JPS6169897A - Production of high density detergent improved in flowability - 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 [Industrial Field of Application] The present invention relates to a method for producing a powder detergent having high density and excellent fluidity.

[Conventional technology and problems]

Traditionally, detergents used in the home have been required to have good productivity, be easy to handle, and have good solubility when used by consumers, and for this reason, most detergents have been powdered detergents manufactured by the spray drying method. there were. q Here, ease of handling refers to the fact that the powder has high free-flowing properties and is difficult to consolidate, and that no dust is generated.

However, in recent years, demand for high-density powder detergents has been increasing due to their rationality from a resource-saving perspective and convenience such as ease of portability for consumers. High density refers to powder having an apparent specific gravity of 0.5 g/cm" or more. It is extremely difficult to obtain powder detergent with such high density by conventional spray drying methods.

Generally, the apparent specific gravity of spray-dried detergent particles is 0.4.
g/cm3 or less, average particle size 200-1000 μm
However, it is difficult to directly obtain high-density detergent particles.

On the other hand, the spray drying method has the advantage that any composition containing various raw materials including an anionic surfactant containing a large amount of water can be easily dried, except for thermally unstable components. Therefore, the spray-dried detergent particles are processed to
It has been desired to establish a manufacturing method for producing particles with high density and excellent fluidity.

For example, there is an attempt to obtain a high-density powder detergent by processing spray-dried detergent particles, as disclosed in Japanese Patent Application Laid-Open No. 51-67302.

In JP-A No. 51-67302, spray-drying was carried out using a granulation device called Marmerizer, which includes a substantially horizontal, rotatable rough surface table located inside and at the bottom of a substantially vertical smooth wall surface. Although a manufacturing method for densifying powder detergent has been disclosed and is a pioneering technology of the present invention, no consideration is given to the fluidity of the powder, and as a result, the fluidity of the product is similar to that of the original powder. It is worse than detergents and provides insufficient convenience for consumers.

[Means for solving problems]

Based on the above technical background, we conducted research to produce a high-density powder detergent that exhibits good fluidity, and as a result, we completed the present invention described below.

The present invention relates to a mixer having a vertical stirring shaft, for example, a stirring shaft protruding from the bottom inside a solid mixing tank, and mixing and transferring powder by attaching stirring blades to this shaft, or the inside of this tank. agitated granulation of the spray-dried product of the detergent containing at least one surfactant and at least one builder in the presence of a surface modifier and a binder by a mixer with a chopper for crushing or transferring; The process produces a powdered detergent with high density and excellent fluidity.

Aluminosilicates are preferred as surface modifiers because they act as calcium ion scavengers during washing. Particularly desirable is an aluminosilicate in which the average particle size of secondary particles is 10 μm or less. In addition to aluminosilicate, surface modifiers include silicon dioxide and bentonite with an average particle size of 10 μm or less.

Inorganic fine powders such as talc and clay can be used.

Further, metal soaps having an average particle diameter of 10 μm or less can also be used.

The purpose is achieved by using the surface modifier in an amount of 0.5 to 35 parts by weight per 100 parts by weight of the spray-dried detergent particles. If the surface modifier is less than 0.5 parts by weight, it is difficult to obtain a powder with good fluidity, and if it exceeds 35 parts by weight, fluidity decreases and the amount of binder is unnecessarily reduced. If the amount is not increased, dust may be generated and may damage areas of use by consumers.

Furthermore, the apparent specific gravity of the high-density detergent particles is 0.5 g/cm.
3 or more, preferably 0.5 to 1.2 g/cm3. This is because if the apparent specific gravity is greater than this, it tends to have an adverse effect on the solubility of the powder. Moreover, it is desirable that the average particle size is from 200 to 800 μm, because if the average particle size is less than 200 μm, dust will be generated, and if it exceeds 800 μm, solubility tends to deteriorate. .

Surfactants that can be used in the present invention include the following.

1) Straight chain or branched alkylbenzene sulfonate having an alkyl group with an average carbon number of 10 to 16 2) A straight chain or branched chain alkyl group or alkenyl group having an average carbon number of 10 to 2 o, 1 molecule Average within 0.5-8
Mol of ethylene oxide or propylene oxide or butylene oxide or ethylene oxide/propylene oxide = 0.1/9.9 to 9.9
Alkyl or alkenyl ether sulfate added in a ratio of 70.1 or in a ratio of ethylene oxide/butylene oxide = 0.1/9.9 to 9.910.1 3) Alkyl group or alkenyl having an average carbon number of 10 to 2o Alkyl or alkenyl sulfate having a group 4) Olefin sulfonate having an average of 10 to 20 carbon atoms in one molecule 5) Alkanesulfonate having an average of 10 to 20 carbon atoms in one molecule 6) An average of 10 Saturated or unsaturated fatty acid salt having ~24 carbon atoms in one molecule 7) An alkyl group or alkenyl group having an average of 10 to 20 carbon atoms, and an average of 0.5 to 8 moles of ethylene oxide or Propylene oxide or butylene oxide, or ethylene oxide/propylene oxide = 0.1/9.9 to 9.910.1 ratio, or ethylene oxide/butylene oxide = 0.
Alkyl or alkenyl ether carboxylic acid salt added at a ratio of 1/9.9 to 9.910.1 8) α-Sulfo fatty acid salt or ester represented by the following formula R-CHCOzY 03Z (wherein Y has 1 carbon number ~3 alkyl group or counterion, Z
is the counterion. R represents an alkyl group or alkenyl group having 10 to 20 carbon atoms; 9) An amino acid type surfactant represented by the following general formula (where R3'' represents an alkyl group or alkenyl group having 8 to 24 carbon atoms; , l represents hydrogen or an alkyl group having 1 to 2 carbon atoms, R, l represents an amino acid residue, and X represents an alkali metal or alkaline earth metal ion.) F&L 2 R1'-GO-N (CHz) a-CO
OX♂ R2''(R+',Rz' and X are as described above, n is an integer from 1 to 5 -) (R,' is as described above, 0m is an integer from 1 to 8)
(R,", R1' and Number 6
~28 β-hydroxyalkyl or β-hydroxyalkenyl groups) (US°+ R5 and
Polyoxyethylene alkyl or alkenyl ether to which 1 to 20 moles of ethylene oxide have been added 11) Having an alkyl group with an average carbon number of 6 to 12, 1 to 2
Polyoxyethylene alkyl phenyl ether with 0 mol of ethylene oxide added 12) Polyoxypropylene alkyl or alkenyl group with an average carbon number of 10 to 2 o and with 1 to 20 mol of propylene oxide added Alkaniyl ether 13) Polyoxybutylene alkyl or alkenyl ether having an alkyl group or alkenyl group having an average carbon number of 10 to 20 and added with 1 to 20 moles of butylene oxide 14) An alkyl group having an average carbon number of 10 to 20 Or a nonionic surfactant having an alkenyl group and adding a total of 1 to 30 moles of ethylene oxide and propylene oxide or ethylene oxide and butylene oxide (the ratio of ethylene oxide to propylene oxide or butylene oxide is 0.1/ 9.9-9.910.1)1
5) Higher fatty acid alkanolamide or its alkylene oxide adduct represented by the following general formula R'RIB' (wherein R1' is an alkyl group or alkenyl group having 10 to 20 carbon atoms, and RIZ' is H or CH2, n,
is an integer of 1 to 3, and m3 is an integer of O to 3. ) 16) Sucrose fatty acid ester consisting of a fatty acid having an average carbon number of 10 to 20 and sucrose 17) Fatty acid glycerin heptanoester consisting of a fatty acid having an average carbon number of 10 to 20 and glycerin 18) Alkylamine oxide represented by the following general formula R14" Tatami R,!'-N→0 ■ RIS' (In the formula, RI2° is an alkyl group or alkenyl group having 10 to 20 carbon atoms, and RI4°+I?ts° is an alkyl group or alkenyl group having 1 carbon number.
~3 alkyl group. ) 19) Betaine type amphoteric surfactant Rtz represented by the following general formula (where Ro is an alkyl or alkenyl group having 8 to 24 carbon atoms or β-hydroxyalkyl or β-hydroxyalkenyl group, I?zz is an alkyl or alkenyl group having 8 to 24 carbon atoms, and I?zz has 1 to 24 carbon atoms 4 alkyl group, R2
3 represents an alkyl or hydroxyalkyl group having 1 to 6 carbon atoms. )(CzH*0) n2H (Here, RZI and RZ3 are as described above. n2 is 1 to 2
Indicates an integer of 0. ) 2z4 (Here, RZI and I?zz are as described above. R24 represents a carboxyalkyl or hydroxyalkyl group having 2 to 5 carbon atoms.) 20) Sulfonic acid type amphoteric surfactant 11h l represented by the following general formula R,3 IcI G R++C0NH-Rtz-N R+a 503 (Here, R11 is an alkyl or alkenyl group having 3 to 24 carbon atoms, R, □ is an alkyl group having 1 to 4 carbon atoms, and R13 is an alkyl group having 1 to 5 carbon atoms. The alkyl group, R+4 represents an alkyl or hydroxyalkyl group having 1 to 4 carbon atoms.) ■ RI& (Here, Ro and l?+4 are as described above. RI5+R
I& represents an alkyl or alkenyl group having 8 to 24 carbon atoms or 1 to 5 carbon atoms. ) (CtH*0) nIH (Here, R11 and R14 are as described above, and nl is 1 to 2
Indicates an integer of 0. ) 21) Phosphate ester activator 1 Alkyl (or alkenyl) acidic phosphate ester (R' 0), -P-(OH), - (R' is a furkyl group having 8 to 24 carbon atoms, or alkenyl base, n'tenm'
=3 + n″=1-2) Floor 2 Alkyl (or alkenyl) phosphate ester (R' O) n-P-(OH) 1IN (R' is as described above, n″+m” = 3 r n” = 1 to 3) lVk13 Alkyl (or alkenyl) phosphate ester salt (R″0)7·-P-(OM′), (R′+ n″+ cm″ is as described above, M′ is Na,
K+Ca) 22) A cationic surfactant represented by the following general formula (where at least one of Rl'+ Rt'+ R3'1 R#' is an alkyl or alkyl group having 8 to 24 carbon atoms)
(Here, R1'l R1'+ 1?, l and X' are as described above.) (Here, R1'l R1'+ 1?, l and RI'+ R2'' and X' are as described above, a R5'' is an alkylene group having 2 to 3 carbon atoms, and n o is an integer of 1 to 20.) The surfactant content is 10 to 70% by weight. , preferably 2
It is 5 to 50% by weight.

Further, inorganic builders that can be used in the present invention include the following.

Alkaline salts such as soda carbonate, sodium sesquicarbonate, and sodium silicate, neutral salts such as mirabilite, phosphates such as orthophosphate, pyrophosphate, tripolyphosphate, metaphosphate, hexametaphosphate, and phytate. It can also include aluminosilicates sold externally.

Crystalline aluminosilicate x' (
Mz'0 or M”O) ・Al2O3・V' (SiO
z) ・11' (HzO) (where h' is an alkali metal atom, M'' is an alkaline earth metal atom exchangeable with calcium, x+.

yl, -1 represents the number of moles of each component, generally 0
．． 7 ≦X゛≦1.5.0.8≦y"=6, where ≦y is any integer.) As the magnetic 2 detergent builder, those represented by the following general formula are particularly preferred.

NazO・AlzO,・n5iOz・wH,0 (where n represents a number from 1.8 to 3.0, - represents a number from 1 to 6) Amorphous aluminosilicate x (Mz
O) ・Altos ・Y(SiQz) ・w(HzO
) (In the formula, M represents a sodium and/or potassium atom, and x, y, and w represent the number of moles of each component within the following marginal value range.

0.7≦X≦1.2 1.6≦y≦2.8 W is any positive number including 0) Amorphous aluminosilicate X (M2
O)' AlzOs ・Y(SiOz) ・Z(hO
s) ・ω(H2O) (In the formula, A is Na or K, x,
y, z, - represent the number of moles of each component within the following numerical range.

' 0.20≦X≦1.10 0.20≦Y≦4.00 0.001≦Z≦0.80 W: Any positive number including 0) Furthermore, in the present invention, the following additives Can be used.

(1) Divalent metal ion scavenger 1) Ethane-1,1-diphosphonic acid, ethane-1,2
-) diphosphonic acid, ethane-1-hydroxy-1,1-
Diphosphonic acid and its derivatives, ethanehydroxy-1,
Phosphonate salts such as 1,2-) diphosphonic acid, ethane-1,2-dicarboxy-1°2-diphosphonic acid, and methanehydroxyphosphonic acid.

2) 2-phosphonobutane-1,2-dicarboxylic acid, 1-
Phosphonocarboxylic acid salts such as phosphonobutane-2,3,4-tricarboxylic acid and α-methylphosphonosuccinic acid.

3) Amino acid salts such as aspartic acid and glutamic acid.

4) Nitrilotriacetate, ethylenediaminetetraacetate,
Diethylenetriaminepentaacetate, etc.

Aminopolyacetate of.

5) Polyacrylic acid, polyaconitic acid, polyitaconic acid, polycitraconic acid, polyfumaric acid, polymaleic acid, polymethaconic acid, poly-α-hydroxyacrylic acid, polyvinylphosphonic acid, sulfonated polymaleic acid,
Maleic anhydride-diisobutylene copolymer, maleic anhydride-styrene copolymer, maleic anhydride-methyl vinyl ether copolymer, maleic anhydride-ethylene copolymer, maleic anhydride-ethylene crosslink copolymer,
Maleic anhydride-vinyl acetate copolymer, maleic anhydride-acrylonitrile copolymer, maleic anhydride-acrylic ester copolymer, maleic anhydride-butadiene copolymer, maleic anhydride-isoprene copolymer, maleic anhydride Poly-β-ketocarboxylic acids derived from acids and carbon monoxide, itaconic acid, ethylene copolymers, itaconic acid-aconitic acid copolymers, itaconic acid-maleic acid copolymers, itaconic acid-acrylic acid copolymers , malonic acid-methylene copolymer, methaconic acid-fumaric acid copolymer, ethylene glycol-ethylene terephthalate copolymer, vinylpyrrolidone-vinyl acetate copolymer, 1-butene-2
, 3,4-1-ricarboxylic acid-itaconic acid-acrylic acid copolymer, polyester polyaldehyde carboxylic acid having quaternary ammonium group, cis- of epoxysuccinic acid
isomer, poly(N,N-bis(carboxymethyl)acrylamide), poly(oxycarboxylic acid), starch succinic acid or maleic acid or terephthalic acid ester, starch phosphate ester, dicarboxy starch, dicarboxymethyl starch, carboxy Polyelectrolytes such as methylcellulose and succinate esters.

6) Non-dissociable polymers such as polyethylene glycol, polyvinyl alcohol, polyvinylpyrrolidone, cold water soluble urethanized polyvinyl alcohol.

7) Cyfuricolic acid, oxydisuccinic acid, carboxymethyloxysuccinic acid, cyclopentane-1,2,3,4
-tetracarboxylic acid, tetrahydrofuran-1,2,3
, 4-tetracarboxylic acid, tetrahydrofuran-2,2
, 5,5-tetracarboxylic acid, citric acid, lactic acid, tartaric acid, carboxymethylated products such as Sigll, lactose, raffinose, carboxymethylated products of penquerythritol, carboxymethylated products of gluconic acid, polyhydric alcohols or sugars, and maleic anhydride. Condensates of acids or succinic anhydride, condensates of oxycarboxylic acids and maleic anhydride or succinic anhydride, benzene polycarboxylic acids represented by mellitic acid, ethane-1,1,2,2-
Tetracarboxylic acid, ethene-1.1.2.2-tetracarboxylic acid, butane-L2.3.4-tetracarboxylic acid,
Propane-1,2,3-) IJ carboxylic acid, butane-
1,4-dicarboxylic acid, chelic acid, sulfosuccinic acid, decane-1,10-dicarboxylic acid, sulfotricarballylic acid, sulfoitaconic acid, malic acid, oxydisuccinic acid,
Organic acid salts such as Curconic acid, 0MO3, Builder M, etc.

(2) Re-staining prevention agent The composition may further contain one or more of the following compounds as a re-staining prevention agent in an amount of 0.1 to 5%.

Polyethylene glycol, polyvinyl alcohol, polyvinylpyrrolidone, carboxymethyl cellulose, etc.

(3) Bleach agents such as sodium percarbonate, sodium percarbonate, and sodium sulfate hydrogen peroxide adducts.

(4) Enzymes (enzymes that perform their original enzymatic action during the cleaning process) Classified based on their reactivity, they include hydrolases, hydrolases, oxidoreductases, desmolases, transferases, and isomerases. , both are applicable to the present invention. Particularly preferred are hydrolases, including proteases, esterases, carbohydrases and nucleases.

Specific examples of proteases include pepsin, trypsin, chymotrypsin, collagenase, keratinase, elastase, sptilisin, BPN, papain, promelin,
These are carboxybeptidase A and B, aminopeptidase, and aspergylopeptidase A and B.

Specific examples of esterases include gastric lipase, pancreatic lipase, plant lipases, phospholipases, cholinesterases, and phosphotases.

Carbohydrases include cellulase, maltase, saccharase, amylase, pectinase, lysozyme, α-
Included are glycosidases and β-glycosidases.

(5) Blue tinting agent Various bluing agents can also be added as needed.

For example, the following structure is recommended: (wherein represents a blue to purple monoazo, disazo or anthraquinone dye residue, X and Y are hydroxyl group, amino group, hydroxyl group, sulfonic acid group, carboxylic acid group) group, an aliphatic amino group which may be substituted with an alkoxy group, a halogen atom, a hydroxyl group, a sulfonic acid group, a carboxylic acid group, a lower alkyl group, an aromatic amino group which may be substituted with a lower alkoxy group, or It is a cycloaliphatic amino group.

R is a hydrogen atom or a lower alkyl group. However, this excludes cases in which R represents a hydrogen atom; (i) cases in which X and Y simultaneously represent a hydroxyl group or an alkanolamino group; and (ii) cases in which either one of X and Y is a hydroxyl group and the other is an alkanolamino group. . n represents an integer of 2 or more. ) (In the formula, D represents a blue to purple azo or anthraquinone dye residue, and X and Y represent the same or different alkanol amino residues or hydroxyl groups.) (6) Anti-caking agent para-toluenesulfonic acid salts, xylene sulfonates, acetates, sulfosuccinates, talc, finely divided silica, clays, calcium-silicates (e.g. Johns Man
vil1's microcell, etc.), magnesium oxide, etc.

(7) Antioxidant tert-butylhydroxytoluene, 4.4'-butylidenebis-(6-tert-butyl-3-methylphenol')
, 2.2''-butylidenebis-(-tert-butyl-4-methylphenol), monostyrenated cresol, distyrenated cresol, monostyrenated phenol, distyrenated phenol, 1,1°-bis-(4-hydroxyphenyl) ) Antioxidants such as cyclohexane.

(8) Fluorescent dye 4.4°-bis-(2-sulfostyryl)-biphenyl salt, 4.4''-bis-(4-chloro-3-sulfostyryl)-biphenyl salt, 2-(styrylphenyl) Naphthothiazole derivative, 4.4°-bis(triazole-2
The composition may contain 0 to 1% by weight of one or more of the following: -yl) stilbene derivatives and bis(triazinylamino)stilbene disulfonic acid derivatives.

(9) Photoactivated bleach One or two of sulfonated aluminum phthalocyanine and sulfonated zinc phthalocyanine are added to the composition in an amount of 0 to 0.
It can be contained in an amount of 2% by weight.

Binders that can be used in the present invention include carboxymethyl cellulose, polyethylene glycol, water-soluble polymer solutions such as polycarboxylic acid salts such as sodium polyacrylate, polyoxyethylene alkyl ether, fatty acid monoethanolamide, fatty acid jetanol, etc. Examples include nonionic substances such as amides, aqueous sodium silicate solutions, and water.

In practicing the present invention, spray-dried detergent particles can be obtained as follows. That is, thermally unstable raw materials,
For example, it consists of anionic surfactant solutions, aluminosilicate slurries, fluorescent dyes, pigments, etc. that require drying, excluding enzymes, bleaching agents, and inorganic builders that do not require drying, such as sodium carbonate and sodium sulfate. Spray dry the slurry. If the spray-dried particles are highly sticky, it is optional to incorporate sodium carbonate, sodium sulfate, sodium silicate, etc. into the detergent slurry.

The apparent specific gravity and particle size of the spray-dried detergent particles do not matter. The water content is preferably 12% or less. If there is more water than that, it will have a negative effect on the fluidity of the particles after granulation.

Next, the granulation process in the method of the present invention will be explained.

The granulation treatment method in the present invention basically consists of the following two steps.

i Crushing process Spray-dried detergent particles are mixed in a solid mixing tank with a vertical stirring shaft, for example, a stirring shaft protruding from the bottom, and a stirring blade attached to this shaft to mix the powder. The apparent specific gravity is 0.05 to 0.05 lower than the original particle.
Grind until the size is 0-3g/ca+3. At this time, if the temperature of the powder exceeds 60 degrees Celsius, the stickiness of the powder will increase and agglomeration will occur.In order to avoid this, it is effective to provide a jacket around the mixer and run cold water through it.

In this step, other inorganic and/or organic raw materials of the detergent other than the spray-dried product may be mixed.

ii Stirring granulation step Following the above steps, stirring and granulation is carried out while adding a surface modifier and a binder. The surface modifier and the binder may be added at the same time, one of them may be added first, or they may be added alternately.

In this step, it is optional to mix other inorganic and/or organic raw materials of the detergent.

Examples of mixers used in the present invention include high-speed mixers (stirring transfer granulators) and Henschel mixers (
(high-speed stirring granulator) can be used.

The detergent particles produced by the present invention can be easily distinguished from detergent particles produced by other methods because they have the following two characteristics.

One of these is that the particle surface is covered with a surface modifier, which can be easily confirmed by observation with an electron microscope.

Another feature is that the detergent particles of the present invention are composed of mechanically broken, spray-dried particles. This is easy because when detergent particles are soaked in ethyl alcohol, the detergent particles of the present invention become a fine powder and disperse, whereas particles of laundry detergent spray-dried on cars do not disperse in this way. It can be confirmed.

〔Example〕

Examples of the present invention are shown below, but these Examples do not limit the present invention.

Example 1 A detergent having the following composition was spray dried.

Linear alkylbenzene sulfonate 35 Parts by weight Alkyl sulfate ester salt 10 Sodium carbonate 21.5 Sodium silicate 7 Sodium aluminosilicate 14 Sodium sulfate
3 Nonionic surfactant 3
．． 5 ~ Moisture 6 〃
The detergent particles obtained had an average particle size of 600 μm and an apparent specific gravity of 0.31 g/m 7 .

100 parts by weight of the spray-dried detergent particles were placed in a high-speed mixer (manufactured by Fukae Kogyo Co., Ltd.), stirred and pulverized for 10 minutes, and the apparent specific gravity was 0.43 g/ml and the average particle size was 1.
It became 30 μm. Next, 2 parts by weight of water and 4 parts by weight of aluminosilicate fine powder having an average particle size of 2.7 μm were added, and after granulation with stirring, coarse particles were removed using a 16-mesh sieve.

The apparent specific gravity, average particle size, and fluidity of the detergent thus obtained were measured and are shown in Table 1 together with other Examples and Comparative Examples.

Here, the fluidity of the powder is determined by measuring the time required for 100-g of powder to flow out from a hopper for measuring specific gravity as specified in JIS K 3362, and the shorter the time, the greater the fluidity. is judged to be good.

Example 2 A detergent having the following composition was spray dried.

Linear alkylbenzene sulfonate 35 parts by weight Alkyl sulfate ester salt 10 Sodium carbonate 30 Sodium silicate
7 Sodium aluminosilicate
9 Sodium sulfate
3 Moisture 6
The average particle diameter of the obtained detergent particles was 500 μm, and the apparent specific gravity was 0.34 g/ff+7. This detergent particle 10
0 parts by weight was placed in a high-speed mixer (manufactured by Fukae Kogyo Co., Ltd.), stirred and ground for 10 minutes, and the apparent specific gravity was 0.44 g.
/m7, and the average particle size was 110 μm. Next, 4.6 parts by weight of a nonionic surfactant and 17 parts by weight of aluminosilicate fine powder having an average particle size of 2.7 μm were added, and granulation was performed with stirring. After removing coarse particles using a 16-mesh sieve, specific gravity, average particle size, and fluidity were measured.

Example 3 100 parts by weight of the spray-dried detergent particles used in Example 1 were placed in a high-speed mixer (manufactured by Fukae Kogyo Co., Ltd.), stirred and pulverized for 10 minutes, and the apparent specific gravity was 0.43 g/rn.
! , ``The average particle size was 130 μm. Next, 2 parts by weight of water and 1 part by weight of silicon dioxide fine powder having a particle size of 20 mμ (0.02 μm) were added, and after stirring and granulation, coarse particles were removed using a 16-mesh sieve.

Example 4 In Example 3, 2 parts by weight of the same aluminosilicate and 2 parts by weight of talc fine powder having an average particle size of 1.5 μm were used in place of the silicon dioxide fine powder.

Comparative Example 1 In Example 1, stirring granulation was performed without adding a surface modifier.

Comparative Example 2 In Example 1, the same aluminosilicate as in Example 1 was
0 parts by weight was added and granulation was performed with stirring.

As is clear from the above Examples and Comparative Examples, according to the production method of the present invention, a granular detergent with high density and excellent fluidity can be obtained.

Claims (1)

[Claims] 1. At least one type of surfactant and at least one type of surfactant are mixed by a mixer having a vertical stirring shaft inside a rigid mixing tank and a stirring blade attached to the shaft to mix powders. A method for producing a high-density granular detergent with improved fluidity, characterized in that a spray-dried detergent product containing a seed builder is subjected to agitation granulation treatment in the presence of a surface modifier and a binder. 2. The manufacturing method according to claim 1, wherein the surface modifier is an aluminosilicate. 3. The manufacturing method according to claim 2, wherein the aluminosilicate has an average primary particle diameter of 10 μm or less. 4 The surface modifier is silicon dioxide with an average diameter of 10 μm or less,
The manufacturing method according to claim 1, which is an inorganic fine powder such as bentonite, talc, or clay. 5. The manufacturing method according to claim 1, wherein the surface modifier is a metal soap having an average diameter of 10 μm or less. 6 0 parts of surface modifier per 100 parts by weight of spray-dried product
．． The method according to any one of claims 1 to 5, wherein the amount is 5 to 35 parts by weight. 7. The manufacturing method according to any one of claims 1 to 6, in which a powder or granular inorganic raw material or (and) organic raw material other than the spray-dried product is added and granulation is performed at the same time.