsed and dried) are predetermined. The bath ratio (30 times) was weighed and put into the washing tank, and then the washing liquid was put into the washing tank. As the cleaning liquid, one prepared by dissolving each powdered detergent in 900 mL of tap water at 25° C. to a concentration of 1667 ppm (mass standard) was used.
After washing at a rotation speed of 120 rpm and a temperature of 25° C. for 10 minutes, 900 mL of tap water at 25° C. was rinsed for 3 minutes twice. The reflectance of the stained cloth after rinsing, drying and washing was measured using a 460 nm filter, and the washing rate was calculated by the following formula.

Cleaning rate (%)=(K/S of contaminated cloth−K/S of cleaning cloth)/(K/S of contaminated cloth−K/S of uncontaminated cloth)×100 (i)
(In the formula (i), K/S is (1-R/100) ² /(2R/100), the contaminated cloth is the artificial contaminated cloth, and the cleaning cloth is the contaminated cloth. The latter cloth and uncontaminated cloth represent the original white cloth (original cloth) without stain, K is the extinction coefficient, S is the scattering coefficient, and R is the absolute reflectance, respectively.)
The larger the value of the cleaning rate obtained, the higher the cleaning power. If the average value of the cleaning rate of five sheets is 80% or more, it is ◎ (pass), if 65% or more and less than 80%, it is ◎ (pass), and if it is 50% or more and less than 65%, it is ○ (pass), 35. % Or more and less than 50% was evaluated as Δ (pass), and less than 35% was evaluated as x (fail).

[Liquidity evaluation]
Each powder detergent was measured according to [Method of measuring angle of repose] described in paragraph [0010] of JP-A-2018-30925.
If it is less than 40°, it is ◎ (pass), if it is 40° or more and less than 50°, it is ○ (pass), if it is 50° or more and less than 60°, it is Δ (pass), and if it is 60° or more, it is x (fail). Evaluated as.

[Solubility evaluation]
1 liter of water at 25° C. is put into a beaker, and a cell for measuring conductivity is inserted therein. Then, 1 g of each powder detergent was added to water and stirred at a speed of 250 rpm using a constant speed stirrer, and the time (seconds) for 90% dissolution of the added particles was measured.
If transparent, it was evaluated as ⊚ (pass), if it was slightly cloudy, it was evaluated as ○ (pass), if it was cloudy, it was evaluated as Δ (pass), and if it was considerably cloudy, it was evaluated as × (fail).

[Rinseability evaluation]
1 g of each powder detergent was added to 1 L of 20° C. tap water prepared in a 1 L beaker and stirred for 1 minute. After stirring, the mixture was allowed to stand for 3 minutes, and the appearance of turbidity was visually evaluated from above the beaker.
If transparent, it was evaluated as ⊚ (pass), if it was slightly cloudy, it was evaluated as ○ (pass), if it was cloudy, it was evaluated as Δ (pass), and if it was considerably cloudy, it was evaluated as × (fail).

As shown in the results of Table 1, all of Examples 1 to 24 prepared by the production method of the present invention were excellent in fluidity, solubility, rinseability, and detergency.
Comparative Example 1 in which the component (A) was added after stirring and granulation had poor solubility.
Comparative Example 2 in which the content of the component (B) was 10% by mass was inferior in fluidity.
Comparative Example 3 in which the content of the component (C) was 20% by mass was inferior in rinsability.

From the above results, it was confirmed that the powder detergent prepared by the production method of the present invention was excellent in fluidity, solubility, rinseability and detergency.

Claims (3)

(A) α-sulfofatty acid ester salt: 0.1 to 5% by mass
A method for producing a powder detergent containing (B) a surfactant other than (A) component: 0.1 to less than 25% by mass (C) a water-insoluble component: 0.1 to less than 20% by mass,
Characterized in that a solid α-sulfo fatty acid ester salt is added during stirring granulation,
Powder detergent manufacturing method. The method for producing a powder detergent according to claim 1, wherein the component (C) is zeolite. The method for producing a powder detergent according to claim 1 or 2, wherein the component (B) is at least one selected from LAS, soap, and nonionic surfactant.