JP2003105398A - Method for producing granular detergent composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method for producing a granular detergent composition prevented from attaching on a pulverizer or the like. SOLUTION: The method for producing a granular detergent composition comprises producing the granular detergent composition by pulverizing a solid detergent containing a surfactant and a builder. When the values of hardness and strain (displacement) are in the region of Fig. 1 (a), the pulverization treatment is carried out by supplying air of >=26 deg.C and at a peripheral speed of a pulverizer's rotor of <=50 m/s; when they are in the region of Fig. 1 (b), by supplying air of <=25 deg.C; and when they are in the region of Fig. 1 (c), at a peripheral speed of a pulverizer's rotor of <=50 m/s.

Description

DETAILED DESCRIPTION OF THE INVENTION [0001] BACKGROUND OF THE INVENTION 1. Field of the Invention
The present invention relates to a method for producing a granular detergent composition which avoids trouble.
You. [0002] 2. Description of the Related Art Japanese Patent Publication No. 08-16235 discloses
Is a particle having a particle size of 50 μm or less (preferably 20 μm or less).
A crushing aid is added in an amount of 0.5 to 10% by mass based on the material to be crushed.
Reduces the surface activity of the material to be crushed,
Techniques for preventing the adhesion of odor have been proposed. In addition,
JP-A-09-13086 discloses the production of granulated bleach activator.
Method, ie, crushing of extruded granules at least 45 ° C
Using a granulator, inorganic powder with an average particle size of 20 μm or less
% Of the crushed product while blowing cold air at 20 ° C or less.
By crushing and granulating so that the temperature is 35 ° C or less, crushing
Techniques for preventing machine adhesion have been proposed. Further, JP
No. 000-1696 discloses the production of a bleaching activator granulated product.
Method, that is, a water-soluble inorganic electrolysis having an average particle size of 20 to 50 μm.
Particles and cold air with a temperature of 20 ° C or less and a humidity of 60% or less
With crusher by crushing and granulating while supplying to crusher
Techniques for preventing wearing have been proposed. JP-A-09-10
No. 0497 discloses that iminodisuccinate is contained in detergent dough.
Crushing equipment or screen
There has been proposed a technique for preventing the adhesion to the surface. However, the aim is to further improve the adhesion of the crusher.
When the amount of crushing aid added increases, the adhesion of the crusher
Although improved, the flow of crushed material obtained by increasing the fines
There is a problem that causes deterioration of mobility. Also
High content of minodisuccinates absorbs moisture into detergent
And the fluidity deteriorated, causing a problem. [0004] SUMMARY OF THE INVENTION The present invention
Tasks to solve the problems in
The title. That is, the present invention is to deteriorate the powder properties
Of a granular detergent composition that has been prevented from adhering to a crusher, etc.
It is intended to provide a manufacturing method. [0005] Means for Solving the Problems The present inventor has made intensive studies.
As a result, it contains at least a surfactant and a builder
A solid detergent is crushed to produce a granular detergent composition.
At this time, the relationship between hardness and strain (displacement) in the solid detergent
Are divided into three regions as shown in FIG.
And setting the crushing conditions for each area
Adhesion to crusher without deteriorating powder properties
Was found to be able to be prevented. That is, as means for solving the above problems,
Is as follows. <1> Contains at least a surfactant and a builder
Granules obtained by crushing a solid detergent to produce a granular detergent composition
A method for producing a detergent-like composition, the hardness of the solid detergent and
Depending on the value of strain (displacement), any of the following (a) to (c)
Granular detergent set characterized by crushing under any of these conditions
This is a method for producing a product. (A): The hardness of the solid detergent is 50 ≦ hardness
[G] <1000, strain (displacement) is 1.0 ≦ strain
(Displacement) When [mm] <2.5 is satisfied and solid washing
When the hardness of the agent is 1000 ≦ hardness [g] ≦ 3000, strain
(Displacement) is 1.0 ≦ strain (displacement) [mm] <4.8
When it is satisfied, supply hot air of 26 ° C or more to the crusher,
Reduce the peripheral speed of one or more crushing granulator rotating bodies to 50 m / s or less
Set and crush processing. (B): The hardness of the solid detergent is 50 ≦ hardness [g] <1000
And the strain (displacement) is 5.0 ≦ strain (displacement) [mm] ≦
8.0 and the hardness of the solid detergent is 1000
≤ hardness [g] ≤ 3000 and strain (displacement) 4.8 ≤
If the displacement (displacement) [mm] ≦ 8.0 is satisfied, 25
Crushed air is supplied to the crusher at a temperature of less than ℃. (C): The hardness of the solid detergent is 50 ≦ hardness [g] <1000
And the strain (displacement) is 2.5 ≦ strain (displacement) [mm] <
When 5.0 is satisfied, one or more crushing granulator rotating bodies
Crushing process with peripheral speed set to 50m / s or less. [0008] BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in detail.
In the method for producing a granular detergent composition of the present invention,
The detergent is crushed under predetermined conditions to produce a granular detergent composition.
You. [Solid detergent] The above-mentioned solid detergent is used in the present invention.
In addition, kneaded (kneaded) material, or stirring granulation, rolling granulation
Refers to the granulated material before the crushing treatment. -Composition of solid detergent- The solid detergent contains a surfactant and a builder.
Contains other components as needed. -Surfactant- As the surfactant, anionic surfactant, nonionic surfactant
Surfactants, cationic surfactants, and amphoteric surfactants
And the like. As the anionic surfactant, conventionally,
It is particularly limited as long as it is used in detergents.
Without known various anionic surfactants
You. For example, the following anion fields (1) to (12)
Surfactants. (1) having an alkyl group having 8 to 18 carbon atoms
Linear or branched alkylbenzene sulfonate (L
AS or ABS). (2) An alkane sulfonate having 10 to 20 carbon atoms. (3) α-olefin sulfonate having 10 to 20 carbon atoms
(AOS). (4) Alkyl sulfate or alkenyl having 10 to 20 carbon atoms
Sulphate (AS). (5) A linear or branched alkyl group having 10 to 20 carbon atoms
Or having an alkenyl group, on average 0.5-10 mol
Ethylene oxide, propylene oxide, butylene
Oxide and ethylene oxide and propylene
Oxide (molar ratio: 0.1 / 9.9 to 9.9 / 0.9.
Alkyl ether to which at least one of 1) is added
Sulphate or alkenyl ether sulphate (AE
S). (6) Straight or branched chain having 10 to 20 carbon atoms
Is an alkylphenyl or alkenylphenyl group
Having an average of 3 to 30 moles of ethylene oxide and propylene.
Len oxide, butylene oxide, and ethylene
Oxide and propylene oxide (molar ratio: 0.1
/9.9 to 9.9 / 0.1)
Alkyl phenyl ether sulfate or Al
Kenyl phenyl ether sulfate. (7) A linear or branched alkyl group having 10 to 20 carbon atoms
Or having an alkenyl group, on average 0.5-10 mol
Ethylene oxide, propylene oxide, butylene
Oxide and ethylene oxide and propylene
Oxide (molar ratio: 0.1 / 9.9 to 9.9 / 0.9.
Alkyl ether to which at least one of 1) is added
Carboxylate or alkenyl ether carboxylate. (8) Alkyl glycer having 10 to 20 carbon atoms
Alkyl polyhydric alcohols such as
-Sulfate. (9) Saturated or unsaturated α-sulfo fat having 8 to 20 carbon atoms
Acid salt or its methyl ester, ethyl ester, or
Is a propyl ester (α-SF or MES). (10) Long-chain monoalkyl phosphate, dialkyl phosphoric acid
Salt or sesquialkyl phosphate. (11) polyoxyethylene monoalkyl phosphate,
Lioxyethylene dialkyl phosphate or polyoxy
Siethylene sesquialkyl phosphate. (12) Higher fatty acid salts having 10 to 20 carbon atoms. The anionic surfactant is sodium,
Alkali metal salts such as potassium, amine salts, ammonium
It may be used as a salt or the like. The anionic surfactant
May be used alone or in combination of two or more.
Good. Among the anionic surfactants, for example, linear
Alkali metal of alkylbenzene sulfonic acid (LAS)
Salt (eg, sodium or potassium salt), AO
Alkali metal salts of S, α-SF and AES (for example,
Lium or potassium salts), alkali metals of higher fatty acids
Salts (eg, sodium or potassium salts) are preferred
No. As the nonionic surfactant, conventionally,
It is particularly limited as long as it is used in detergents.
Without known various nonionic surfactants
You. For example, the nonionic field shown in the following (1) to (11)
Surfactants. (1) C6 to C22 (preferably carbon
The aliphatic alcohols of formulas 8 to 18) are
The alkylene oxide is used in an amount of 3 to 30 mol on average (preferably,
5 to 20 mol) added polyoxyalkylene alkyl
(Or alkenyl) ether. Among these, polio
Xylene ethylene (or alkenyl) ether,
Lioxyethylene polyoxypropylene alkyl (or
Alkenyl) ethers and the like are preferred. Used here
As aliphatic alcohols, primary alcohols and secondary alcohols
And primary alcohols are preferred.
No. Further, the alkyl group may have a branched chain.
No. (2) Polyoxyethylene alkyl (or
Alkenyl) phenyl ether or long-chain fatty acid alkyl
Alkylene oxide between the ester bonds of the kill ester
A fatty acid alkyne represented by the following general formula (I)
Ester alkoxylate. Formula (I) R¹CO (OA)_nOR² In the general formula (I), R¹CO has 6 to 22 carbon atoms.
(Preferably 8 to 18) fatty acid residues. OA is
2 to 2 carbon atoms such as ethylene oxide and propylene oxide
4 (preferably 2 to 3) alkylene oxide addition units
Represents the position. n is the average number of moles of alkylene oxide added
And generally 3 to 30 (preferably a number of 5 to 20)
is there. R²Is low which may have a substituent having 1 to 3 carbon atoms.
Represents a lower alkyl group. [0021] (3) Polyoxyethylene sorbitan fatty acid esters. (4) Polyoxyethylene sorbite fatty acid ester. (5) Polyoxyethylene fatty acid esters. (6) Polyoxyethylene hydrogenated castor oil. (7) Glycerin fatty acid ester. (8) fatty acid alkanolamides. (9) Polyoxyethylene alkylamine. (10) Alkyl glycosides. (11) Alkylamine oxide. Among the above nonionic surfactants, the melting point is
Polyoxyethylene alcohol having an HLB of 9 to 16 at 40 ° C or lower
Alkyl (or alkenyl) ether, polyoxyethylene
Polyoxypropylene alkyl (or alkenyl)
Ethylene oxide in ether and fatty acid methyl ester
Added fatty acid methyl ester ethoxylate, fatty acid
Ethylene oxide and propyleneoxy to methyl ester
Fatty acid methyl ester ethoxypropoxy
The rate is preferred. These nonionic surfactants
One type may be used alone, or two or more types may be used in combination.
No. As the above-mentioned cationic surfactant, conventionally,
It is particularly limited as long as it is used in detergents.
Without known various cationic surfactants
You. For example, the cation interface shown in the following (1) to (4)
Activators and the like. (1) Dilong chain a represented by the general formula (II)
Lucildi short chain alkyl type quaternary ammonium salt. General formula (II) [0025] Embedded image In the general formula (II), R¹And R
²Has usually 12 to 26 carbon atoms (preferably 14 to 1
8) represents an alkyl group. R³And R⁴Is usually the carbon number
Is an alkyl group of 1-4 (preferably 1-2), benzyl
Group, usually having 2 to 4 (preferably 2 to 3) carbon atoms
Xylalkyl group or polyoxyalkylene group
It represents this. X is halogen, CH₃SO₄, C₂H₅
SO₄, 1 / 2SO₄, OH, HSO₄, CH₃CO₂
And CH₃-C₆H₄-SO₃Represents any of The above-mentioned di-long-chain alkyl di-short-chain alkyl type quaternary
As the ammonium salt, specifically, distearyl di
Methyl ammonium salt, dihydrogenated tallow alkyl dimethyla
Ammonium salt, dihydrogenated beef tallow alkylbenzene methylan
Monium salt, distearylmethylbenzylammonium
Salt, distearyl methyl hydroxyethyl ammonium
Salt, distearylmethylhydroxypropylammonium
Salt, distearyl dihydroxyethyl ammonium
Salt, dioleyl dimethyl ammonium salt, coconut
Alkyl dimethyl ammonium salts and the like. or,
Specific examples of the halogen represented by X include a chlorine atom, bromine
Atoms and the like. (2) Mono-length represented by the general formula (III)
Chain alkyl tri-short chain alkyl type quaternary ammonium salt. General formula (III) [0029] Embedded image In the general formula (III), R¹Is
Usually, an alcohol having 12 to 26 (preferably 14 to 18) carbon atoms
Represents a alkyl group. R², R³And R⁴Is usually the number of carbon atoms
Is an alkyl group of 1-4 (preferably 1-2), benzyl
Group, usually having 2 to 4 (preferably 2 to 3) carbon atoms
Xylalkyl group or polyoxyalkylene group
It represents this. X is halogen, CH₃SO₄, C₂H₅
SO₄, 1 / 2SO₄, OH, HSO₄, CH₃CO₂
And CH₃-C₆H₄-SO₃Represents any of ) The above-mentioned mono long chain alkyl tri short chain alkyl type
As the quaternary ammonium salt, for example, lauryl trime
Tylammonium salt, stearyltrimethylammonium
Um salt, hydrogenated tallow alkyltrimethylammonium salt,
Hydrogenated beef tallow alkylbenzene dimethyl ammonium salt,
Tearyl dimethyl benzyl ammonium salt, stearyl
Dimethyl hydroxyethyl ammonium salt, stearyl
Dimethyl hydroxypropyl ammonium salt, steari
Rutrihydroxyethylammonium salt, oleyltri
Methyl ammonium salt, coconut alkyl trimethyl
Ammonium salts and the like. Also, halo represented by X
Examples of the gen include a chlorine atom and a bromine atom. (3) Tetra short represented by the general formula (IV)
Chain alkyl type quaternary ammonium salts. General formula (IV) [0033] Embedded imageIn the general formula (IV), R¹~ R⁴
Is usually an alkyl having 1 to 4 (preferably 1 to 3)
A kill group or a benzyl group, usually having 2 to 4 carbon atoms (preferably
Is a hydroxyalkyl group of 2-3) and polyoxy
Represents any of alkylene groups. X is a halogen element,
CH₃SO₄, C₂H₅SO₄, 1 / 2SO₄, OH,
HSO₄, CH₃CO₂, And CH₃-C₆H₄-S
O₃Represents any of The above-mentioned tetra short chain alkyl type quaternary ammonium
For example, tetramethylammonium chloride
Ride, tetraethylammonium chloride, tetra
Butyl ammonium bromide, tetrabutyl ammonium
Tetrabutylammonium hydroxide
Gensulfate, benzyltrimethylammonium
Chloride, benzyltrimethylammonium hydroxy
Side, benzyltriethylammonium chloride,
Benzyl tributyl ammonium bromide, benzyl
Tributyl ammonium chloride, trimethyl phenyl
Ruammonium chloride and the like. (4) Tri long chain a represented by the general formula (V)
Alkyl mono short chain alkyl type quaternary ammonium salt General formula (V) [0037] Embedded image In the general formula (V), R¹~ R³Is
Al having 12 to 26 (preferably 14 to 18) carbon atoms
Represents a kill group. R⁴Has usually 1 to 4 carbon atoms (preferably
Is an alkyl group or benzyl group of 1-2), usually having 2 carbon atoms.
-4 (preferably 2-3) hydroxyalkyl groups, and
And any of polyoxyalkylene groups. X is
Halogen element, CH₃SO₄, C₂H₅SO₄, 1/2
SO₄, OH, HSO ₄, CH₃CO₂And CH₃-C
₆H₄-SO₃Represents The above tri long chain alkyl mono short chain alkyl type
As quaternary ammonium salts, for example, trilaurylme
Tylammonium chloride, tristearyl methyl alcohol
Nmonium chloride trioleyl methyl ammonium
Chloride, tricoconut alkyl methyl ammonium
Muchloride and the like. As the amphoteric surfactants, there are conventionally known detergents.
If it is used in
And various known amphoteric surfactants. example
For example, the following amphoteric surfactants shown in (1) to (3) are mentioned.
Can be (1) Betaines. For example, lauric acid
Midopropyl betaine, amide ethyl stearate beta
In, carbobetaine, sulfobetaine, etc.
You. (2) imidazoline derivatives. For example, 2-alkyl-
N-carboxymethyl-N-hydroxyethylimidazo
Linium betaine, N-coconut fatty acid acyl-N-cal
Boxyethyl-N-hydroxyethylethylenediamine
Sodium and the like. (3) Phosphate type phosphate type. For example, lecithin (phos
Fatidylcholine and the like. These amphoteric surfactants
The sexual agent may be used alone or in combination of two or more.
May be. --- Builder-- Examples of the builder include a chelate builder and an builder.
Lucari builder and neutral builder. As the chelate builder, A-type zeo
Light, P-type zeolite, X-type zeolite, amorphous zeolite
Aluminosilicates such as light;
Condensed phosphoric acid such as lithium metal salts and alkali metal salts of pyrophosphoric acid
Salt; alkali metal salt of citric acid, ethylenediaminetetravinegar
Acid alkali metal salts (EDTA), nitrilotriacetic acid
Lucari metal salt (NTA), alkali gold of polyacrylic acid
Genus, copolymers of acrylic acid and maleic anhydride
Limetal salt, polyacetal carboxylate, hydroxy
Organic builders such as alkali metal salts of siminodisuccinic acid
ー; and the like. These can be used alone
Well, two or more kinds may be used in combination. The alkali builder includes sodium carbonate
Lium, potassium carbonate, sodium hydrogen carbonate, hydrogen carbonate
Alkali metal charcoal such as potassium and sodium potassium carbonate
Acid salt: sodium silicate (water glass), layered sodium silicate
Alkali metal silicates such as these
May be used alone or in combination of two or more.
Good. As the neutral builder, sodium sulfate
Sulfates such as potassium and potassium sulfates; sodium chloride, potassium chloride
Chlorides such as lithium; and the like. These are single types
They may be used alone or in combination of two or more. --- Other components-- As the other components, usually blended in detergent raw materials
Any optional component, without any particular restrictions.
Can be used. As such components
Examples include the following components. These are one kind
They may be used alone or in combination of two or more. (1) Recontamination inhibitor Carboxymethyl cellulose, polyethylene glycol
, Polyvinyl alcohol, polyvinyl pyrrolidone, etc. (2) viscosity modifier P-toluenesulfonate, toluenesulfonate,
Silene sulfonate, urea and the like. (3) Softener Quaternary ammonium salt, montmorillonite, saponai
, Hectorite, smectite such as stevensite
Minerals, etc. (4) Reducing agent Sodium sulfite, sodium bisulfite and the like. (5) Bleach Sodium percarbonate, sodium perborate, sodium sulfate
Hydrogen peroxide adducts and the like. (6) Bleaching activator Ethylenediaminetetraacetate, octanoyloxy
Sodium sibenzenesulfonate, dodecanoyloxy
Sodium benzenesulfonate, decanoyloxybe
Benzenecarboxylic acid and the like. (7) Optical brightener 4,4'-bis- (2-sulfostyryl) -biphenyl
Salt, 4,4'-bis- (4-chloro-3-sulfostili
B) -biphenyl salt, 2- (styrylphenyl) naphtho
Thiazole derivative, 4,4'-bis (triazole-2
-Yl) stilbene derivatives, bis (triazinylamido)
No.) Stilbene disulfonic acid derivatives and the like. (8) Fragrance C10-C15 alcohol, C7-C10 fragrance
Aliphatic alcohol, formic acid ester having 8 to 17 carbon atoms or acetic acid
Ester, C10-C15 hydrocarbon, C7-1
5 aromatic aldehydes, aliphatic alde having 8 to 14 carbon atoms
Hyd, phenolic fragrance, etc. (9) Enzyme Protease, lipase, cellulase, amylase and the like. (10) Dye Ultramarine, Koranil Green CG-130 (CI number:
74260), Food Color Red No. 102, Acid Dye Acid
De yellow 141 and the like. (11) Oil-absorbing carrier Amorphous silicate, white carbon, amorphous calcium silicate
, Amorphous aluminosilicate, magnesium silicate,
Gnesium, calcium carbonate, spinel, cordiera
Litter, mullite, starch decomposition products, etc. (12) Surface modifier Fine calcium carbonate, fine zeolite, fine silica, fine
Powdered alumina, finely powdered starch, clay mineral, polyethylene
Recall etc. (13) Foam inhibitor Silicone, silicone compound, wax, etc. (14) Antioxidant Tertiary butyl hydroxytoluene, 4,4'-butylidene
Bis- (6-tert-butyl-3-methylphenol),
2,2'-butylidenebis- (6-tert-butyl-4-me
Tylphenol), monostyrenated cresol, dist
Cresol, styrene, monostyrenated phenol, dist
Renated phenol, 1,1'-bis- (4-hydroxy
Phenyl) cyclohexane and the like. (15) Photoactivated bleach Sulfonated aluminum phthalocyanine, sulfonated aluminum
Lead phthalocyanine and the like. -Preparation of solid detergent- As described above, the solid detergent may be kneaded (kneaded) or
Refers to the granulated material before crushing treatment by stirring granulation or tumbling granulation.
You. In the method of preparing the solid detergent, it is usually performed
Known drying step, concentration step, and known granulation step
(However, it is preferable to have after the crushing process.)
No. --- Drying Step-- In the drying step, a detergent slurry is prepared and dried.
You. (1) Preparation of detergent slurry When preparing the solid detergent, in the detergent slurry
Preferably has a water content of 30 to 60% by mass,
More preferably 0 to 50% by mass, 35 to 45 mass
More preferably, the amount is%. The water content is 30 mass
%, The viscosity of the detergent slurry increases,
Problems may occur with the ring. In addition, water-soluble inorganic
Ruder, the inorganic builder remains undissolved.
Cause problems such as aggregation or sedimentation
Sometimes. On the other hand, the water content exceeds 60% by mass.
And the energy required for drying is increased,
May be disadvantageous. As the amount of the surfactant in the detergent slurry,
Is preferably not more than 60% by mass, and not more than 50% by mass.
More preferably, it is below. When the amount of the surfactant is 60,
If the amount exceeds the mass%, atomization of the slurry at the nozzle outlet may occur.
It may worsen, leading to a decrease in drying efficiency. Washing
The amount of inorganic builder in the agent slurry is 15 to 70
%, Preferably 20 to 65% by mass.
More preferred. The amount of the inorganic builder is less than 15% by mass.
, The viscosity of the slurry increases, and the
Poor slurry atomization leading to poor drying efficiency
On the other hand, if the content exceeds 70% by mass,
May cause problems such as agglomeration or settling.
There is. Preparation method of detergent slurry and addition of composition
There are no particular restrictions on the order of addition, and any preparation method, etc.
Are also suitable. However, linear alkyl benzene sulfone
Acid salt, alpha sulfo fatty acid ester salt, alkali builder,
And zeolites are included,
As described in JP 4-349787, linear
Add the slurry containing the alkylbenzene sulfonate to an alkali
After adding rebuilder or zeolite, alpha sulfo fat
It is preferred to add an acid alkyl ester salt. The temperature at which the detergent slurry is prepared is
Is preferably 50 to 90 ° C, more preferably 55 to 85 ° C.
More preferably, 55 to 80 ° C. is more preferable. The detergent slurry
It is also advisable to circulate at the same time as stirring when preparing
New Circulation facilitates slurry mixing
Thus, problems such as precipitation of the inorganic builder can be solved. Also, special
Unneutralized as described in Japanese Patent Application No. 07-184928.
When neutralizing the anionic surfactant at the time of slurry preparation
From the circulation line where the shear force of the pump is available.
Preferably. The viscosity of the detergent slurry (Brook fee)
Model (measured with a viscometer (B type))
In view of the above, the pressure is preferably 30 Pa · s or less.
Pa · s or less is more preferable, and 20 Pa · s or less
More preferably, it is below. After adding all the components of the detergent slurry,
The stirring time until drying is not particularly limited.
However, 3 min or more is preferable, and 5 min or more is more preferable.
New If this time is less than 3 minutes, especially inorganic
Dissolution residue of rudder increases, dissolving high bulk density granular detergent
May be reduced. (2) Drying of detergent slurry The method for drying the detergent slurry is not particularly limited.
However, due to the ability to dry a large amount of detergent slurry, spray drying
Particularly preferred. As a spray drying tower used for the spray drying
Can be either countercurrent or cocurrent,
Counter-current type because it can dry dried powder to low moisture
Is preferred. The temperature of the hot gas supplied to the spray drying tower
Then, usually 150 to 350 ° C. is preferable, and 170 to 350 ° C.
300 ° C is more preferred, and 200 to 280 ° C is even more preferred.
New If it exceeds 350 ° C., when continuous operation is performed,
Organic matter in the solid matter adhering to the spray drying tower burns.
And may cause trouble. Also spray drying
The temperature of the gas discharged from the tower is usually 70 to 1
25 ° C is preferred, and 70 to 115 ° C is more preferred. 1
If the temperature exceeds 25 ° C, the thermal efficiency of the spray drying tower decreases.
There is. In the case of countercurrent drying, the temperature of the resulting dry powder
May be high, and if the temperature of the dry powder is high, the flowability may deteriorate.
-Adhesion etc. become a problem. In this case, cool down from the bottom of the drying tower.
The powder temperature can be lowered by introducing wind. Ma
At the same time, inorganic fine particles were introduced from the bottom of the hot air outlet,
By contacting with dry particles,
Prevents adherence to the wall of the medical part and prevents the flow of detergent particles.
Mobility can be improved. The detergent slurry atomizer includes:
Pressure spray nozzle, 2 fluid spray nozzle, rotating disk type
The average particle size of the dried powder (“Sieve
Weight average particle size ”. Hereinafter, the same applies. ) Is 1
00 to 700 μm (preferably 150 to 500 μm)
Because of this, a spray device that can obtain the average particle size
In particular, a pressure spray nozzle is particularly preferred. As the shape of the pressure spray nozzle,
There are no restrictions, for example, Japanese Utility Model Publication No. 40-26461,
No. 40-27165, Japanese Patent Publication No. 41-16342, actual
No. 53-24510, Japanese Patent Publication No. 55-39376,
JP-A-04-63154, JP-A-09-75786
And the like. When spraying
The pressure is 15 to 45 kg / cm²Is preferred, and 2
0-40kg / cm²Is more preferred. Detergent when spraying
The temperature of the rally is the same as the temperature during preparation of the detergent slurry,
There is no particular limitation. (3) Dried powder The temperature of the dry powder obtained by drying the detergent slurry
Is preferably 55 ° C or less, more preferably 50 ° C or less.
No. When the temperature exceeds 55 ° C., organic components in the dried powder soften,
The fluidity of the dried powder may deteriorate. The dried powder
As properties, a bulk specific gravity of 0.10 to 0.50 g / cc is preferred.
New In terms of handling, the angle of repose is 6
0 ° or less is preferable, and 55 ° or less is more preferable. The cheap
When the angle of repose exceeds 60 °, the discharge from silos etc. becomes significant.
May worsen. --- Concentration step-- In the concentration step, in the drying step, consideration is given to the environment.
It is preferably provided to reduce the load on the drying tower.
No. This involves drying the detergent slurry in the drying step.
Exhaust gas generated by the use of a drying tower
Because it contains volatile components from activators, etc.
The surfactant that was blended into the
Reduced and dried the resulting concentrate and other ingredients
Dry granules can be mixed in the granulation process to obtain detergent granules.
You. (1) Concentration method In the concentration step, the concentration method is not particularly limited.
For example, vacuum thin film evaporation, flash concentration, heating and stirring
Evaporation and the like. Among these, vacuum thin film evaporation is
preferable. The vacuum thin film evaporator used for the vacuum thin film evaporation
The raw material slurry is thinned under reduced pressure and the transfer surface is transferred.
Especially if it has a structure that evaporates water while moving
No restrictions. The evaporation method using a general thin film evaporator is as follows.
It is on the street. That is, the raw slurry was stirred with a stirring blade (plate).
Cylindrical shape under reduced pressure with
Into the heat transfer surface and slide along the heat transfer surface due to the centrifugal force of the stirring blade.
Forcibly thin the lead. At this time, inside the wall jacket
Low-boiling components and moisture are removed by heat transfer from the heat medium and stirring heat.
Evaporate. Adjustment of the amount of evaporated water depends on the addition speed of the raw slurry.
Degree, rotation speed and tip peripheral speed of stirring blade, wall and blade tip
Clearance, vacuum inside the concentrator, jacket temperature
Is preferably operated. The peripheral speed at the tip of the stirring blade is 5 to 30 m.
/ S is preferable, and 5 to 25 m / s is more preferable. 5m
/ S, the thin film of the concentrated paste existing on the wall
And liquid exchange may not be performed smoothly.
/ S, frictional heat with the paste may be generated
The temperature of the concentrate may increase. At the same time, the concentrator
The mechanical load on the device may increase. As clearance between the wall surface and the tip of the blade
Is preferably 0.5 to 5 mm, more preferably 1 to 4 mm.
Preferably, it is 1 to 3 mm. Less than 0.5mm
Is mechanically stable at the actual machine size for mass production
Operation may be difficult.
Thinning of paste and liquid exchange may not be performed smoothly
is there. The degree of vacuum inside the concentrator is 4 to 80 kP
a is preferable, and 7 to 70 kPa is more preferable. 4kP
If the viscosity is less than a, the concentrated product viscosity is high,
Exhaust may be difficult, but exceeds 80 kPa
And the temperature of the concentrated product increases, and the evaporation efficiency decreases.
There is. The size of the concentrator is not particularly limited.
However, for example, the inner diameter of the cylindrical casing is 0.2 to 4.0.
m, the length of the heat transfer section is 0.5 to 10 m, and the area of the heat transfer section is
0.2-126m²Size is often used. concentrated
The residence time on the transmission surface in the aircraft is preferably 10 seconds to 5 minutes.
Preferably, 20 seconds to 4 minutes are more preferable, and 30 seconds to 3 minutes.
min is more preferred. Sakura is an example of a thin film evaporator
“Biolator” manufactured by Hitachi, Ltd. “Controller” manufactured by Hitachi, Ltd.
B), Shinko Pantech “Exeva” and the like. (2) Concentrated raw material paste Activator contained in the concentrated raw material paste, as a builder
Use any of the detergent slurry described above.
Can be As the water content of the concentrated raw material paste
Is preferably from 15 to 50% by mass, and more preferably from 20 to 45% by mass.
More preferably, the content is 22 to 42% by mass. In the concentration step, an anionic activator is added
When concentrating, handle with low moisture after concentration.
Can be a problem. To avoid this problem
Therefore, it is preferable to add additives that contribute to viscosity reduction as additives.
Good. Examples of substances that function as a viscosity reducing agent are given below.
However, the present invention is not limited to this. Polyoxyethylene alkyl ether:
C8-C40 saturated or unsaturated, EO, PO or B
O, preferably EO, PO, alone or as a mixture of 3
Compound added with up to 35 mol (preferably 5 to 30 mol)
Are preferred.・ Polyoxyalkylene alkyl phenyl
Ruether: an alkyl or alkenyl group having 8 carbon atoms
EO, PO or BO are preferred for
Preferably, EO or PO is used alone or in a mixture of 5-2.
5 moles (preferably 8 to 20 moles) of the compound added
preferable. Polyethylene glycol: weight average molecule
Compounds having an amount of 200 to 20,000 are preferred. ・ Polyethylene glycol fatty acid ester: fatty acid group
8 to 22 carbon atoms, degree of polymerization of ethylene glycol (ethylene
5 to 25 compounds are preferred.
No. ・ Decaglycerin fatty acid ester: The number of carbon atoms in the fatty acid group is
Preferred are compounds 8 to 22 and the like. -Sorbitan fatty acid ester: fatty acid residue having 8 carbon atoms
To 22 are preferred. ・ Water-soluble polycarboxylic acid and its salt: acrylic acid, meta
One kind selected from crylic acid, maleic acid and itaconic acid
Or a copolymer of two or more selected from
preferable. As counter ion, alkali metal, alkali
At least one selected from earth metals and ammonium is preferred.
New The weight average molecular weight is preferably 10,000 or less.
And 300 to 10,000 are more preferable. (3) Concentrate Viscosity of the concentrate (Brookfield type (B type) viscosity
From the viewpoint of handling properties.
000 Pa · s or less, preferably 1000 Pa · s or less
Is more preferable, and 500 Pa · s or less is further preferable.
If the viscosity exceeds 2000 Pa · s, transport becomes extremely difficult.
It can be difficult. The water content of the concentrate is 2
-26% by mass is preferred, and 5-25% by mass is more preferred.
No. The temperature of the concentrate depends on the degree of vacuum in the concentrator,
The temperature is almost the same as the boiling point at the air temperature. Friction from stirring blades
When the frictional heat is large, the temperature may be higher than the boiling point. The concentration
The temperature of the product is preferably 50 to 98 ° C, and 52 to 9 ° C.
6 ° C. is more preferred. --- Granulation step-- In the granulation step (densification of granular detergent), as described above,
Spray-dried particles and / or powder raw material obtained in
Kneading granulation method, kneading granulation method, crushing after extrusion (kneading), stirring granulation method,
And a known granulation method selected from tumbling granulation methods (however,
Except after crushing. ) To increase the density of granular detergent
You. The following describes each granulation method (until crushing).
Will be described. <Kneading granulation method> In the above-mentioned kneading granulation method,
Knead the detergent raw materials and spray-dried particles obtained as described above.
The mixture is kneaded and extruded to prepare a solid detergent. The detergent
Raw materials and spray-dried particles are introduced into a kneading (kneading) device.
Transport, consolidation, kneading (kneading) while applying shear force
To form a solid detergent. As the kneading (kneading) device, various types of
Can be used. Specifically, closed consolidation
Treatment apparatus, more preferably a horizontal continuous kneader.
Suitable. In addition to kneaders, uniaxial or biaxial screws
And a press extruder. These devices are
Any of a formula and a continuous formula may be used. Continuous kneading (mixed
When using kneading equipment, it is particularly involved in kneading (kneading).
Paddle placement is important in the quality of the resulting detergent.
You. It is disclosed in JP-A-2000-144194.
As in the case of a kneading machine with stirring blades,
Continuously to produce a kneaded product of detergent components.
(A) In the kneading (kneading) machine,
(B) Detergent component that transports detergent component to outlet direction
(C) a function to knead detergent components
The stirring blades having the respective functions are placed in a kneading (kneading) machine.
Continuous kneading (mixing) by sequentially arranging from the supply port to the discharge port side
Kneading) is preferred. In addition, when running for a long time,
Screws, paddles and fuselage (casing
G) treatment of stellite, tungsten carbide, etc.
It is preferred to apply. As a device for kneading (kneading)
Include the following devices, but are particularly limited
is not. (1) Continuous kneading (kneading) device Example 1: KRC kneader [manufactured by Kurimoto Iron Works Ltd.] Example 2: Extruded Omics [Hosokawa Micron
Co., Ltd.] Example 3: Fine louser [Fuji Paudal Co., Ltd.] Example 4: Continuous kneader [Dalton Co., Ltd.] Example 5: JP-A-63-242334, JP-A-6-2
No. 3251, No. 6-23252, No. 7-26
Apparatus described in Japanese Patent No. 5679 Example 6: Twin Dome Gran [Fuji Paudal Co., Ltd.] Example 7: Dome Gran [Fuji Paudal Co., Ltd.] (2) Batch kneading (kneading) device Example 1: Kneader [Dalton Co., Ltd.] Example 2: Universal mixing stirrer [Dalton Co., Ltd.] It is preferable that the kneading (kneading) operation conditions be used.
Examples are shown below. (1) Temperature Generally, 30 to 80 ° C is preferable, and 35 to 75 ° C is preferable.
And 40 to 70 ° C. is more preferable. The temperature is 30 ° C.
If it is less than this, the load on the kneading (kneading) device becomes excessive.
On the other hand, if the temperature exceeds 80 ° C., kneading (kneading) is reversed.
Is likely to adhere to equipment used in subsequent processes such as crushers.
There is. (2) Processing time In the case of the batch type, the processing time is usually 1 to 20 minutes.
Preferably, 2 to 15 minutes is more preferable, and 3 to 10 minutes is further preferable.
Preferred. In the case of the continuous type, the processing time is usually
10 to 120 seconds are preferred, 20 to 90 seconds are more preferred
And more preferably 30 to 60 seconds. (3) Pressure As disclosed in JP-A-61-118500.
The internal pressure of the kneader is 0.01 to 5 kg / cm²・ G
And kneading (kneading) continuously. (4) Binder Water is generally used as a binder during kneading (kneading).
Anionic surfactant, aqueous solution of anionic surfactant, noni
On-surfactant, nonionic surfactant aqueous solution, and it
Nonionic surfactants, nonionic surfactants,
Surfactant aqueous solution and anionic surfactant and nonionic
A mixed aqueous solution of a surfactant is preferred. (5) Cooling It suppresses the temperature rise of the solid detergent due to kneading (kneading).
While passing the refrigerant through the jacket of the kneading device.
It is preferable to perform kneading (kneading). Ethylene as a refrigerant
An aqueous solution of lenglycol is preferred and its concentration
Is preferably from 15 to 30% by mass, and more preferably from 20 to 25% by mass.
More preferred. Generally, the dimension is preferably 10 to 500 mm.
Preferably, a screw of an extruder that introduces a kneaded material
If the pitch is smaller than the pitch of the
No. In the extrusion, the obtained kneading (mixing
The kneaded material is formed into pellets by an extruder. As the extruder
Is generally a single or twin screw extruder or disc
Can be used extruder or roll extruder
However, in the case of detergent, the screw type is preferable, and the biaxial type is more preferable.
preferable. A typical extruder is illustrated below. (1) Single screw type Example 1: Dome Gran [Fuji Paudal Co., Ltd.] Example 2: Single screw continuous granulator [Fukae Kogyo Co., Ltd.] (2) Twin screw type Example 1: Pelleter double [Fuji Paudal Co., Ltd.] Example 2: Twin Dome Gran [Fuji Paudal Co., Ltd.] Example 3: TEX65αII twin screw extruder [Nippon Steel Works Co., Ltd.
Made Example 4: Screw W-type continuous granulator [Fukae Kogyo Co., Ltd.] (3) Disk type Example 1: Disk pelleter [Fuji Paudal Co., Ltd.] (4) Roll type Example 1: Cylindrical granulator [Fukae Kogyo Co., Ltd.] Example 2: Open roll continuous extruder [Mitsui Mining Co., Ltd.] The extruder is used for the physical properties and crushing of the detergent to be treated.
For ease of processing, it is preferable to set as follows
No. (1) Die thickness Generally, it is set by the extrusion pressure. Usually press the detergent
When put out, preferably 10-30 mm, 15-20 mm
Is more preferred. (2) Die opening ratio Generally, it is set according to the processing capacity and the extrusion pressure. Normal,
When extruding a detergent, 10-60% is preferable, and 15-
50% is more preferable, and 20 to 40% is still more preferable. (3) Die hole diameter Generally determined by the desired pellet size,
When considering the load in the crushing and granulating process, 1 to 20 mmφ is
Preferably, 3 to 15 mmφ is more preferable, and 5 to 12 m
mφ is more preferred. Die hole diameter becomes too small
And the extruder attached to the extruder
While this may cause troubles such as chair deformation,
If the chair hole diameter is too large, the load on the crusher may increase.
There is. (4) Die shape The hole shape is preferably circular considering wear and pressure (load).
Good. Also improved the introduction of the extrudate into the die
To reduce the pressure rise,
It is preferable to design it larger than the outlet hole diameter. Preferred Embodiment as Operating Conditions for the Extrusion
Examples are shown below. (1) Temperature Generally, 20 to 80 ° C is preferable, and 30 to 70 ° C is more preferable.
More preferably, the temperature is 40 to 60C. The temperature is 20
If the temperature is lower than ℃, the load on the extruder may be excessive.
On the other hand, when the temperature exceeds 80 ° C., the extrudate tends to adhere.
Sometimes. (2) Processing time Generally, 1 to 20 seconds is preferred, and 3 to 15 seconds is more preferred.
New If the processing time is less than 1 second, pellet molding
While the property is poor and the uniformity of the components may be reduced,
If the time exceeds 20 seconds, productivity may decrease. (3) Cutting The cutting of pellets is generally performed using a cutter or hard wire cutter.
Pellet discharged from the extruder die by rotating the tool
Disconnect. This peripheral speed is preferably 1 to 5 m / s. Peripheral speed
Slower, the resulting pellets may be too large.
On the other hand, if it is too fast, coalescence of pellets may occur.
is there. The clearance between the die and cutter is as much as possible
Zero is preferred. If the clearance is large, the pellets
When cutting, the pellets are
Coalescence of the moving pellets may occur. However,
In this case, it is preferable to set the thickness to about 10 mm or less. (4) Adhesion measures The object to be extruded obtained by the extrusion is screwed into an extruder.
If it adheres to the
It is preferable to cool or heat by heating. Also wash
In the case of chemicals, it is advisable to introduce steam to the screw surface.
The effect of restraining wearing is great. Of pellets obtained by extrusion
In general, the diameter is preferably 1 to 20 mmφ and 3 to
15 mmφ is more preferable, and 5 to 12 mmφ is still more preferable.
New If the diameter of the pellet becomes too small,
Deformation of the die attached to the extruder due to the rise in the pressure
May cause troubles such as
If the diameter is too large, the load on the crusher may increase.
is there. The length of the pellet is determined by the knife for pellet cutting.
Considering the adhesion to the crusher and the load on the crusher, 5-30mm
Is preferable, and 5 to 15 mm is more preferable. <Stirring granulation method> In the stirring granulation method,
Uses a stirring granulator (internal
(Stirring mixer), shearing action, compaction action and rolling action
Obtain a solid detergent by using [0097] The stirring granulation apparatus is provided with a stirring blade provided with stirring blades.
A stirring shaft is provided at the center of the inside, and when the stirring blade rotates,
A structure that forms a clearance between the stirring blade and the vessel wall.
It's important to. The average clearance is 1 to
30 mm is preferable and 3 to 10 mm is more preferable. The
If the average clearance is less than 1 mm,
While the mixing machine is likely to be overpowered,
If the particle size exceeds the limit, the compaction efficiency will decrease and the particle size distribution will be reduced.
Loads and granulation time increase, reducing productivity
Sometimes. As a stirring type mixer having such a structure,
Is, for example, Henschel mixer [Mitsui Miike Kakoki Co., Ltd.
High-speed mixer [Fukae Kogyo Co., Ltd.]
Optical granulator (made by Powrex Corporation)
Device. Especially in the center of the cylinder in a horizontal mixing tank
It has a stirring shaft, and a stirring blade is attached to this shaft to mix powder.
Is preferred, such as Lady Gemiki
Sir [Matsubo Co., Ltd.], Blowshare Mixer [Taihei
Manufactured by Yoki Co., Ltd.]. Preferred as granulation conditions for the stirring granulation method.
An embodiment is illustrated below. (1) Fluid number (Fr number) It is preferable that the Froude number defined by the following equation is 1 to 4.
More preferably, it is 1.2 to 3. The fruit
If the number is less than 1, consolidation may not be promoted.
On the other hand, if it exceeds 4, the particle size distribution may be wide.
You. formula : Froude number (Fr number) = V / (R × g)^0.5 V: Peripheral speed at the tip of the stirring blade [m / s] R: radius of rotation of the stirring blade [m] g: Gravitational acceleration [m / s²] (2) Granulation time Granulation in palindrome granulation to obtain a suitable solid detergent
Time, as the average residence time in continuous granulation,
Preferably 0.5 to 20 minutes, more preferably 3 to 10 minutes
No. If the time is less than 0.5 minutes, the granulation time is short.
Granulation control to obtain suitable average particle size and bulk density
Is difficult and the particle size distribution may be broad.
On the other hand, if it exceeds 20 minutes, the granulation time is too long and the productivity is low.
May drop. (3) Filling rate of detergent raw material As the filling rate (preparation amount) of the detergent raw material into the granulator,
It is preferably 70% by volume or less of the total internal volume of the mixing machine.
40% by volume is more preferred. If it exceeds 70% by volume,
Since the mixing efficiency of the detergent raw materials in the
In some cases, grain cannot be formed. (4) Temperature The granulator preferably has a structure with a jacket.
The temperature of the medium passing through the tray is preferably 5 to 40 ° C,
10-20 degreeC is more preferable. Keep in this temperature range
Therefore, the granulation time for obtaining a suitable granulated product is shortened.
The productivity is improved and the particle size distribution becomes sharp. Also detergent
Of the raw materials, the powder raw material is at room temperature, and the nonionic activator
The temperature inside the mixer should be particularly controlled.
No need to control. The temperature of the granulated material is the temperature of the feedstock.
The temperature is usually 30 to 60 ° C. depending on the degree and heat of stirring. (5) Additive In the above-mentioned granulation, in order to promote granulation, a
May be added. As a specific example of a binder
Is carboxymethylcellulose, polyethylene glyco
And polycarboxylates such as sodium polyacrylate
Water-soluble polymer solution of polyoxyethylene alkyl ester
-Tel, fatty acid monoethanolamide, fatty acid diethanol
Nonionic substances such as ureamide; fatty acids; sodium silicate water
A solution; water; and the like. Distribution of the binder
The total amount is 0.1 to 100 parts by mass of the detergent raw material.
10 parts by mass is preferred, and 0.5 to 5 parts by mass is particularly preferred.
No. <Rolling granulation method> In the rolling granulation method,
Uses a tumbling granulator (container)
(Rotary mixer), shearing action, compaction action and rolling
It granulates using the action to obtain a solid detergent. [0105] The above-mentioned tumbling granulation apparatus includes the following container jars.
An inversion mixer can be suitably used. <Batch type device> (1) V-shaped mixing tank rotates for mixing.
A form of mixer to do. Example 1: V-type mixer [manufactured by Fuji Paudal Co., Ltd.] Example 2: V-type mixer [manufactured by Seishin Enterprise Co., Ltd.] (2) Rotation of the cylindrical mixing tank
A mixer that mixes by Example 1: Rocking mixer (Aichi Electric Trading Co., Ltd.) Example 2: Doria coater [manufactured by Powrex Corporation] Example 3: Rotary mixer [Maywa Kogyo Co., Ltd.] Example 4: Drum mixer [Sugiyama Heavy Industries Ltd.] (3) The double-cone type mixing tank rotates.
A mixer that mixes by mixing. Example 1: W type mixer [manufactured by Seishin Enterprise Co., Ltd.] Example 2: Double cone mixer (ASR) (4) The cylindrical mixing tank rotates and revolves.
Mixer that performs mixing. Example 1: Dyna mixer [Mori Machinery Co., Ltd.] Example 2: Cross rotary mixer [Maywa Kogyo Co., Ltd.] <Continuous system> (1) Mixing is performed by rotating the cylindrical mixing tank.
A form of mixer to do. Example 1: Rocking mixer (Aichi Electric Trading Co., Ltd.) Example 2: Doria coater [manufactured by Powrex Corporation] [0110] Preferable operating conditions for the above-mentioned rolling granulation are as follows.
An embodiment is illustrated below. (1) Processing time Processing time for high bulk density in batch type or continuous type
The average residence time defined by the following equation is 5
-120 minutes is preferable, 10-90 minutes is more preferable,
10 to 40 minutes are more preferred. The time is less than 5 minutes
In some cases, the bulk density cannot be sufficiently increased.
If it exceeds 20 minutes, the productivity may decrease or the detergent granules
Collapse may occur. Formula: Tm = (m / Q) × 60 Tm: average residence time (hr) m: Detergent granule retention amount in the container rotary mixer (kg) Q: Capacity in continuous operation (kg / hr) (2) Froude number (Fr) The Froude number defined by the following equation is 0.01 to 0.8.
It is preferable to select conditions such that
It is more preferable to select a condition that satisfies 0.7.
It is more preferable to select a condition that satisfies ０．６0.65. Previous
When the Froude number is less than 0.01, uniform and high
While detergent particles of bulk density may not be obtained, 0.8
Above, for example, in the case of a drum-type mixer, detergent granules
Particles may be scattered, resulting in improper shear mixing. [0112] Formula: Froude number (Fr) = V²/ (R × g) V: Peripheral speed (m / s) at the outermost periphery of the container rotary mixer R: radius from the center of rotation of the outermost periphery of the container rotary mixer
(M) g: Gravitational acceleration (m / s²) (3) Volume filling rate (x) The volume filling rate (x) defined by the following equation is 15 to 50
%, Preferably 20 to 45%.
It is more preferable to select the following condition: 25 to 40%
More preferably, the following conditions are selected. The volume filling rate
If (x) is less than 15%, productivity may be poor.
On the other hand, if it exceeds 50%, good shear mixing is not obtained.
Sometimes. [0114] Formula: Volume filling rate (x) = (M / ρ) / V × 100 M: Amount of detergent granule particles charged to the container rotary mixer
(G) ρ: bulk density (g / L) of detergent granule particles V: Volume (L) of the container rotary mixer In the granulation, a batch type or a continuous type may be used.
May be. To produce detergent particles continuously, plug plugs
Mixers with mixing characteristics close to low (extrusion flow) are preferred
New In this case, one side (the side flat plate of the container rotary mixer)
Part), feed the raw material continuously, transfer it to the flow type and
(The flat plate on the side opposite to the container rotating mixer)
From the input side to the discharge side.
It may be inclined in a downward direction to facilitate discharge. Inclination
The bevel angle is preferably 0 to 20 °, more preferably 0 to 5 °.
No. If the tilt angle exceeds 20 °, ungranulated particles are mixed.
Sometimes. In the case of a continuous type, a container rotating type mixer
Further enhances mixing characteristics closer to plug flow
In order to do this, use several partition plates perpendicular to the rotation center line of the container rotation.
Are attached at several points in the direction of the rotation center line, and the particle layer slope is
It is preferable to prevent rolling in the discharge direction when
No. In addition, the center parallel to the rotation center line of the container rotary mixer
Granulation time is shortened by having stirring blades on the shaft
be able to. Detergent granulation particles flow down the particle layer slope
By adding agitation to the part where
Shearing force and impact force are applied, and granulation is performed in a short time.
Time is reduced. The rotating direction of the stirring blades is
It can be in the same direction as the rotation direction of the machine or in the opposite direction,
Preferably the direction opposite to the downward movement of the granulated particles (the container rotation direction)
Stirring in the same direction), detergent granulated particles
And the relative speed of the stirring blades increases,
Great effect. The rotating radius of the stirring blade is determined by the rotating type mixer of the container.
0.8 times or less, preferably 0.7 times or less of the turning radius of
I do. The distance between the inner wall of the rotary mixer and the stirring blade is small.
When this happens, a strong shearing force is applied to the detergent granule particles,
As a result, the detergent granules are disintegrated and granulation is hindered.
In order to prevent such situations, the rotation radius of the stirring blade should be
It is preferably 0.8 times or less the rotation radius of the rotary mixer. Stir
The tip speed of the stirring blade is 1 to 6 m / s. Preferably
Is 2.5 to 5 m / s. In addition, detergent granule particles
The speed is 1m / s or more from the viewpoint of giving sufficient stirring power.
Preferably, the granulation is prevented by the collapse of the detergent granule particles
6 m / s or less is preferable from the viewpoint of preventing the occurrence. In the continuous type, the shape of the stirring blades is
Significantly hinders mixing characteristics close to plug flow of rotary mixer
It is preferable not to have them. For example, container rotation type mixing
Examples of rod-shaped or plate-shaped blades parallel to the rotation center line of the machine
It is. Products with mixing characteristics close to plug flow are impeded
Detergent granulated product with increased residence time distribution width
Particles and non-granulated particles are mixed, and as a result
It may become particles containing a large amount of granules. Also continuous
In the direction of detergent granulation flow of the container rotary mixer.
Granulation can be controlled by adjusting the number of stirring blades
It becomes. At the time of granulation, fine powder is added.
Re-granulation and aggregation can be prevented. This phenomenon
In order to prevent this, the average primary particle size is 10 μm or less.
The fine powder is usually added in an amount of 0.1 part by mass per 100 parts by mass of the detergent granule particles.
1 to 10.0 parts by mass (preferably 0.2 to 5.0 parts by mass)
Parts) can be added. For the addition of such fine powder
Thus, the powder on the surface of the detergent granules is reduced
Detergent particles with physical properties are formed. The amount of the fine powder is
Exceeds 10.0 parts by mass with respect to 100 parts by mass of granular particles
And the excess of fine powder causes poor flow of detergent granules
And the resulting decrease in granulation efficiency may occur. The average particle size of the primary particles of the fine powder is
A method that uses turbulence, such as a particle analyzer
(Manufactured by Horiba, Ltd.) and by microscopic observation
It is measured by measurement or the like. As such fine powder, usually
Known ones used may be used. At the time of the above-mentioned granulation, the detergent granulated particles and the container rotation
Detergent granulation with small wall friction coefficient with the inner wall of the mold mixer
When it is difficult to apply sufficient ascent motive force to object particles
Is to install multiple baffles on the inner wall of the container.
It is preferable to forcibly perform the upward movement. Bag
The full height controls the movement of particles as they flow down the slope of the particle layer.
From the viewpoint of not hindering, the rotation radius of the container rotary type mixer is set at 0.
It is preferably 25 times or less. [Crushing Process] In the crushing process,
Solid detergent (mixture, mixed
(Kneaded material, pellet, or granulated material)
Crushing treatment to adjust to the desired particle size to produce granular detergent composition
I do. That is, the hardness and strain (displacement) of the solid detergent
Accordingly, crushing treatment is performed under any of the following conditions (a) to (c)
To produce a granular detergent composition. (A): Hardness of the solid detergent is 50 ≦ hardness
[G] <1000, strain (displacement) is 1.0 ≦ strain
(Displacement) When [mm] <2.5 is satisfied and solid washing
When the hardness of the agent is 1000 ≦ hardness [g] ≦ 3000, strain
(Displacement) is 1.0 ≦ strain (displacement) [mm] <4.8
When it is satisfied, supply hot air of 26 ° C or more to the crusher,
Reduce the peripheral speed of one or more crushing granulator rotating bodies to 50 m / s or less
Set and crush processing. (B): The hardness of the solid detergent is 50 ≦ hardness [g] <1000
And the strain (displacement) is 5.0 ≦ strain (displacement) [mm] ≦
8.0 and the hardness of the solid detergent is 1000
≤ hardness [g] ≤ 3000 and strain (displacement) 4.8 ≤
If the displacement (displacement) [mm] ≦ 8.0 is satisfied, 25
Crushed air is supplied to the crusher at a temperature of less than ℃. (C): The hardness of the solid detergent is 50 ≦ hardness [g] <1000
And the strain (displacement) is 2.5 ≦ strain (displacement) [mm] <
When 5.0 is satisfied, one or more crushing granulator rotating bodies
Crushing process with peripheral speed set to 50m / s or less. In the crushing treatment, the solid detergent
Crusher of a cutter mill type with a classification screen
Crusher with large screen hole diameter
It is particularly preferred that the mixture is sequentially supplied to a crusher and crushed in multiple stages. The crushing granulator used in the crushing process
Examples are given below. (1) Crushing granulator Generally, crushing granulation with a rotating body and a screen inside
Machine is preferred, hammer mill, atomizer, parpera
Impact type crusher such as Iser, cutter mill, feather mill
And the like are more preferable. [0125] Example 1: Fitzmill [manufactured by Hosokawa Micron Corporation] Example 2: Speed mill [Made by Okada Seiko Co., Ltd.] Example 3: Crushing type granulator power mill [Fuji Paudal Co., Ltd.]
Made Example 4: Atomizer [Fuji Paudal Co., Ltd.] Example 5: Pulverizer [manufactured by Hosokawa Micron Corporation] Example 6: Commutator [Fuji Paudal Co., Ltd.] The type of crusher is not particularly limited.
Has a rotary crushing blade in the crushing chamber,
Crushed and crushed detergent granules into a screen with a predetermined hole diameter.
And the like discharged from the apparatus are preferably used. (2) Screen Screen is wire mesh type, herringbone type, punch
There is no particular limitation on the metal type, but the screen strength
Considering the shape of the crushed material, punched metal etc.
preferable. (3) Rotating body A hammer or a cutter is used.
A cutter type is preferable to avoid generation of powder. However
And prevent wear of the cutter blade during long hours of operation
Therefore, treatment with stellite, tungsten carbide, etc.
Is preferred. The conditions for the crushing process are described below.
You. (1) Circumferential velocity of rotating body of granulator Generally, the peripheral speed of the rotating body of the crushing and granulating machine is the
) And the desired particle size. The present invention
In the case where the solid detergent is brittle, that is, as described above
When the hardness of the solid detergent is 50 ≦ hardness [g] <1000,
Strain (displacement) is 1.0 ≦ strain (displacement) [mm] <2.
When 5 is satisfied, the hardness of the solid detergent is 1000 ≦ hardness
[G] ≦ 3000, strain (displacement) 1.0 ≦ strain
(Displacement) [mm] <4.8 and solid washing
When the hardness of the agent is 50 ≦ hardness [g] <1000,
Satisfies 2.5 ≦ strain (displacement) [mm] <5.0
In this case, the peripheral speed of one or more crushing granulation rotating bodies
It is necessary to set it to 0m / s or less, and to 40m / s or less
It is preferable to set it, and set it to 10-40 m / s
Is more preferred. By setting like this, crushing
Adhesion to the machine is prevented. On the other hand, when the hardness of the solid detergent is 50 ≦ hardness [g]
<1000, strain (displacement) is 5.0 ≦ strain (displacement)
When [mm] ≦ 8.0 is satisfied, the hardness of the solid detergent is 10
00 ≦ hardness [g] ≦ 3000 and strain (displacement) 4.8
≦ strain (displacement) [mm] ≦ 8.0
In the case of crushing at 50m / s or more,
At this point, at which point 50 to 70 m / s
Crushing is more preferred. (2) Cold air supply In the crushing treatment, the hardness of the solid detergent is 50 ≦ hardness.
[G] <1000 and strain (displacement) is 2.5 ≦ strain
(Displacement) [mm] ≦ 8.0 and hardness of solid detergent is 100
0 ≦ hardness ≦ 3000 and strain (displacement) 4.8 ≦ strain
(Displacement) If satisfies ≤ 8, crushed material by crushing heat
To prevent softening and sticking to the crusher.
It is necessary to supply cold air of 25 ° C. or less into the crusher. The cold
The temperature of the wind is preferably 5 to 25 ° C, and 10 to 25 ° C.
C is more preferred. The humidity of the cold air is not particularly limited,
The lower the better, the better. The amount of the cold air is 0.1 to 5 m³
/ Kg (crushed material) is preferred. Too much cold air will break
Because the temperature of the crushed material drops significantly and the crushed material becomes hard and brittle,
It may cause over-crushing and increase fines and shape deterioration.
You. As for the method of introducing the cold air, the necessary amount for the first stage
Either batch introduction or divisional introduction into each stage may be used. Also break
The cool air discharged from the crusher is separated from the powder and recirculated.
Wrapping is preferable in terms of economy. Resai at this time
Volatile recovery rate in wrap air is about 0.1 to 1.5%
And the amount of fresh air input is recycled
It is about 0 to 15% with respect to air. (3) Hot air supply In the crushing treatment, when the solid detergent is brittle,
In addition, as described above, the hardness of the solid detergent is 50 ≦ hardness [g].
<1000, strain (displacement) is 1.0 ≦ strain (displacement)
When [mm] <2.5 is satisfied, the hardness of the solid detergent is 10
When 00 ≦ hardness [g] ≦ 3000 and strain (displacement) is 1.
When 0 ≦ strain (displacement) [mm] <4.8
In order to prevent adhesion to the crusher,
It is necessary to supply warm air of 26 ° C. or higher. The temperature of the hot air
Is preferably 26 to 45 ° C, more preferably 30 to 35 ° C.
Is more preferable. There is no particular limitation on the humidity of the warm air.
However, the lower, the better. The amount of hot air is 0.1
~ 5m³/ Kg (crushed material) is preferred. How to introduce hot air
, The required amount is batch-introduced to the first stage, and divided into each stage
Any of introduction may be used. In addition, the temperature discharged from the crusher
It is economical to recycle wind after separating it from powder
It is preferred in terms of. Volatile content in recycled air at this time
The recovery rate is about 1.0 to 3.5%,
-The input amount is 0 to 15 with respect to the recycled air.
%. FIG. 1 shows the hardness and strain of the solid detergent.
It is a figure showing the relationship of (displacement). In FIG. 1, the area
(A) is the condition of the above (a), that is, the hardness of the solid detergent is
50 ≦ hardness [g] <1000 and strain (displacement) is 1.0
≤ strain (displacement) [mm] <2.5
And the hardness of the solid detergent is 1000 ≦ hardness [g] ≦ 3000
And the strain (displacement) is 1.0 ≦ strain (displacement) [mm]
<4.8 is satisfied, and the region (b) is a solid detergent
Strain (displacement) when the hardness is 50 ≦ hardness [g] <1000
Is 5.0 ≦ strain (displacement) [mm] ≦ 8.0
When the hardness of the solid detergent is 1000 ≦ hardness [g] ≦ 3
And the strain (displacement) is 4.8 ≦ strain (displacement) [m
m] ≦ 8.0, and the region (c) is solid
Detergent (hardness [g] <1000)
Satisfies 2.5 ≦ strain (displacement) [mm] <5.0
This is the case. (4) Crushing aid In the crushing treatment, it is preferable to add a crushing aid.
New The crushing aid is generally a grinding aid (grinding aid).
aid), added in small amounts in the crusher
By reducing crushing power, improving crushing particle size, crushing
It has the effect of improving the properties of the product. The particle size of the crushing aid is 50 μm or less.
Lower is preferable, and 20 μm or less is more preferable. Also,
The addition amount is preferably 0.5 to 10% by mass based on the crushing amount.
New Examples of the type of the crushing aid include stearates, A
Aluminosilicates such as zeolite, calcium carbonate, charcoal
Magnesium oxide, alkaline earth metal carbonate, amorphous silicon
Mosquito, silicic acid such as calcium silicate and magnesium silicate
Clay minerals such as salt, talc, bentonite, silicon dioxide,
Titanium dioxide, finely ground sodium carbonate, sodium sulfate
Lium and the like are preferred. These crushing aids are used on the surface of the crushed material.
By adhering to the surface and reducing the surface activity of the crushed material,
Prevention of adhesion to crusher and reduction of crushing power,
The fluidity of the crushed material is improved. The method for adding the crushing aid is as follows.
The method of mixing before crushing and the required amount
The method of adding the amount all at once, the method of adding separately for each stage,
Is mentioned. Either method may be used, but the auxiliary effect
From the viewpoint of economy and economy, batch addition is preferred. In addition, crusher
By connecting directly to each other and creating a closed system between each stage
(Sealing direct connection type), loss of crushing aid is small,
It is preferable to use the
New (5) Processing time The time of the crushing treatment is not particularly limited,
Usually, 1 to 30 seconds is preferable, and 3 to 30 seconds is more preferable.
No. (6) Screen hole diameter Generally, it depends on the friability of the material to be crushed (crushing material) and the desired particle size.
Is set. Usually, the desired average particle size is 3.0 to 30.0.
Times is preferable, and 4.0 to 25.0 times is more preferable. An example
For example, when obtaining detergent particles having an average particle size of 500 μm,
A screen with a pore size of 5 to 15 mm is
And use it. Also, two or more types in one stage
More effective crushing by setting the hole diameter
You can also. (7) Multi-stage crushing The crushing capacity of multi-stage crushing of high bulk density detergent
Because they are connected in series, they have a large capacity and are common to all stages.
Preferably. In order to achieve this,
The crusher inlet and outlet obtained by selecting the clean hole diameter
It has been found that there is an optimal value for the ratio of the average particle sizes. Shatter
Average particle size at the start of treatment and average particle size of desired crushed granulated material
Is set, the number of crushing stages is naturally determined in accordance with this.
Is determined. At that time, the screen hole diameter and the crushed material obtained
If it is possible to predict in advance the relationship with the average particle size of
is there. Also, with large particle size, powder surface area is small and crushed
Since the load on the machine is small, the average particle size at the inlet-outlet
Ratio can be widened. Therefore, when performing multi-stage crushing,
It is desirable to reduce the crushing particle size as much as possible
New At the time of multi-stage crushing, use the outlet of the crusher for each stage.
Provide a sieve and supply only the desired amount of crushed material to the next crusher
However, clogging of the sieve, complication of the system, and installation
It is disadvantageous in terms of increased area. Therefore, the first stage crusher
Waste (crushed material) from the second stage (and
The direct connection type for supplying to the crusher of the third stage or later) is preferable. The average particle size of the crushed granules after the crushing treatment was
Therefore, the thickness is preferably 300 to 1500 μm,
000 μm is more preferred. If the particle size is large,
Solubility slows down, causing problems with cloth adhesion and detergency
On the other hand, if the size is small, the amount of dust increases due to the increase in fine powder.
Large size may result in lower crushing yield and lower fluidity.
You. [Others] After granulation, fluidity and non-caking
Fine powder is added as a surface coating agent to improve
Preferably, the surface of the granulated material is coated. Surface coating agent
If added at the beginning or middle of granulation,
To improve the fluidity and non-caking properties of the granulated material
Is added after granulation because it does not contribute to the production. Here,
“After granulation” means that the average particle size of the granulated product is the desired average particle size.
It refers to the point after granulation to a diameter. The fluidity and non-caking properties of the granules were
Fine powder for surface coating of granulated material to improve
The compounding amount of 0.1 to 100 parts by mass of the granulated product
30 parts by mass is preferable, and 0.2 to 20 parts by mass is more preferable.
New When the amount is less than 0.1 part by mass, it is good.
It may be difficult to obtain a powder with good fluidity
On the other hand, if it exceeds 30 parts by mass, the fluidity is reduced and dust is
Occasionally, this may impair the consumer's feeling of use. The fine powder has an average primary particle size of 10
It is preferably at most μm. As this surface coating
Is a point that acts as a calcium ion scavenger during washing.
Aluminosilicate is preferred, especially the average of the primary particles
Aluminosilicates having a particle size of 10 μm or less are preferred. A
Other than luminosilicate, the average primary particle size is 10 μm.
m or less of silicon dioxide, bentonite, talc, clay,
Inorganic fine powder such as silicate compounds such as amorphous silica derivatives
The body is also preferred. Also, the average primary particle size is 10 μm or less.
The metal soap below can be used as well. Of primary particles
The average particle size of fine powder having an average particle size of 10 μm or less is determined by light scattering.
Using a method such as a particle analyzer (Hori
(Manufactured by Jiba Seisakusho) and by microscopic observation
And so on. A coating apparatus used for the surface coating;
Although not particularly limited, the following devices and the like are preferably
No. Also, the general coating conditions are as follows
Show. -Coating device- Rolling drum (horizontal cylindrical mixer), double cone type mixer, V
Mold mixer, Lödige mixer, ribbon mixer -Coating conditions- Fr number: generally 0.01 to 0.8, preferably 0.0
5 to 0.6, but 1.0 to 3.0 for Reedige ribbon Mixing time: generally 0.5 to 5 minutes [Physical Properties of Granular Detergent Composition] The book described above
Granular obtained by the method for producing a granular detergent composition of the invention
The following embodiments are preferable as physical properties of the detergent composition. (1) Bulk density The bulk density is preferably 0.6 to 1.2 g / ml.
And 0.7 to 1.0 g / ml is more preferable. Said dense
If the degree exceeds 1.2 g / ml, the solubility may deteriorate.
There is. (2) Average particle size (mass average particle size on sieve) The average particle size is preferably 300 to 1500 μm.
And 400 to 1000 μm is more preferable. The average grain
If the diameter is less than 300 μm, dust may be generated.
On the other hand, if it exceeds 1500 μm, the solubility deteriorates.
Sometimes. (3) Liquidity The fluidity is preferably 60 ° or less in repose angle.
When the angle of repose exceeds 60 °, the handleability of detergent deteriorates.
Sometimes. [0148] The present invention will be further described below with reference to Examples and Comparative Examples.
The present invention is not limited to the following examples.
It is not done. (Examples 1-122 and Comparative Examples 1-63)
Detergent compositions of each composition and properties are obtained by the following production methods 1 to 6.
Was. Composition, manufacturing method, and composition in each of Examples and Comparative Examples
And the evaluation of the adhesion in the crusher is shown in Tables 10 to 15.
You. <Production Method 1> Tables 1 to 9 (in the table, each composition is
Expressed in numerical values in parts by mass. Dried powder shown in)
Is dissolved and dispersed in tap water (Edogawa-ku, Tokyo)
Number: 60 rpm, jacket temperature: 70 ° C), solid content concentration
A slurry having a degree of about 60% by mass was prepared. This is countercurrent dry
Using a drying tower, spray-dry under the conditions described below, and
Of dried particles were obtained. Add granulation process with these dried particles
Ingredient and tap water (Edogawa-ku, Tokyo), continuous kneader
(Kurimoto Iron Works Co., Ltd., KRC-S4 type)
Add (rotation speed 135 rpm, jacket temperature about 50
℃) Amorphous solid detergent is formed and this is pelletized
(EXP-100 manufactured by Fuji Paudal Co., Ltd.)
And extrude from a die of about 10mmφ and cut at the same time
And pelletized solid detergent (about 10 mm in diameter, 70 m in length)
m or less) (Cutter circumference of pelletizer (cutter))
Speed is 5m / s). Next, the obtained pelleted solid detergent was
Add the crushing aid shown in Tables 1 to 9 (auxiliary species
・ Amount is described in the table), warm air (temperature about 30 ° C, wind (air))
And the ratio of kneaded material (solid) is qi / solid = about 3.0m³/ Kg,
(Wind speed about 20 m / s)
Zmill (Hosokawa Micron Corporation, DKSO-6
(Rotational speed of the crushing blade, screw speed)
The diameters are shown in Tables 10 to 15). Temperature of the obtained crushed product
Was about 30 ° C., and the average particle size was about 500 μm. [Slurry preparation conditions] ・ Ingredients not to be blended: enzymes, fragrances, pigments, bleach, bleaching activity
Activating agent, nonionic surfactant, layered silicate, silica ・ Blending order: For each composition, blended according to the prescribed blending order
did. Specific examples are shown in FIGS. ・ Temperature: about 70 ° C -PH: 10 to 11.5 [Spray drying conditions] Spray dryer: countercurrent type, tower diameter 2.0 m, effective length 5.
0m ・ Atomization method: Pressure nozzle method ・ Spray pressure: about 30kg / cm² ・ Hot air inlet temperature: 260 ° C ・ Hot air outlet temperature: 90 ° C ・ Discharge method: zeolite at the bottom of the tower with cold air
Emission after introduction and improvement of liquidity [Physical Properties of Spray-Dried Particles] ・ Average particle size: about 400 μm -Passing through a sieve with openings of 150 μm: about 10% by mass ・ On a sieve with openings of 1000 μm: about 3% by mass -Bulk density: about 300g / L -Angle of repose: 40 degrees ・ Moisture: about 5.5% by mass Cool air: The introduced air is
Cycle air only, fresh air only, recycle
Mixed air of fresh air and fresh air
No matter which air is introduced, it will affect the crusher adhesion.
Absent. If recycled air is used,
The volatile content recovery rate is about 0.1 to 1.5%,
As for the amount of air supplied,
It is about 0 to 15%. (Common to Manufacturing Examples 1 to 6) ・ Hot air: The introduced air is recycled air
Only, fresh air only, recycled air and air
Any air mixed with fresh air may be used.
The introduction of air does not affect the adhesion of the crusher. Resai
When using air, recover volatiles in the air
Rate is about 1.0 to 3.5%,
About 0-15% of recycled air
Degrees. (Common to Manufacturing Examples 1 to 6) <Production Method 2> α-SF slurry (water content of about 2
6 mass%, viscosity 7 Pa · s) with a capacity of about 115 kg / h
r, a vacuum thin film evaporator with an evaporation efficiency of about 17 kg / hr (d
Xeva (Shinko Pantech), transmission surface (contact with slurry)
Area) 0.5m², Clearance 3mm,)
Inner wall heating temperature about 115 ° C, degree of vacuum about 0.45 MPa, times
Concentration was performed under the conditions of a rotating blade peripheral speed of 11 m / s. Got
The physical properties of the concentrate include a water content of about 20% and a viscosity of 20 Pa
(Measured with a look field type (B type) viscometer)
Was. Then, the obtained concentrate and other granulation steps
Continuous kneading of additive and tap water (Edogawa-ku, Tokyo)
-(Model KRC-S4, manufactured by Kurimoto Iron Works, Ltd.)
Knead (rotation speed 135 rpm, jacket temperature about 80
℃) Amorphous solid detergent is formed and this is pelletized
(EXP-100 manufactured by Fuji Paudal Co., Ltd.)
And extrude from a die of about 10mmφ and cut at the same time
And pelletized solid detergent (about 10 mm in diameter, 70 m in length)
m or less) Cutter peripheral speed of the obtained (pelleter (cutter))
Is 5 m / s). Next, the resulting pelleted solid detergent
Add the crushing aid listed in Tables 1 to 9
The amount is described in the table), warm air (temperature: about 35 ° C, wind (air))
And the ratio of kneaded matter (solid) is qi / solid = about 4.0m³/ Kg,
(Wind speed 18m / s)
Tsumir (manufactured by Hosokawa Micron Corporation, DKSO-6 type)
(The peripheral speed of the rotary crushing blade and the screen diameter are
See Tables 10-15. ). The temperature of the obtained crushed product is about 4
At 0 ° C., the average particle size was about 500 μm. <Production Example 3> Dry powder components shown in Tables 1 to 9
Is dissolved and dispersed in tap water (Edogawa-ku, Tokyo) (rotation speed
60 rpm, jacket temperature 70 ° C), solid content concentration about 6
A slurry of 0% by mass was prepared. This is a countercurrent drying tower
Spray-dry (conditions refer to Production Method 1)
Particles were obtained (the physical properties of the particles were the same as in Production Method 1). This dry particles
With the granulation process additive and tap water (Edogawa, Tokyo
Ward) continuous kneader (Kurimoto Corporation, KRC-S)
4 type), knead (135 rpm, jaw)
(Ket temperature 40-60 ° C) Form an amorphous solid detergent,
The pelletizer double (Fuji Powdal Co., Ltd., EXD
-100 type) and push from about 10mmφ dice
The pellets are cut at the same time as they are put out, and solid detergent pellets (about 10 mm in diameter)
mm, length 70 mm or less) (pelleter (cutter)
-) Cutter peripheral speed is 5 m / s). Then, the obtained paper
Also described in Tables 1 to 9 as a crushing aid in a red solid detergent
(Additional species and amount are listed in the table), and cool air (temperature approx.
At 15 ° C, the ratio of wind (spirit) to kneaded product (solid) is approx.
2.5m³/ Kg, wind speed 20m / s) 3 stages in series in coexistence
Fitzmill (Hosokawa Micron Corporation)
(DKSO-6 type) and crushed using a rotary crushing blade.
The peripheral speed and the screen diameter are described in Tables 10 to 15). Got
The temperature of the crushed product is about 25 ° C and the average particle size is about 500 μm.
Was. <Production Example 4> The dry powder components shown in Tables 1 to 9
Dissolve and disperse in tap water (Edogawa-ku, Tokyo) (60 rpm)
rpm, jacket temperature 70 ° C), solid content concentration approx. 60
% Slurry was prepared. Using a countercurrent drying tower
And spray-dry (conditions refer to Production Method 1)
(The physical properties of the particles were the same as in Production Method 1). The dried particles obtained
Is a Redigue mixer (Matsubo Co., Ltd., M-20)
Mold) (filling rate 50%), spindle 200rpm,
While stirring under the condition of hopper 6000 rpm (stirring temperature
(Degree: room temperature), granulation process additives and water (Edogawa-ku, Tokyo)
And agitated granulation until the average particle size becomes about 650 μm.
(Stirring temperature: room temperature). Then break the resulting particles
As the crushing aid, those described in Tables 1 to 9 were added.
The amount is described in the table), warm air (temperature about 30 ° C, air (air) and kneading)
The ratio of Japanese (solid) is qi / solid = about 3.0m³/ Kg, wind speed
Fitz arranged in three stages in coexistence
Mill (Hosokawa Micron Co., Ltd., DKSO-6 type)
(The peripheral speed of the rotary crushing blade and the screen diameter are shown in the table.
10-15). The temperature of the obtained crushed product is about 30
° C, average particle size was 500 µm. Nonionic addition method: dripping <Production Example 5> α-SF slurry (water content of about 2
6 mass%, viscosity 7 Pa · s (Brookfield type (B
Type) Measured with a viscometer)) is about 115 kg / hr,
Vacuum thin film evaporator with an evaporation efficiency of about 17 kg / hr (Excel
Ba (Shinko Pantech), transmission surface (surface in contact with slurry)
Product) 0.5m², Clearance 3mm,)
Wall heating temperature about 115 ° C, degree of vacuum about 0.45MPa, rotation
Concentration was performed under the conditions of a blade peripheral speed of 11 m / s. The obtained darkness
The physical properties of the condensed material are about 20% moisture and 20 Pa · s viscosity (blue
(Measured with a Brookfield type (B type) viscometer)
Was. The components added in the granulation process excluding the concentrate were
Introduced to Ige Mixer (M-20, manufactured by Matsubo Corporation)
(Filling rate 50%), spindle 200rpm, chopper 6
While stirring under the condition of 000 rpm (stirring temperature: room
Temperature), concentrate and tap water (Edogawa-ku, Tokyo)
Stir granulation was performed until the average particle size became about 650 μm (stirring
Temperature: room temperature). Next, the obtained particles are used as a crushing aid.
Add the ingredients listed in Tables 1 to 9 (subsidies and amounts are listed in the table).
On), warm air (temperature: about 35 ° C, wind (air) and kneaded material (solid)
The ratio of gas / solid = about 4.0m³/ Kg, wind speed about 18m /
s) Three-stage Fitzmill (Hoso
Crushed using Kawamicron Co., Ltd., DKSO-6 type
(The peripheral speed of the rotary crushing blade and the screen diameter are shown in Table 12.
On). The temperature of the obtained crushed product is about 40 ° C, and the average particle size is about
It was 500 μm. <Production Example 6> The dry powder components shown in Tables 1 to 9
Dissolve and disperse in tap water (Edogawa-ku, Tokyo) (60 rpm)
rpm, jacket temperature 70 ° C), solid content concentration approx. 60
% Slurry was prepared. Using a countercurrent drying tower
And spray-dry (conditions refer to Production Method 1)
(The physical properties of the particles were the same as in Production Method 1). The dried particles obtained
To the Reedige Mixer (M-20, manufactured by Matsubo Corporation)
(Filling rate 50%), spindle 200rpm, chopping
While stirring under the condition of par 6000 rpm (stirring temperature:
Room temperature), granulation process additive and tap water (Edogawa-ku, Tokyo)
And agitated granulation until the average particle size becomes about 650 μm.
(Stirring temperature: room temperature). Then break the resulting particles
As the crushing aid, those described in Tables 1 to 9 were added.
The amount is described in the table), cold air (temperature about 15 ° C, wind (air) and kneading)
The ratio of Japanese (solid) is ki / solid = about 2.5m³/ Kg, wind speed
Fitz arranged in three stages in coexistence
Mill (Hosokawa Micron Co., Ltd., DKSO-6 type)
(The peripheral speed of the rotary crushing blade and the screen diameter are shown in the table.
10-15). The temperature of the obtained crushed product is about 25
° C., the average particle size was about 500 μm. <Evaluation of adhesion of detergent composition in crusher
> Shown in the section "Crusher peripheral speed and rotation speed" in Tables 10 to 15
Depending on the conditions, the peripheral speed is 50 m / s at 50 Hz, and the number of rotations is 470.
Using a 0rpm crusher, a crusher for multi-stage crushing
The amount of adhesion in the sample was evaluated as follows. Table 10 shows the results.
FIG. -Evaluation of adhesion amount in crusher- *: The amount of adhesion in the crusher is small. ・ △: Despite the adhesion to the crusher, but no problem
Is the amount of adhesion. *: The adhesion amount in the crusher is large. In the present embodiment, the static bounce of the solid detergent
The sexual behavior was measured as follows. << Measurement of static elasticity of solid detergent >> Bending of solid detergent
・ The stresses such as tension and shear are converted to the strain (change
Position), the Leotech (formerly Fudo Kogyo)
Using a rheometer manufactured by the Company under the following conditions:
I did. -Sample adjustment- Using the sample immediately after kneading and dough formation,
(0 × 50 × 5 mm). When the material to be crushed is granular
The kneading (kneading) apparatus, for example, KRC
Using a kneader [made by Kurimoto Iron Works Ltd.]
Mold into the above shape. At this time, the temperature of the molding container is
Use at the same temperature as the sample or at about + 5 ° C for molding
You. -Measurement method- After molding the sample, place the sample on the stage
Transfer the pull and apply the load at a constant speed from above
Measure the strain (displacement) of the sample. The condition is
Using a head capable of measuring load up to 2kg, 2mm / mi
Apply a load at speed n. With a hardness of 2kg or more
Uses a head capable of measuring a load up to 10 kg. Load
The position to apply is to divide the long side direction of the molded sample into two
Part with a width that traverses in the short side direction at this position
Apply the load with the attachment. -Data processing- When the sample and attachment come into contact,
The place where the maximum was reached was the end point, and it was applied from the base point to the end point
The load is hardness [g], and the changed length in the load direction is strain (change).
Position) [mm]. [0170] [Table 1][0171] [Table 2] [0172] [Table 3][0173] [Table 4] [0174] [Table 5][0175] [Table 6] [0176] [Table 7][0177] [Table 8] [0178] [Table 9][0179] [Table 10] [0180] [Table 11] [0181] [Table 12]In Table 12, “*” indicates the first stage.
Uses two types of screens. [0183] [Table 13] [0184] [Table 14] [0185] [Table 15] The raw materials used in the present invention are shown below.
You. In addition, "%" means mass%. Α-SF-Na: C obtained by the following production method
Alpha sulfo fatty acid nato having a 14-16 alkyl chain
Lithium (65.6% pure and other, methyl sulfate
3.28%, sodium sulfate 1.31%, alpha sul
3.08% of sodium salt of fatty acid sodium, methanol 1.
51%, unreacted methyl ester 1.21%, water 24.0
1%), provided that the sodium alpha sulfo fatty acid is
7% equivalent in the detergent composition manufacturing process, and more detergent composition
25% equivalent of alpha sulfo in long term storage
May be converted to sodium salt of fatty acid sodium. (Production method) Thin-film reactor (single tube, inner diameter = 10 m)
m, reactor length = 2.5 m)
Methyl myristate (manufactured by Lion Corporation, Pastel M-
14) and methyl palmitate (Lion Co., Ltd., Paste
M-16) mixed at a weight ratio of 2: 8.
Using an ester (iodine value 0.40, molecular weight 264)
SO₃Liquid SO as gas equipment₃Using the dilution gas
8% SO using nitrogen gas₃Containing inert gas and
And the reaction molar ratio (SO₃/ Methyl ester) = 1.2
Perform the gas absorption reaction in a thin film reactor, and after gas-liquid separation,
An aging reaction at 80 ° C. for 60 minutes was performed, and the reaction rate was 97%.
Fonic acid was obtained. Then 20% by weight of methanol to sulfone
Acid, 35% aqueous hydrogen peroxide (2% as pure hydrogen peroxide
Sulfonic acid), and after uniform mixing, drift at 80 ° C for 180 minutes.
A white reaction was performed. Then with aqueous sodium hydroxide
Perform neutralization reaction to neutralize 47% concentration (surfactant concentration)
Product, and recycle flash concentration to methanol
(Reused by rectification in a later step), water is evaporated to 65.6
% Concentrated (surfactant concentration) neutralized product was obtained. Color
(A 5% by weight ethanol solution was passed through a 40 mm optical path length, No. 4
2 Measured with a Krett photoelectric meter using a blue filter
Constant) was 30. LAS: Rypon LH-200 (Rio
(Made in February 2001) AOS-K: carbon obtained by the following production method
Α-Olefi of the number 14: 16: 18 = 15: 50: 35
Potassium sulfonate and hydroxyalkylsulfonic acid
Mixture of potassium (pure content 70%, α-olefin sulfone
Potassium acid: Potassium hydroxyalkyl sulfonate
The ratio is 7: 3, the remainder is unreacted α-olefin, sodium sulfate
(Lium, sultone, sodium hydroxide, water, etc.) (Production method) α-olefin (Dialen 14 at 25 ° C)
8, Mitsubishi Chemical Corporation) at a capacity of 970 kg / hr
Successive TO reactors (TO-500, Lion Corporation)
, Film type reactor)₃gas
At about 35 ° C.
α-olefin sulfonic acid and impurities (mainly sultone)
The resulting sulfonate was obtained. This sulfonated product 1370k
g / hr, 630 kg / hr of caustic potash (moisture 52%
Aqueous solution) to perform a neutralization reaction,
Potassium olefin sulfonate was obtained. In this impurity
Shell and tube type to hydrolyze sultone
Heat the temperature to 140 ° C through a heat exchanger, and further react
Keep it at 170 ° C through 1.4MPa steam in a coiled tube.
That is, hydrolysis was promoted. Then, at pressure of 1MPa
Rush concentration and dehydration were performed to reduce the water content to about 27%. This
The pure content of AOS-K thus obtained is usually 66-74%
And the main component is potassium α-olefin sulfonate (about 7
0%) and potassium hydroxyalkyl sulfonate (about 3%).
0%), and the color is (10% solution LK value) 70,
1.8% of free alkali (KOH) (AOS-K pure
Minute). ・ Soap: stone obtained by the following production method
The soap has an AI of 66 to 67%, and as an impurity,
0.01% fatty acid, about 0.2% unreacted fatty acid ester
About 0.2% NaOH, about 0.4% methanol
Including. (Production method) Fatty acid methyl ester (P
Stele MC-O *, manufactured by Lion Oreo Chemical Co., Ltd.)
1576 kg / h, 48% NaOH aqueous solution at 40-60 ° C
Liquid 445 kg / h, water (Lion Chiba Plant Nakasui) 336
kg / h to the mixing pump continuously
110-130 ° C with & tube type heat pre-heater and pre-heater
The saponification reaction was allowed to proceed for 9 to 10 minutes while maintaining (reaction
Rate 99.5 to 99.8%). Then, the overhead pressure is 0.2 to 0.1.
Flash steam with 6 kPa and tower temperature of 98-100 ° C
The reaction product is introduced into the
The ethanol was evaporated. Finally removed the methanol
Soap is introduced into a stirring tank with paddle-type stirring blades and retained
80 ° C while maintaining at 98 ° C with stirring for 140 minutes
Add water and concentrate to a soap concentration of 66-67%.
The degree was adjusted. Nonion 1: Diadol 13 (Mitsubishi Chemical)
12-15 mol adduct of ethylene oxide on average, manufactured by Gaku Co., Ltd.
Was obtained by the following production method. (Production method) 4 liter autoclave (pressure-resistant glass
Diamond Doll 13 (Mitsubishi Chemical Corporation)
400 g) and 2.3 g of a 30% NaOH aqueous solution.
Charge, replace the inside of the autoclave with nitrogen, and stir
The temperature was raised (while dehydrating at 100 ° C for 30 minutes)
). Next, the temperature was set to 180 ° C and the pressure was set to 300 kPa.
While maintaining ethylene oxide (EO: Mitsubishi Chemical
1056 g (average number of moles added: 12) to 1
320 g (average number of moles added: 15) were introduced, and
The reaction between EO 13 and EO was carried out. Finally mature for 30 minutes
Thus, a nonionic surfactant was obtained. In nonionic surfactant
Is about 2.0% of PEG and about 0.1% of unreacted alcohol.
9%. Nonon 2: Diamond Doll 13 (Mitsubishi Chemical)
The average 25 mol ethylene oxide adduct of Gaku Co., Ltd.)
Was obtained by the production method described above. (Production method) 4 liter autoclave (pressure-resistant glass
Diamond Doll 13 (Mitsubishi Chemical Corporation)
400 g) and 2.3 g of a 30% NaOH aqueous solution.
Charge, replace the inside of the autoclave with nitrogen, and stir
The temperature was raised (while dehydrating at 100 ° C for 30 minutes)
). Next, the temperature was set to 180 ° C and the pressure was set to 300 kPa.
While maintaining ethylene oxide (EO: Mitsubishi Chemical
2200g (average number of moles added: 25)
, And reacted with Diamond Doll 13 and EO. last
For 30 minutes to obtain a nonionic surfactant. Nonion
Impurities in the surfactant were about 2.0% PEG, unreacted alcohol
The call was about 0.4%.・ Nonion 3: Diamond
13 (manufactured by Mitsubishi Chemical Corporation)
Propylene oxide 3 mol adduct is produced by the following production method.
Was obtained. (Production method) 4 liter autoclave (pressure-resistant glass
Diamond Doll 13 (Mitsubishi Chemical Corporation)
400 g) and 2.3 g of a 30% NaOH aqueous solution.
Charge, replace the inside of the autoclave with nitrogen, and stir
The temperature was raised (while dehydrating at 100 ° C for 30 minutes)
). Next, maintain the temperature at 180 ° C and the pressure at 3 atm
Ethylene oxide (EO: Mitsubishi Chemical Corporation)
1320 g (average number of moles added: 15).
The reaction between iador 13 and EO is carried out, and the mixture is aged for 30 minutes.
Was. Thereafter, the reaction solution was cooled to a temperature of 120 ° C.
While maintaining a pressure of 300 kPa at 0 ° C., propylene oxa
Id (PO: manufactured by Asahi Glass Co., Ltd.) 350 g (average additional module
And the reaction was carried out. Finally ripened for 30 minutes
To obtain a nonionic surfactant. Nonionic surfactant
Approximately 2.0% of PEG and approximately unreacted alcohol
0.7%. ・ Nonion 4: Emarex 705 (Nippon Emulsion
(Manufactured by Corporation: purchased in October 1999) ・ Zeolite: 4A zeolite (Mizusawa Chemical Co., Ltd.)
(Made in February 2001) -Potassium carbonate: food grade (Asahi Glass Co., Ltd .: 20
(Purchased in April 2001) ・ Sodium sulfite: Anhydrous sulfite (Shinshu Chemical Co., Ltd.)
Made: Purchased in January 2001) ・ Sodium carbonate: Granulated ash (made by Asahi Glass Co., Ltd .: 2001)
(Purchased in January) MA agent: Aquaric TL-400 (JP
Made by this catalyst: Purchased in February 2001) -Glauber's salt: neutral anhydrous sodium sulfate (manufactured by Shikoku Chemicals Co., Ltd .: 199)
(Purchased in February 2009) PAA: Junron PW-111, average molecular weight 400
Man (manufactured by Nippon Pure Chemical Co., Ltd.) -Sodium silicate: JIS No. 1 sodium silicate
Umm (Nippon Chemical Industries: Purchased in April 2000) ・ Fluorescent agent: Tinopearl CBS-X (Ciba Specialty)
Chemicals: Purchased December 1999) or / or
AMS-GX (Ciba Specialty Chemicals: 199
(Purchased in December 2009) ・ Zeolite (crushing aid): Zeolite (Cosmo:
(Purchased in January 2000) ・ Sodium carbonate (crushing aid): Granulated ash (Asahi Glass Co., Ltd.)
(Purchased in January 2001) to an average particle size of 10 to 20 μm
Crushed [0193] According to the present invention, the physical properties of powder are deteriorated.
Granular detergent composition without adhesion to crushers etc.
A method for manufacturing a product can be provided.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 shows the hardness and strain (displacement) of a solid detergent.
FIG. FIG. 2 is a schematic diagram showing a mixing order of slurries in Examples. FIG. 3 is a schematic diagram showing a mixing order of slurries in Examples. FIG. 4 is a schematic diagram showing a mixing order of slurries in Examples. FIG. 5 is a schematic diagram showing a mixing order of slurries in Examples. FIG. 6 is a schematic diagram showing a mixing order of slurries in Examples.

Claims (1)

Claims: 1. A method for producing a granular detergent composition, which comprises crushing a solid detergent containing at least a surfactant and a builder to produce a granular detergent composition. Depending on the values of hardness and strain (displacement),
A method for producing a granular detergent composition, comprising crushing under any of the conditions (c). (A): Hardness of solid detergent is 50 ≦ hardness [g] <1000
And the strain (displacement) is 1.0 ≦ strain (displacement) [mm] <
2.5 and the hardness of the solid detergent is 1000
≤ hardness [g] ≤ 3000 and strain (displacement) 1.0 ≤
If the strain (displacement) [mm] <4.8 is satisfied, 2
Hot air of 6 ° C. or more is supplied to the crusher, and the peripheral speed of one or more rotating bodies of the crushing granulator is set to 50 m / s or less to perform a crushing process. (B): The hardness of the solid detergent is 50 ≦ hardness [g] <1000
And the strain (displacement) is 5.0 ≦ strain (displacement) [mm] ≦
8.0 and the hardness of the solid detergent is 1000
When ≦ hardness [g] ≦ 3000 and strain (displacement) satisfies 4.8 ≦ strain (displacement) [mm] ≦ 8.0, 25
Crushed air is supplied to the crusher at a temperature of less than ℃. (C): The hardness of the solid detergent is 50 ≦ hardness [g] <1000
And the strain (displacement) is 2.5 ≦ strain (displacement) [mm] <
When 5.0 is satisfied, the peripheral speed of the rotating body of one or more crushing granulators is set to 50 m / s or less, and crushing processing is performed.