JP2008150522A - Method for producing surfactant-containing particles - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for producing surfactant-containing particles which are decreased in the adhesion of a powder on a crusher and the inner side of pipes. <P>SOLUTION: The method for producing surfactant-containing particles comprises a step in which spray-dried particles (A) containing an anionic surfactant and an alkali builder and having 3-8 mass% moisture content and a liquid component (B) containing anionic surfactant and/or nonionic surfactant are fed to a kneader having stirring blades in a manner so that the mass ratio B/A of the liquid component (B) to the spray-dried particles (A) is 0.1-0.4, the obtained is mixed and pelletized with 250-1,000 J/kg stirring power to prepare granules having <50 mass% content of particles having ≥1,000 μm particle diameter and 6-9 mass% moisture content. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

  The present invention relates to a method for producing a surfactant-containing particle suitably used in a granular detergent composition.

  Granular detergent compositions such as garment detergents contain surfactant-containing particles as a major constituent. Such surfactant-containing particles are generally obtained by spray-drying a detergent slurry (a slurry for spray-drying) containing a surfactant such as an anionic surfactant or an alkali builder to form a detergent composition base powder (a spray-dried particle). The base powder (spray-dried particles) is manufactured to have a high bulk density.

As a method for increasing the bulk density of spray-dried particles, for example, Patent Document 1 discloses that a base powder and a liquid binder component are continuously supplied to a kneader and 1 to 10 kW / t (about 3.6 × 10 ^3). It describes a method of kneading with a kneading energy of about 36 × 10 ³ J / kg), extruding the obtained kneaded product, and further crushing and granulating.
JP 2000-144194 A

However, in the crushing and granulating step, there is a problem that the crushed powder adheres to the inside of the crushing device or to the inside of the pipe that is pneumatically transported.
In recent years, environmental awareness has increased, and it has become desirable to reduce the environmental burden of granular detergent compositions. To cope with this, non-soap anionic surfactants such as alkylbenzene sulfonates have been developed. A detergent composition with a reduced amount of agent used has been proposed. However, according to the knowledge of the present inventors, particularly when the content of the non-soap anionic surfactant in the surfactant-containing particles is reduced, the adhesion of the powder to the pulverizer and the piping becomes remarkable.

  This invention is made | formed in view of the said situation, and provides the manufacturing method of surfactant containing particle | grains which enabled it to reduce adhesion of the powder to the inside of a grinding | pulverization apparatus or piping.

As a result of intensive studies by the present inventors in order to solve the above problems, a kneader is usually used to obtain a relatively large lump kneaded product. In order to complete the present invention, it is found that appropriate mixing and granulation can be performed by making the content range, and a granule that can be used as a surfactant-containing particle to be blended in a granular detergent composition is obtained. It came.
The method for producing a surfactant-containing particle of the present invention comprises a spray-dried particle (A) containing an anionic surfactant and an alkali builder and having a water content of 3 to 8% by mass, an anionic surfactant, and / or Alternatively, the liquid component (B) containing the nonionic surfactant is mixed with a stirring blade so that the mass ratio B / A of the liquid component (B) to the spray-dried particles (A) is 0.1 to 0.4. Is mixed and granulated with a stirring power of 250 to 1000 J / kg, the content of particles having a particle diameter of 1000 μm or more is less than 50 mass%, and the water content is 6 to 9 mass. % Of obtaining a granular material that is%.
The content of the linear alkyl benzene sulfonate (hereinafter sometimes abbreviated as LAS) in the spray-dried particles (A) is 6.5% by mass or less, and the anionic surfactant in the granular material. The total content is preferably 15 to 28% by mass, and the LAS content is preferably 4.5% by mass or less.

  According to the present invention, a powder and granular material is obtained by mixing and granulating with a specific stirring power in a kneader, so that the subsequent crushing treatment can be omitted or reduced, whereby the powder into the pulverizer and the pipes can be reduced. Body adhesion can be reduced.

<Spray-dried particles (A)>
The spray-dried particles (A) used in the present invention contain an anionic surfactant (A1) and a builder (A2), and at least an alkali builder (A21) as the builder (A2). You may contain another component (A3) as needed.
[Anionic surfactant (A1)]
As an anionic surfactant (A1), if it is conventionally used in detergent, it will not specifically limit but various well-known anionic surfactants are mentioned. For example, the anionic surfactant shown to the following (1)-(12) is mentioned.

(1) A linear or branched alkylbenzene sulfonate (LAS or ABS) having an alkyl group having 8 to 18 carbon atoms.
(2) Alkanesulfonate having 10 to 20 carbon atoms.
(3) C10-20 α-olefin sulfonate (AOS).
(4) Alkyl sulfate or alkenyl sulfate (AS) having 10 to 20 carbon atoms.
(5) C10-20 linear or branched alkyl or alkenyl groups having an average of 0.5 to 10 moles of ethylene oxide, propylene oxide, butylene oxide, and ethylene oxide and propylene oxide (moles) Ratio: 0.1 / 9.9 to 9.9 / 0.1), or an alkyl ether sulfate or an alkenyl ether sulfate (AES).
(6) C10-20 linear or branched alkylphenyl or alkenylphenyl groups having an average of 3 to 30 moles of ethylene oxide, propylene oxide, butylene oxide, and ethylene oxide and propylene oxide (moles) Ratio: 0.1 / 9.9 to 9.9 / 0.1), or an alkylphenyl ether sulfate or an alkenylphenyl ether sulfate.
(7) C10-20 linear or branched alkyl or alkenyl groups having an average of 0.5 to 10 moles of ethylene oxide, propylene oxide, butylene oxide, and ethylene oxide and propylene oxide (moles) Ratio: 0.1 / 9.9 to 9.9 / 0.1), or an alkyl ether carboxylate or alkenyl ether carboxylate.
(8) Alkyl polyhydric alcohol ether sulfate such as alkyl glyceryl ether sulfonic acid having 10 to 20 carbon atoms.
(9) C8-20 saturated or unsaturated α-sulfo fatty acid salt or methyl ester, ethyl ester or propyl ester (α-SF or MES) thereof.
(10) Long chain monoalkyl phosphate, dialkyl phosphate, or sesquialkyl phosphate.
(11) Polyoxyethylene monoalkyl phosphate, polyoxyethylene dialkyl phosphate, or polyoxyethylene sesquialkyl phosphate.
(12) A higher fatty acid salt having 10 to 20 carbon atoms.

  The anionic surfactant (A1) may be used as alkali metal salts such as sodium and potassium, amine salts, ammonium salts and the like. An anionic surfactant (A1) may be used individually by 1 type, and may use 2 or more types together. Among the anionic surfactants, alkali metal salts of linear alkylbenzene sulfonic acid (LAS) (for example, sodium or potassium salt), alkali metal salts of AOS, α-SF, AES (for example, sodium or potassium salt, etc.) ), Alkali metal salts of higher fatty acids (for example, sodium or potassium salts) and the like.

In the spray-dried particles (A), the content of the non-soap anionic surfactant is reduced, and the content of LAS is particularly preferably 6.5% by mass or less. The non-soap anionic surfactant in the present invention includes anionic surfactants other than soap. The soap here means a fatty acid salt (wherein the fatty acid may be a saturated fatty acid or an unsaturated fatty acid, and preferably has 6 to 22 carbon atoms, more preferably 10 to 20 carbon atoms). .
Specific examples of the non-soap anionic surfactant include the anionic surfactants shown in the above (1) to (11). Among these, linear alkylbenzene sulfonate (LAS) is preferable, and alkali metal salts thereof (for example, sodium or potassium salts) are particularly preferable.
When the content of LAS in the spray-dried particles (A) is 6.5% by mass or less, a granular detergent composition suitable for the environment is easily obtained. The lower limit of the LAS content may be zero, but is preferably 1% by mass or more from the viewpoint of improving detergency. A more preferable range is 1.5 to 6.5% by mass.

  The content of the anionic surfactant (A1) in the spray-dried particles (A) is preferably 6 to 15% by mass and more preferably 8 to 12% by mass in total of the non-soap anionic surfactant and soap. When it is at least the lower limit of the above range, the detergency is good, and when it is at most the upper limit, the slurry viscosity is suitable for spray drying.

[Builder (A2)]
Examples of the builder (A2) include inorganic builders and organic builders.
(Inorganic builder)
Examples of inorganic builders include alkaline salts such as sodium carbonate, potassium carbonate, sodium bicarbonate, sodium sulfite, sodium sesquicarbonate, sodium silicate, crystalline layered sodium silicate, and amorphous layered sodium silicate; Salts: phosphates such as orthophosphates, pyrophosphates, tripolyphosphates, metaphosphates, hexametaphosphates and phytates; crystalline aluminosilicates represented by the following general formula (VI); Amorphous aluminosilicate represented by (VII); Amorphous aluminosilicate represented by the following general formula (VIII) and the like.

Formula _{(VI): x1 (M 2} O) · Al 2 O 2 · y1 (SiO 2) · w1 (H 2 O).
In general formula (VI), M represents an alkali metal atom such as sodium or potassium. x1, y1 and w1 represent the number of moles of each component. Generally, x1 is any number from 0.7 to 1.5, y1 is any number from 0.8 to 6, and w1 is arbitrary. Represents a positive number.

Formula _{(VII): x2 (M 2} O) · Al 2 O 3 · y2 (SiO 2) · w2 (H 2 O).
In general formula (VII), M represents an alkali metal atom such as sodium or potassium. x2, y2 and w2 represent the number of moles of each component. Generally, x2 is any number from 0.7 to 1.2, y2 is any number from 1.6 to 2.8, w2 represents 0 or an arbitrary positive number.

Formula _{(VIII): x3 (M 2} O) · Al 2 O 3 · y3 (SiO 2) · Z3 (P 2 0 5) · w3 (H 2 O).
In general formula (VIII), M represents an alkali metal atom such as sodium or potassium. x3, y3, Z3 and w3 represent the number of moles of each component. Generally, x3 is any number from 0.2 to 1.1, and y3 is any number from 0.2 to 4.0. Number, z3 represents any number from 0.001 to 0.8, and w3 represents 0 or an arbitrary positive number.

  Among the inorganic builders, sodium carbonate, potassium carbonate, sodium silicate, sodium tripolyphosphate, sodium aluminosilicate, and the like are preferable. These inorganic builders may be used alone or in combination of two or more.

(Organic builder)
Examples of the organic builder include aminocarboxylates such as nitrilotriacetate, ethylenediaminetetraacetate, β-alanine diacetate, aspartate diacetate, methylglycine diacetate, and iminodisuccinate; serine diacetate, hydroxyimino Hydroxyaminocarboxylates such as disuccinate, hydroxyethylethylenediamine triacetate, dihydroxyethylglycine; Hydroxycarboxylates such as hydroxyacetate, tartrate, citrate, gluconate; pyromellitic acid salt, Cyclocarboxylates such as benzopolycarboxylates, cyclopentanetetracarboxylates; ether carboxylates such as carboxymethyltaltronate, carboxymethyloxysuccinate, oxydisuccinate, tartaric acid mono- or disuccinate; Acrylic acid polymers and copolymers such as reacrylic acid, acrylic acid-allyl alcohol copolymer, acrylic acid-maleic acid copolymer, hydroxyacrylic acid polymer, polysaccharide-acrylic acid copolymer; maleic acid, itacon Polymers or copolymers of acids, fumaric acid, tetramethylene 1,2-dicarboxylic acid, succinic acid, aspartic acid; polysaccharide oxides such as starch, cellulose, amylose, pectin; polysaccharides such as carboxymethyl cellulose; polyethylene Non-dissociative polymer compounds such as glycol, polyvinyl alcohol, and polyvinyl pyrrolidone are listed.

  Among these organic builders, citrate, aminocarboxylate, polyacrylate, acrylic acid-maleic acid copolymer, and the like are preferable. These organic builders may be used alone or in combination of two or more.

In the present invention, the spray-dried particles (A) contain at least an alkali builder (A21). Among the specific examples of the builder (A2) listed above, the alkali builder (A21) is sodium carbonate, potassium carbonate, sodium bicarbonate, sodium sulfite, sodium sesquicarbonate, sodium silicate, crystalline layered sodium silicate, and amorphous layered layer. Sodium silicate. Among these, sodium carbonate, potassium carbonate, sodium bicarbonate, and sodium sulfite are preferable, and sodium carbonate, potassium carbonate, and sodium sulfite are particularly preferable. An alkali builder (A21) can be used individually by 1 type or in combination of 2 or more types.
The content of the alkali builder (A21) in the spray-dried particles (A) is preferably 40 to 75% by mass, and more preferably 50 to 65% by mass. When it is at least the lower limit of the above range, the detergency is good, and when it is at most the upper limit, the dust generation is low.
The total content of the builder (A2) in the spray-dried particles (A) is preferably 70 to 90% by mass and more preferably 80 to 90% by mass in order to impart sufficient detergency.

[Other components (A3)]
Other components (A3) other than the anionic surfactant (A1) and the builder (A2) can be appropriately selected from components conventionally used in detergents.
For example, surfactants other than the anionic surfactant (A1), water-soluble polymer compounds, fluorescent brighteners, and the like can be mentioned.
Examples of other surfactants include known nonionic surfactants, cationic surfactants, and amphoteric surfactants. These can be used singly or in appropriate combination of two or more. When the surfactant other than the anionic surfactant (A1) is contained in the spray-dried particles (A), the content is not particularly limited, but from the viewpoint of handling the spray-dried particles, the spray-dried particles ( 0.01-1.0 mass% is preferable with respect to A), and 0.1-0.5 mass% is more preferable.

As the water-soluble polymer compound, any of natural polymer compounds, semi-synthetic polymer compounds, and synthetic polymer compounds can be suitably used.
The “water-soluble polymer compound” in the present specification has a solubility in water at 20 ° C. of 0.1 g / (100 g water) or more, preferably 0.2 g / (100 g water) or more, more preferably Is a compound that is 0.3 g / (100 g water) or more. The mass average molecular weight is preferably 500 or more, more preferably 2000 or more, and the upper limit is preferably 100,000 or less. Here, the “mass average molecular weight” means a value measured by gel permeation chromatography using polyethylene glycol as a standard substance.

Examples of the natural polymer compound include seaweed polymer compounds such as agar and sodium alginate; gum polymer compounds such as xanthan gum and gum arabic; and polymer compounds of proteins such as gelatin, casein and collagen. It is done.
Examples of the semi-synthetic polymer compound include cellulose derivatives such as methyl cellulose, ethyl cellulose, hydroxyethyl cellulose, and carboxymethyl cellulose; starch derivatives such as carboxymethyl starch and dialdehyde starch.
Examples of the synthetic polymer compound include acrylic acid polymers, maleic acid polymers, acrylic acid / maleic acid copolymers, polyvinyl alcohols, carboxyvinyl polymers, and highly polymerized polyethylene glycols.

Among the above water-soluble polymer compounds, carboxymethyl cellulose, acrylic acid polymer, maleic acid polymer, acrylic acid / maleic acid copolymer, and salts thereof, which are generally used for washing; highly polymerized polyethylene glycol, etc. More preferred is an acrylic acid / maleic acid copolymer.
The said water-soluble polymer compound can be used individually by 1 type or in combination of 2 or more types.
When the water-soluble polymer compound is contained in the spray-dried particles (A), the content is not particularly limited, but is preferably 0.5 to 5% by mass, and 1 to 3% by mass with respect to the spray-dried particles (A). % Is more preferable. When it is at least the lower limit of the above range, the low dusting property of the spray-dried particles is good, and when it is at most the upper limit, the handleability of the spray-dried particles is good.

  Examples of optical brighteners include Disodium 4,4′-bis (2-sulfostyryl) -biphenyl, Disodium 4,4′-bis [(4-anilino-6-morpholino-1,3,5-triazine-2-yl). ) Amino] stilbene-2,2'-disulfonate and the like.

[Method for producing spray-dried particles (A)]
The spray-dried particles (A) are prepared, for example, by preparing a slurry containing an anionic surfactant, an alkali builder, and other components as necessary, and preferably containing about 34 to 39% by mass of water. Obtained by spray drying.
Spray drying can be performed by a known method. For example, spray dried particles can be produced by transferring the slurry to a spray drying tower and spraying at a predetermined spray pressure from a spray drying slurry atomizer installed near the top of the spray drying tower. .

The spray-drying tower may be a counter-current type or a co-current type. Among them, the counter-current type is preferable because thermal efficiency and dry powder (spray-dried particles) can be sufficiently dried.
Examples of the atomizer for the slurry for spray drying include a pressure spray nozzle, a two-fluid spray nozzle, and a rotary disk type. Among them, it is preferable to use a pressure spray nozzle that can easily obtain a desired average particle diameter.
During spray drying of the slurry for spray drying, high temperature gas is supplied into the spray drying tower. This hot gas is supplied from, for example, the lower part of the spray drying tower and discharged from the top of the spray drying tower.
The temperature of the high-temperature gas is preferably 170 to 300 ° C, and more preferably 200 to 280 ° C. If it is this range, the slurry for spray-drying can fully be dried, and the spray-dried particle | grains of the desired water content can be obtained easily.
Moreover, it is preferable that the temperature of the gas discharged | emitted from a spray-drying tower is 70-125 degreeC normally, and it is more preferable that it is 70-115 degreeC.
In addition, when high temperature gas is supplied from the lower part of a spray-drying tower and discharged | emitted from the tower top of a spray-drying tower (countercurrent type), in order to suppress that the temperature of the spray-dried particle obtained becomes too high, it sprays. Cold air can be supplied from the bottom of the drying tower. At the same time, for example, inorganic fine particles (such as zeolite) are introduced from the lower part of the spray drying tower and brought into contact with the spray drying particles, thereby preventing the adhesion of the spray drying particles to the inner wall of the spray drying tower. The fluidity of the spray-dried particles can be improved.

The drying conditions in the spray drying are set so that the water content in the obtained spray dried particles is 3 to 8% by mass. The water content in the spray-dried particles is preferably 3.5 to 7.5% by mass, more preferably 4 to 7% by mass. When it is at least the lower limit of the above range, the low dusting property is good, and when it is at most the upper limit, aggregation of particles is easily suppressed.
The water content in the spray-dried particles can be controlled by, for example, a method of adjusting the temperature of the hot gas supplied into the spray-drying tower.
Although the average particle diameter of spray-dried particle (A) is not specifically limited, Preferably it is about 100-700 micrometers, and 150-500 micrometers is more preferable. When it is at least the lower limit of the above range, the low dusting property is good, and when it is at most the upper limit, the particle strength becomes relatively strong. The average particle diameter can be controlled by slurry viscosity, spray pressure, and tower temperature.
Here, the average particle diameter in the present specification is a mass-based median diameter.

<Liquid component (B)>
The liquid component (B) used in the present invention contains an anionic surfactant (B1) and / or a nonionic surfactant (B2).
As an anionic surfactant (B1), what was mentioned as an example of the said anionic surfactant (A1) can be used. Among them, α-sulfo fatty acid alkyl ester salt (MES), polyoxyethylene alkyl ether sulfate (LES), secondary alkane sulfonate (SAS) and the like are preferable as the anionic surfactant (B1). Can be mentioned. MES is preferably used in the form of a concentrate.

As a nonionic surfactant (B2), if it is conventionally used in a detergent, it will not specifically limit but well-known various nonionic surfactant is mentioned.
For example, the nonionic surfactant shown to the following (1)-(12) is mentioned.

(1) An average of 3 to 30 mol (preferably 5 to 20 mol) of an alkylene oxide having 2 to 4 carbon atoms was added to an aliphatic alcohol having 6 to 22 carbon atoms (preferably 8 to 18 carbon atoms). Polyoxyalkylene alkyl (or alkenyl) ether. Among these, polyoxyethylene alkyl (or alkenyl) ether, polyoxyethylene polyoxypropylene alkyl (or alkenyl) ether, and the like are preferable. Examples of the aliphatic alcohol used here include primary alcohols and secondary alcohols, and primary alcohols are preferred. The alkyl group may have a branched chain.

(2) Fatty acid alkyl ester alkoxylates represented by the following general formula (I) in which an alkylene oxide is added between the ester bonds of polyoxyethylene alkyl (or alkenyl) phenyl ether or long-chain fatty acid alkyl ester.
General formula ^{(I): R 1 CO (} OA) nOR 2.
In the general formula (I), R ¹ CO represents a fatty acid residue having 6 to 22 (preferably 8 to 18) carbon atoms. OA represents an addition unit of alkylene oxide having 2 to 4 carbon atoms (preferably 2 to 3 carbon atoms) such as ethylene oxide and propylene oxide. n shows the average addition mole number of alkylene oxide, and is generally 3-30 (preferably the number of 5-20). R ² represents a lower alkyl group which may have a substituent having 1 to 3 carbon atoms.

(3) Polyoxyethylene sorbitan fatty acid ester.
(4) Polyoxyethylene sorbite oleate.
(5) Polyoxyethylene fatty acid ester.
(6) Polyoxyethylene hydrogenated castor oil.
(7) Glycerin fatty acid ester.
(8) Fatty acid alkanolamide.
(9) Polyoxyethylene alkylamine.
(10) Alkyl glycoside.
(11) Alkylamine oxide.
(12) Polyoxyethylene alkyl ether.

  A nonionic surfactant (B2) may be used individually by 1 type, and may use 2 or more types together. Of those mentioned above, polyoxyethylene alkyl ether is preferred. Polyoxyethylene alkyl ether is preferably used as a component of the MES concentrate.

The proportion of the total amount of the anionic surfactant (B1) and the nonionic surfactant (B2) in the liquid component (B) is preferably 70 to 95% by mass, and more preferably 80 to 90% by mass. When it is at least the lower limit of the above range, the detergency becomes good, and when it is at most the upper limit, it tends to be highly soluble.
The proportion of the anionic surfactant (B1) in the total amount of the anionic surfactant (B1) and the nonionic surfactant (B2) is preferably 50 to 90% by mass, and more preferably 60 to 85% by mass. When it is at least the lower limit of the above range, high detergency can be easily obtained, and when it is at most the upper limit, high solubility tends to be obtained.

  The liquid component (B) is preferably an aqueous solution. The water content in the liquid component (B) is preferably 10 to 40% by mass, and more preferably 25 to 35% by mass. When it is at least the lower limit of the above range, it tends to be highly soluble, and when it is at most the upper limit, the detergency is good.

  In the present invention, the amount of the liquid component (B) used is such that the mass ratio B / A of the liquid component (B) to the spray-dried particles (A) is in the range of 0.1 to 0.4. When it is 0.1 or more, high bulk density particles are easily obtained, and when it is 0.4 or less, particles having a particle diameter of less than 1000 μm are easily obtained. Preferably, B / A = 0.25 to 0.35.

<Kneader with stirring blades>
1-5 is a figure which shows the example of a stirring blade (paddle), and is explanatory drawing which shows an example of arrangement | positioning (paddle pattern) of the paddle in the kneading machine of FIG. FIG. 7 is an explanatory diagram showing another example of a paddle pattern.
In the kneader used in the present invention, a plurality of stirring blades (paddles) are incorporated in each of two parallel rotating shafts so that the rotating shafts and the stirring blades move integrally. A continuous kneader configured to rotate in the same direction is preferably used. A pair of left and right paddles incorporated in two rotating shafts are set so that their phases are shifted by 90 degrees, and the pair of paddles always rotate so that one tip rubs against the other, and this configuration It is preferable that a cleaning action is obtained.

  As shown in FIGS. 6 and 7, a screw (S) is arranged near the supply port of the kneader so that the supplied components are sent to the processing zone. The treatment zone is divided into (a) a transport zone, (b) a mixing zone, and (c) a kneading zone according to a combination of stirring blades (paddles) provided at the rear stage of the screw. The number of paddles used in the processing zone is not particularly limited. For example, about 20 to 30 paddles are incorporated.

Hereinafter, the configuration of each zone in the processing zone and the stirring blade group incorporated in the zone will be described.
(A) Transport zone: has a function of transporting components (contents) in a direction from the supply port of the kneader toward the discharge port. The blade group in this zone is configured such that a propulsive force is generated in the component transport direction.
(B) Mixing zone: has a function of mixing components. The blade group in this zone is configured so that no propulsive force is generated.
(C) Kneading zone: has a function of kneading the components. The blade group in this zone is configured such that a propulsive force is generated in the direction opposite to the component transport direction.

As the stirring blade (paddle), a flat paddle (F) shown in FIG. 1 and a helical paddle (H) shown in FIG. 2 are preferably used. By changing the combination of paddles having different shapes, the presence and direction of propulsion can be controlled.
The outer surface of the flat paddle (F) is composed of both end surfaces 11, 12 perpendicular to the rotation axis O and a peripheral surface 13. The shape of both end faces 11 and 12 is a substantially convex lens shape. The shape and direction of the cross section of the flat paddle (F) perpendicular to the rotation axis O are constant in the longitudinal direction of the rotation axis O. The pair of left and right flat paddles (F) incorporated in the two parallel rotating shafts O always have the peripheral surface 13 of one paddle and the peripheral surface 13 of the other paddle when the rotating shaft O rotates in the same direction. It is arranged so that and touch. The ratio of the minor axis D1 and the major axis D2 of the both end faces 11, 12 is preferably minor axis D1 / major axis D2 = 1/1 to 1/3. The peripheral surface 13 is a curved surface orthogonal to both end surfaces 11 and 12, and the width W1 in the longitudinal direction of the rotation axis O is preferably 1/6 to 1/2 of the major axis D2, and 1/4 to 1/3. More preferred.

FIG. 2 is a view of the helical paddle (H) viewed from the end face 21 side. The outer surface of the helical paddle (H) is composed of both end faces 21 and 22 perpendicular to the rotation axis O and a peripheral face 23. Both the end faces 21 and 22 have substantially the same convex lens shape as the flat paddle (F). The shape of the helical paddle (H) is different from the shape of the flat paddle (F) in that one end surface 21 and the other end surface 22 are coaxial and have different directions, and the peripheral surface 23 is twisted helically. It is a point. That is, the cross section of the helical paddle (H) perpendicular to the rotation axis O has a constant shape in the longitudinal direction of the rotation axis O, but the direction gradually changes around the rotation axis O. In the projection view of the helical paddle (H) viewed from one end face 21 side, the helical pitch P represented by the deviation width between the tip end of one end face 21 and the tip end of the other end face 22 is 1/10 or less of the major axis D2 is suitable, and preferably 1/10 to 1/30.
The preferred range of the ratio of the minor axis D1 to the major axis D2 of the both end faces 21, 22 and the width W1 in the longitudinal direction of the rotation axis O is the same as that of the flat paddle (F).
Although the screw (S) is not shown, the pitch is preferably 1/2 to 1/3 of the major axis.

FIG. 3 shows a preferred example of a transport zone paddle configuration. In this example, two or more helical paddles (H) are arranged in the discharge port direction while shifting by 45 degrees in the direction opposite to the rotation direction of the rotation shaft.
3 to 7, H represents a helical paddle, and F represents a flat paddle. S represents a screw, FS represents a feed screw, and RS represents a reverse screw. In FIG. 3, “45 °” in “H reverse 45 °” indicates that the direction of the corresponding end surface is shifted by 45 degrees between adjacent paddles, and “reverse” indicates that the shift in the direction of the end surface is opposite to the rotation direction. It shows that.
3, 6 and 7, the numbers 1, 2, 3 and 4 are 45 degrees, 3 is 90 degrees, and 4 are 135 degrees with respect to the reference paddle 1. Is the direction in the direction opposite to the rotation direction. If it is tilted 45 degrees further from 4, the paddle is in its original 1 state.

FIG. 4 shows a preferred example of a paddle configuration in the mixing zone. In this example, two or more helical paddles (H) are arranged in the discharge port direction while being shifted by 90 degrees in the rotation direction of the rotation shaft. H90 ° indicates that H is a helical paddle, and 90 ° indicates that the direction of the corresponding end surface is shifted by 90 degrees between adjacent paddles.
4, 6, and 7, the numbers 1, 3, 1, and 3 indicate that 3 is inclined by 90 degrees with respect to the reference paddle 1, and if the inclination is further 90 degrees from 3, It shows that it becomes the state of 1.

FIG. 5 shows a preferred example of the paddle configuration of the kneading zone. In this example, two or more flat paddles (F) are arranged in the discharge port direction while being shifted by 45 degrees in the rotation direction of the rotation shaft. Note that “positive” at F positive 45 ° indicates that the deviation of the orientation of the end face is the same as the rotational direction (positive direction).
5, 6, and 7, numerals 1, 4, and 3 indicate that 3 is inclined by 90 degrees and 4 is inclined by 135 degrees with respect to the reference paddle 1.

A paddle pattern suitable for the present invention is, for example, as shown in FIG. 6, from the supply port to the discharge port direction of the kneader, screw zone, transport zone, mixing zone, kneading zone, mixing zone, kneading zone, mixing A configuration in which the zone and the transport zone are arranged in this order is preferable.
Or, as shown in FIG. 7, from the supply port of the kneader toward the discharge port, the screw zone, the transport zone, the mixing zone, the kneading zone, the mixing zone, the kneading zone, the mixing zone, the kneading zone, and the transport zone in this order. Arranged arrangements are also preferred.

<Method for producing surfactant-containing particles>
First, spray-dried particles (A) and a liquid component (B) are supplied to a kneader having a stirring blade. If necessary, other components other than (A) and (B) may be supplied at the same time. For example, an inorganic builder such as zeolite or potassium carbonate is preferably added as the other component in terms of reducing coarse particles.
When an inorganic builder is used as the other component, the addition amount is preferably 0 to 30% by mass and more preferably 5 to 20% by mass with respect to the total amount of the kneader.
The kneader is preferably a continuous kneader as described above, and it is preferable to continuously supply the spray-dried particles (A), the liquid component (B) and other components as required.

Mixing and granulation are performed in the kneader by adjusting the stirring power in the kneader so that the properties of the kneaded product discharged from the kneader become powder particles. The granular material in this invention means that whose content of particle | grains whose particle diameter is 1000 micrometers or more is less than 50 mass%. Specifically, the kneaded product discharged from the kneader is sieved and divided into particles having a particle size of 1000 μm or more and less than 1000 μm, and the case where the particles of 1000 μm or more are less than 50% by mass is referred to as powder, The case where it is 50 mass% or more is referred to as a koji product.
When the content of particles having a particle diameter of 1000 μm or more in the kneaded product discharged from the kneader is less than 50% by mass, an effect of omitting or reducing the subsequent crushing treatment is sufficiently obtained. The particle size (particle size distribution) of the powder can be controlled by adjusting the stirring power in the kneader.

The stirring power (unit: J / kg) in this specification is a value calculated by the following mathematical formula (1).

  In Equation (1), the actual current value and the air current value can be obtained by reading the current value of the motor of the kneader. The motor current value (air current value, unit: A) in an empty state before supplying the raw material to the kneader is read in advance, and the motor current value (actual current value, Unit: A) is read. The voltage (unit: V) reads the voltage of the voltmeter. The power factor (unit: none) is calculated as 0.8. The production capacity (unit: t / hr) is obtained from raw material input / time.

In the present invention, the stirring power in the kneader is in the range of 250 to 1000 J / kg. Preferably it is the range of 250-700 J / kg, The range of 250-500 J / kg is more preferable.
When the stirring power exceeds 1000 J / kg, the properties of the kneaded product discharged from the kneader are unlikely to become powder particles, and for example, the particles are likely to have a large particle size or lump shape. Moreover, when the stirring power is less than 250 J / kg, the mixture is not sufficiently mixed and is easily discharged in a non-uniform state. If the mixing is not uniform, the solubility tends to deteriorate.

The stirring power in the kneader is the composition of the raw materials (spray dried particles (A), liquid component (B) and other components) supplied to the kneader; the shape and arrangement of the paddles in the kneader; the throughput per unit time It can be adjusted by changing the operating conditions such as the raw material supply method, the rotational speed, the temperature of the raw material to be supplied, the temperature of the material to be kneaded (kneading temperature) in the kneader.
Specifically, when using a kneader equipped with the above (a) transport zone, (b) mixing zone, and (c) kneading zone, the kneading zone has the largest stirring power among these three types of zones. Followed by a mixing zone and a transport zone. Therefore, the stirring power in the kneader can be adjusted by changing the combination and ratio of the zones. For example, the agitation power can be increased by reducing the transport zone ratio and increasing the mixing zone and / or kneading zone ratio.
Further, when the rotational speed of the paddle is increased, the stirring power increases.
When the temperature of the raw material supplied to the kneader and the kneading temperature are increased, the stirring power increases.
Regarding the raw material composition supplied to the kneader, the stirring power increases when the mass ratio B / A of the liquid component (B) to the spray-dried particles (A) is increased. When the proportion of the total amount of the anionic surfactant (B1) and the nonionic surfactant (B2) in the liquid component (B) is increased, the stirring power increases. When the content of the nonionic surfactant (B2) in the liquid component (B) is increased, the stirring power increases. When the water content in the liquid component (B) is increased, the stirring power increases. In general, since it is difficult to largely change the raw material composition due to restrictions on the detergent composition, it is preferable to adjust the water content when adjusting the stirring power by the raw material composition.

The temperature of the spray-dried particles (A) supplied to the kneader is preferably 15 to 35 ° C, more preferably 20 to 30 ° C. If it is at least the lower limit of the above range, condensation is unlikely to occur, and if it is at most the upper limit, handling properties are good.
60-80 degreeC is preferable and, as for the temperature of the liquid component (B) supplied to a kneading machine, 65-75 degreeC is more preferable. When the amount is not less than the lower limit of the above range, the mixing property of the particles and the liquid component is good, and when it is not more than the upper limit, it is easy to suppress the coarsening of the obtained particles.
In order to prevent the temperature of the material to be kneaded from rising too much in the kneader, it is desirable to knead while passing cooling water through the jacket of the kneader. As the cooling water, for example, an aqueous solution of ethylene glycol is suitable, and its concentration is 15 to 30% by mass, preferably 20 to 25% by mass.
The temperature of the cooling water can be appropriately set according to the control temperature of the material to be kneaded. For example, the inlet temperature of the cooling water is preferably 0 to 10 ° C. The control temperature of the material to be kneaded depends on the composition, but 20 ~
About 50 degreeC is preferable.

The water content in the kneaded material (powder) discharged from the kneader is 6 to 9% by mass. When the water content of the granular material is 6% by mass or more, breakage of particles can be reduced, and when it is 9% by mass or less, aggregation of particles is easily suppressed.
The water content of the granular material can be controlled by adjusting the water content of the spray-dried particles and the amount of water added to the kneader.
The water content of the granular material is more preferably 7 to 8% by mass.

As described above, when producing surfactant-containing particles suitable for the environment by reducing the LAS content, the LAS content is 6.5% by mass or less as spray-dried particles (A). It is preferable that the total content of the anionic surfactant in the granular material discharged from the kneader is 15 to 28% by mass and the LAS content is 4.5% by mass or less. When the total content of the anionic surfactant in the granular material is 15% by mass or more, the detergency is good, and when it is 28% by mass or less, the solubility is good.
The total content of the anionic surfactant in the granular material is determined by the raw material composition supplied to the kneader. A more preferable range is 18 to 28% by mass.
The content of LAS in the granular material is determined by the raw material composition supplied to the kneader. More preferably, it is 1-2 mass%.

  The granular material (surfactant-containing particles) thus obtained can be used as it is as a component of the granular detergent composition. Specifically, the obtained granular material (surfactant-containing particles) is mixed with compounding component particles such as bleaching agent particles, bleaching activator particles, enzyme particles, softening agent particles, and silicone particles. Thus, a granular detergent composition can be produced. Moreover, a fragrance | flavor may be mix | blended as a fragrance | flavor particle | grain, and when mixing, a liquid fragrance | flavor may be spray-added. Moreover, you may use what gave the grinding | pulverization process and the sieving process with respect to the obtained granular material (surfactant containing particle | grains) as needed as a structural component of a granular detergent composition.

According to the method of the present invention, a powder and granular material is obtained by mixing with a specific stirring power in a kneader, so that the subsequent crushing treatment can be omitted or reduced. Thereby, the problem of adhesion of the powder to the inside of the pulverizer or the pipe can be improved.
The method of the present invention can also be applied to detergent compositions other than the composition in which the LAS content is reduced to the above range, and the same effects can be obtained. Since the adhesion to the apparatus and the piping is remarkable, the effect of applying the present invention is great.

Hereinafter, the present invention will be described in more detail using examples, but the present invention is not limited to these examples. In the following, the blending ratio and the unit of content are mass% unless otherwise specified.
<Production Examples 1 to 7 of spray-dried particles>
Spray dried particles having the composition shown in Table 1 were produced. Table 1 shows the content (unit: mass%) of each component when the mass of the spray-dried particles is 100 mass%. Each of the spray-dried particles obtained in Production Examples 1 to 7 was converted into a particle No. 1-7. Production Example 7 is a comparative example. 7 has a water content of more than 8% by mass.
Each raw material shown in Table 1 is as follows.

LAS: Lion Corp., Rypon LH-200.
Soap: Fatty acid (C12-18) sodium (67 mass% pure water solution).
Zeolite: A-type zeolite (pure 40.5 mass% aqueous solution) manufactured by Nippon Chemical Co., Ltd.
MA agent: Nippon Shokubai Co., Ltd., Aquaclick TL-400 (pure 40 mass% aqueous solution).
Potassium carbonate: Asahi Glass Co., Ltd., potassium carbonate (powder).
Sodium carbonate: Asahi Glass Co., Ltd., grain ash.
Sodium sulfite: manufactured by Shinshu Chemical Co., Ltd., anhydrous sodium sulfite.
Sodium sulfate: manufactured by Nippon Chemical Industry Co., Ltd., neutral anhydrous sodium sulfate.
Optical brightener: Chino Pearl CBS-X, manufactured by Ciba Specialty Chemicals.
Other components: Impurities contained in each raw material.

First, the raw materials shown in Table 1 were uniformly mixed to prepare a slurry for spray drying. About components other than water, the compounding quantity was adjusted so that a compounding ratio might correspond with the ratio shown in Table 1. The compounding amount of water was 52 to 64 parts by mass with respect to a total of 100 parts by mass of the components other than water. Zeolite was added as a slurry using water as a dispersion medium, and MA agent was added as an aqueous solution. In all cases, only the pure content was calculated as the blending amount of “components other than water”, and the water as the dispersion medium and the solvent was calculated as part of the blending amount of water.
The order of blending was water, other components, LAS, fluorescent brightening agent, zeolite, MA agent, inorganic compounds (sodium carbonate, potassium carbonate, sodium sulfite, sodium sulfate), and soap.
Next, the obtained slurry for spray drying was transferred to a spray drying tower and sprayed from a pressure spray nozzle installed near the top of the spray drying tower to obtain spray dried particles having the composition shown in Table 1.
The moisture content (% by mass) in the obtained spray-dried particles was measured with a Kett moisture meter (trade name, manufactured by Ketto Scientific Laboratory; infrared moisture meter). The measurement conditions were 170 ° C. and 20 minutes.
The average particle size of the obtained spray-dried particles is determined by performing classification using a 9-stage sieve and a tray having openings of 1680, 1410, 1190, 1000, 710, 500, 350, 250, and 149 μm. The 50% mass was calculated from the mass frequency of each particle size. The results are also shown in Table 1.

<Examples 1-11 and Comparative Examples 1-6>
Using the spray-dried particles (A) obtained in Production Examples 1 to 7, the kneading machine having the paddle pattern shown in FIG. 6 or 7 (made by Kurimoto Iron Works, KRC Kneader S4 type) with the formulation shown in Table 2 ) Was used to produce a granular material.
Each raw material shown in Table 2 is as follows.

MES / nonionic concentrated paste: α-sulfo fatty acid (C14-16) methyl ester sodium salt (AI 90% by mass) and polyoxyethylene (average number of moles added = 15) alkyl (C12-14) ether (pure 90% by mass) ) In AI at a ratio of 8: 2.
Nonionic solution: polyoxyethylene (average number of added moles = 15) alkyl (C12-14) ether (pure content: 90% by mass).
LES solution: Teica Pole NE1230, manufactured by Teika Co., Ltd.
SAS liquid: Hoostup, HOSTAPUR SAS.
Zeolite: Shiruton B, manufactured by Mizusawa Chemical Co., Ltd.
Potassium carbonate: Asahi Glass Co., Ltd., potassium carbonate (powder).
Here, “AI” means a compound contained in a raw material and having a function as a surfactant. For example, it is a by-product generated in the production process of the target surfactant, This includes a compound having a function as an agent.

As the liquid component (B), a mixed liquid in which the raw materials shown in Table 2 were mixed in advance was used.
To the kneader, spray-dried particles (A), liquid component (B), and zeolite and potassium carbonate as other components are continuously fed so as to have the blending ratio shown in Table 2, and mixed and granulated. went. Table 2 shows the mass ratio B / A of the liquid component (B) to the spray-dried particles (A), the value of the stirring power in the kneader (power factor = 0.8), and the spray-dried particles (A ) And the temperature of the cooling water supplied to the cooling jacket of the kneader (inlet temperature). The stirring power was adjusted by changing the temperature of the spray-dried particles (A), the temperature of the cooling water, the paddle pattern of the kneader, and the like.
Table 2 shows the LAS content, the total content of the anionic surfactant, and the content of particles having a particle diameter of 1000 μm or more in the kneaded product (powder) discharged from the kneader.

(Evaluation of solubility)
In order to evaluate the solubility of the kneaded material (powder particles) discharged from the kneader, the following cloth adhesion test was performed.
That is, 30 liters of tap water with a water temperature of 10 ° C. is put into a two-tank washing machine (Mitsubishi Electric, product name: CW-225), two cotton shirts, two black acrylic sweaters, two black nylon slips, A total of 1.5 kg (bath ratio 20 times) of 5 skin shirts as a charge cloth was put, a hollow was made in the center of the cloth to be washed, and 30 g of a sample (powder) was intensively charged there. The sample was allowed to stand for 2 minutes until immersed in water, and then washed with a weak water flow and a washing time of 5 minutes. The sample was naturally drained and dehydrated for 1 minute, and the amount of sample particles adhering to the cloth was visually observed and evaluated according to the following criteria. The evaluation results are shown in Table 2.
0 point: No adhesion.
1 point: A level slightly adhered but improved by rinsing.
2 points: A level at which some adhesion is observed.
3 points: Slightly adhering to the entire fabric, unsatisfactory level after rinsing.
4 points: Adhering to the entire cloth considerably.
5 points: Strongly adhered to the entire cloth.

As shown in the results of Table 2, in Examples 1 to 11, powders were obtained by mixing and granulation using a kneader, and the solubility of the obtained powders was good.
On the other hand, in Comparative Example 1 in which the mass ratio B / A of the liquid component (B) to the spray-dried particles (A) is too large, the obtained kneaded product has a content of particles having a particle diameter of 1000 μm or more of 60% by mass. The solubility was insufficient.
In Comparative Example 2 in which the B / A is too small, the content of particles having a particle diameter of 1000 μm or more is as high as 60% by mass, the solubility is good, but the total content of anionic surfactants is insufficient. Detergency cannot be expected.
In Comparative Examples 3 and 4 in which the stirring power was very large, since the kneaded kneaded product was discharged from the kneader, the solubility was not evaluated.
In Comparative Example 5 where the stirring power was slightly large, the obtained kneaded material had a content of particles having a particle diameter of 1000 μm or more as high as 55% by mass, and the solubility was insufficient.
In Comparative Example 6 having a small stirring power, a granular material was obtained, but its solubility was insufficient. This is considered because it was not mixed uniformly.

It is a perspective view which shows an example of a paddle (stirring blade). It is a front view which shows the other example of a paddle (stirring blade). It is a perspective view which shows the example of the paddle arrangement | positioning in a transport zone. It is a perspective view which shows the example of the paddle arrangement | positioning in a mixing zone. It is a perspective view which shows the example of the paddle arrangement | positioning in a kneading | mixing zone. It is explanatory drawing which shows an example of the paddle arrangement | positioning in a kneading machine. It is explanatory drawing which shows the other example of the paddle arrangement | positioning in a kneading machine.

Explanation of symbols

S ... Screw,
F ... Flat paddle,
H ... Helical paddle.

Claims (2)

Spray-dried particles (A) containing an anionic surfactant and an alkali builder, and having a water content of 3 to 8% by mass;
A liquid component (B) containing an anionic surfactant and / or a nonionic surfactant;
Supply to a kneader having a stirring blade so that the mass ratio B / A of the liquid component (B) to the spray-dried particles (A) is 0.1 to 0.4,
Mix and granulate with a stirring power of 250 to 1000 J / kg to obtain a granule having a content of particles having a particle diameter of 1000 μm or more of less than 50 mass% and a moisture content of 6 to 9 mass%. A method for producing a surfactant-containing particle comprising a step.   The content of the linear alkylbenzene sulfonate in the spray-dried particles (A) is 6.5% by mass or less, and the total content of the anionic surfactant in the granular material is 15 to 28% by mass, and The method for producing a surfactant-containing particle according to claim 1, wherein the content of the linear alkylbenzene sulfonate is 4.5% by mass or less.

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