JP2000160200A - Production of compression-molded detergent - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method for producing a compression-molded detergent, enabling the production of the compression-molded detergent having excellent disintegrating and dispersing characteristics in a short time and in good productivity. SOLUTION: This method for producing a compression-molded detergent comprises (1) a process for stirring and granulating a detergent composition having the same composition as those of preliminarily formed granulates in the presence of the preliminarily formed granulates to produce the detergent granules having an average granule diameter of 300-1,500 μm and a bulk density of 0.6-1.2 g/ml, (2) a process for classifying the obtained detergent granules, and (3) a process for compression-molding the obtained detergent granules.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to a method for producing a compacted detergent excellent in disintegration and dispersion characteristics in a short time and with high productivity.

[0002]

2. Description of the Related Art Conventionally, as a form of a detergent, a liquid type and a granular type are known. Current,
In particular, granular detergents are widely used. However, granular detergents have a problem of scattering of detergent particles at the time of use. In consideration of the convenience of handling by users, particularly recently, attempts have been made to process the granular detergents into tablets (tablets and briquettes). ing. For example, Japanese Patent Laid-Open No. 4-2538
Japanese Patent Application Publication No. 00-114,086 discloses that a tablet detergent is produced by compression-molding such a granular detergent by setting the particle size of the granular detergent constituting the tablet within a predetermined range. It is disclosed that using a granular detergent having a uniform diameter improves the disintegration and dispersing properties of tablets.

[0003] However, when a granular detergent is produced by stirring granulation, the particle size distribution of the granular detergent is relatively wide. Also, if the classification is attempted to narrow this wide particle size distribution, there is a problem that a large amount of coarse particles and fine particles not used for compression molding are generated, and the productivity is reduced.

[0004]

SUMMARY OF THE INVENTION Accordingly, an object of the present invention is to provide a method for producing a compression-molded detergent having excellent disintegration and dispersion characteristics with good productivity.

[0005]

SUMMARY OF THE INVENTION In preparing detergent particles having a specific range of particle size, the present inventors have prepared a pre-granulated detergent granule in the presence of a pre-granulated detergent granulate. By granulating the detergent composition having the same composition as the granulated product by stirring granulation, unexpectedly, compared to the case where the granulated material was stirred in the absence of such a pre-granulated product. ,
It was found that the particle size distribution of the detergent particles was sharpened early. The present invention has been made based on such new findings. That is, the present invention is a method for producing a compression-molded detergent, comprising the following steps: (1) a detergent having the same composition as the previously-granulated granules in the presence of the previously-granulated granules; Stir granulate the composition,
A step of producing detergent particles having an average particle size of 300 to 1500 μm and a bulk density of 0.6 to 1.2 g / ml; (2) a step of classifying the resulting detergent particles; and (3) a compression molding of the resulting detergent particles. A method comprising the steps of:

[0006]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in more detail. The method of the present invention is applied when compression-forming detergent particles containing various surfactants. Preferred components of the detergent composition used to form the detergent particles used in the present invention include the following. (1) Surfactant (a) Anionic surfactant Preferred anionic surfactants include, for example, straight-chain or branched-chain alkylbenzene sulfonates having an alkyl group having 8 to 16 carbon atoms, and those having 10 to 20 carbon atoms. Alkyl sulfate (AS) salt or alkenyl sulfate, having 10 to 2 carbon atoms
Α-olefin sulfonic acid (AOS) salt of 0, carbon number 1
0 to 20 alkanesulfonate, having a linear or branched alkyl or alkenyl group having 10 to 20 carbon atoms, and having an average of 0.5 to 8 mol of ethylene oxide, propylene oxide, butylene oxide or ethylene oxide / Propylene oxide = 0.1 / 9.9-9.
Alkyl ether sulfuric acid (AE) added at a ratio of 9 / 0.1
S) Salt or alkenyl ether sulfate, having 10 to 10 carbon atoms
Having 20 linear or branched alkyl or alkenyl groups, an average of 0.5 to 8 moles of ethylene oxide,
Propylene oxide, butylene oxide or ethylene oxide / propylene oxide = 0.1 / 9.9
Alkyl carboxylate or alkenyl ether carboxylate added at a ratio of の 9.9 / 0.1, alkyl polyhydric alcohol ether sulfate such as alkyl glyceryl ether sulfonic acid having 10 to 20 carbon atoms, Higher fatty acid salts having from 20 to 20 carbon atoms, saturated or unsaturated α-sulfofatty acid (α-SF) salts having 8 to 20 carbon atoms, or anionic surfactants such as methyl and ethyl, especially propyl esters, or mixtures thereof. be able to. Particularly preferred anionic surfactants include, for example, alkali metal salts of linear alkylbenzene sulfonic acid (LAS) (eg, sodium or potassium salts).
And alkali metal salts of AOS, α-SF, and AES (eg, sodium or potassium salts) and alkali metal salts of higher fatty acids (eg, sodium or potassium salts).

(B) Nonionic surfactant Preferred nonionic surfactants include, for example, the following. (i) an aliphatic alcohol having 6 to 22 carbon atoms, preferably 8 to 18 carbon atoms and an alkylene oxide having 2 to 4 carbon atoms on average of 3 to
30 mol, preferably 5 to 20 mol, of a polyoxyalkylene alkyl (or alkenyl) ether added. Among them, polyoxyethylene alkyl (or alkenyl) ether and polyoxyethylene polyoxypropylene alkyl (or alkenyl) ether are preferable.
As the aliphatic alcohol used here, a primary alcohol or a secondary alcohol is used. Further, the alkyl group may have a branched chain. As preferred aliphatic alcohols, primary alcohols are used. (ii) polyoxyethyl alkyl (or alkenyl) phenyl ether. (iii) A fatty acid alkyl ester alkoxylate represented by the following formula, in which an alkylene oxide is added between ester bonds of a long-chain fatty acid alkyl ester.

R ¹ CO (OA) n OR ² (R ¹ CO represents a fatty acid residue having 6 to 22 carbon atoms, preferably 8 to 18 carbon atoms; OA represents a fatty acid residue having 2 to 4 carbon atoms such as ethylene oxide and propylene oxide; It preferably represents an addition unit of alkylene oxide of 2 to 3. n represents an average number of added moles of alkylene oxide, and generally represents 3 to 3
0, preferably a number from 5 to 20. R ² has 1 carbon atom
Represents a lower alkyl group which may have 1 to 3 substituents. (Iv) Polyoxyethylene sorbitan fatty acid esters. (v) Polyoxyethylene sorbite fatty acid esters. (vi) Polyoxyethylene fatty acid esters. (vii) Polyoxyethylene hydrogenated castor oil. (viii) glycerin fatty acid esters.

Among the above-mentioned nonionic surfactants, polyoxyethylene alkyl (or alkenyl) ethers and polyoxyethylene polyoxypropylene alkyl (or alkenyl) having a melting point of 40 ° C. or less and an HLB of 9-16.
Particularly preferred are fatty acid methyl ester ethoxylates in which ethylene oxide is added to ethers and fatty acid methyl esters, and fatty acid methyl ester ethoxypropoxylates in which ethylene oxide and propylene oxide are added to fatty acid methyl esters. Further, these nonionic surfactants may be used as a mixture. (C) Amphoteric surfactant Preferred ampholytic surfactants include, for example, imidazoline-based and amidobetaine-based amphoteric surfactants. Particularly preferred amphoteric surfactants include
For example, 2-alkyl-N-carboxymethyl-N-hydroxyethylimidazolinium betaine, amide amide propyl betaine and the like can be mentioned.

[0010] The above-mentioned surfactant is usually 10 to 60% by weight, preferably 15 to 5% by weight, based on the weight of the detergent particles.
0% by weight, particularly preferably 20 to 45% by weight. (2) Detergent builder As a detergent builder, an alkali builder or a chelate builder usually used for a detergent is preferably used. (A) As alkali builders, sodium carbonate, sodium hydrogen carbonate, potassium carbonate, potassium hydrogen carbonate,
There are alkali metal carbonates such as sodium potassium carbonate and alkali metal silicates such as sodium silicate, potassium silicate and layered sodium silicate. (B) Examples of the chelate builder include aluminosilicate, tripolyphosphate, pyrophosphate, citrate, succinate, polyacrylate, acrylic acid-maleic acid copolymer, iminocarboxylic acid / salt, EDTA, etc. There is. Detergent builders are typically 10 to 9 based on the weight of the detergent particles.
0% by weight, preferably 20 to 80% by weight, particularly preferably 30 to 70% by weight.

(3) Oil-absorbing carrier The oil-absorbing carrier used in the present invention is preferably
Oil absorption is 80m as specified by JIS-K5101 test method
1/100 g or more, preferably 150 to 600 ml / 1
An oil-absorbing substance of 00 g is preferably used. As such an oil-absorbing carrier, for example, as a silicate compound, Tokusil N [manufactured by Tokuyama Co., Ltd .;
1/100 g], Nip Seal NS-K [Nippon Silica Co., Ltd., oil absorption 320 ml / 100 g], Sylysia # 310 [Fuji Silysia Chemical Ltd., oil absorption 340 m]
1/100 g], amorphous hydrous amorphous silicic acid, Sildex H-52 [manufactured by Asahi Glass Co., Ltd., oil absorption 260 ml / 1
Aerosol # 300 [manufactured by Nippon Aerosil Co., Ltd., oil absorption 350 m1]
/ 100 g], and amorphous anhydrous silicic acid, such as Florite R (manufactured by Tokuyama Corporation, oil absorption 600 ml / 100 g)
g], etc., petal-like hydrated amorphous calcium silicate, zonotrite [manufactured by Ube Chemical Co., Ltd., oil absorption 220 m1 / 100
g], etc., acicular hydrated amorphous calcium silicate, amorphous aluminosilicate [manufactured by Mizusawa Chemical Co., Ltd., oil absorption 170 ml / 1
00g], magnesium silicate [oil absorption 180ml / 10
0g]. As a carbonate compound, magnesium carbonate [manufactured by Tokuyama Corporation, oil absorption amount 150 ml / 1
00g], calcium carbonate (manufactured by Shiroishi Kogyo Co., Ltd., oil absorption 110ml / 100g), and as other compounds, ultrafine spinel [manufactured by Sumitomo Cement Co., Ltd., oil absorption 600m
1/100 g], ultrafine particle cordierite [manufactured by Sumitomo Cement Co., Ltd., oil absorption 600 ml / 100 g], ultrafine particle mullite [manufactured by Sumitomo Cement Co., oil absorption 560 ml]
/ 100 g], modified starch Pineflow-S [manufactured by Matsutani Chemical Co., Ltd., oil absorption amount 130 m1 / 100 g] and the like. These oil absorbing carriers may be used as a mixture.

The oil-absorbing carrier is usually 0.1 to 25% by weight, preferably 0.5 to 25% by weight, based on the weight of the detergent particles.
The content is 20% by weight, particularly preferably 1 to 15% by weight. (4) Clay mineral The clay mineral used as the detergent component of the present invention includes:
In particular, those belonging to the smectite group and having a crystal structure of a dioctahedral three-layer structure or a trioctahedral three-layer structure are preferable. The clay mineral which can be preferably used as the detergent component of the present invention preferably has an oil absorption of 80 ml.
/ 100g, more preferably 30-70ml / 10
It is 0 g and the bulk density is preferably 0.1 g / ml or more, particularly preferably 0.2 to 1.5 g / ml. Specific examples of such clay minerals include, for example, montmorillonite (oil absorption: 50 m1 / 100 g, bulk density: 0.3 g / ml), nontronite (oil absorption: 40m1 / 100g, bulk density:
0.5g / ml), beidelite (oil absorption: 62m1 / 10
0 g, bulk density: 0.55 g / ml), pyrophyllite (oil absorption: 70 m1 / 100 g, bulk density: 0.63 g / ml), etc. On the other hand, clay having a trioctahedral type three-layer structure Saponite (oil absorption: 73 m1 /
100 g, bulk density: 0.15 g / ml), hectorite (oil absorption: 72 m1 / 100 g, bulk density: 0.7 g / ml), stevensite (oil absorption: 30 m1 / 100 g, bulk density 1.2 g / ml) , Talc (oil absorption: 70m1 / 100g,
Bulk density: 0.1 g / ml). Clay minerals
Usually 0.1 to 30% by weight, based on the weight of the detergent particles,
Preferably from 0.5 to 20% by weight, particularly preferably from 1 to 20% by weight.
-10% by weight. The raw material components (1) to (4) may be mixed with a slurry and then spray-dried to form a dry powder. The following are shown as specific examples of the components blended in the other detergents.

(5) Fluorescent agents: bis (triazinylamino) stilbene disulfonic acid derivatives, bis (sulfostyryl) biphenyl salts [Tinopearl CBS] and the like. (6) Enzymes: lipase, protease, cellulase, amylase and the like. (7) Bleaching agents: percarbonates, perborates, etc. (8) Antistatic agents: cationic surfactants such as dialkyl-type quaternary ammonium salts. (9) Surface modifier: fine calcium carbonate, fine zeolite, polyethylene glycol and the like. (10) Anti-redeposition agent: cellulose derivatives such as carboxymethyl cellulose. (11) Extenders: sodium sulfate, potassium sulfate, sodium hydrochloride and the like. (12) Reducing agents: sodium sulfite, potassium sulfite and the like. (13) Fragrances (14) Pigments (15) Softener The enzymes, bleaching agents and softeners are usually used in the form of particles.

In the method of the present invention, before the detergent particles are compression-molded, a dissolution accelerator for promoting the disintegration and solubility of the compression-molded article after compression molding, especially a granular dissolution accelerator, is mixed. Preferably. As preferred dissolution promoters, those described in JP-A-7-286199 can be used as appropriate. Such dissolution promoters include, for example, potassium carbonate, inorganic ammonium salts such as ammonium sulfate and ammonium chloride, sodium benzoate, sodium benzenesulfonate, sodium p-toluenesulfonate, sodium xylenesulfonate, sodium chloride, citrate Water-soluble substances such as acids, D-glucose, urea, and sucrose are exemplified.

Further, as a dissolution accelerator used in the present invention,
In addition, a swellable water-insoluble substance is also preferable. In particular,
Powdered cellulose, crystalline cellulose, low etherification carboxymethyl cellulose, cross-linked carboxymethyl cellulose, carboxymethyl cellulose calcium,
Cellulose derivatives such as hydroxypropyl cellulose,
Examples thereof include starch such as corn starch, starch derivatives such as hydroxypropyl starch, crosslinked polyvinylpyrrolidone, polyvinyl alcohol having a low degree of etherification, and the like. These are also preferably granulated beforehand, and particularly preferably those having an average particle diameter of 200 to 1500 μm. The dissolution promoter is usually 1 to 50% by weight, preferably 5 to 30% by weight, based on the weight of the detergent particles before compression molding.
Suitably, it is in an amount of weight percent.

The pre-granulated granules used in the present invention are granulated by any granulation method as long as they have the same composition as the newly granulated detergent composition which is stirred and granulated in the presence thereof. It may be done. For example, the granulation method includes a stirring granulation method, a tumbling granulation method, a fluidized bed granulation method, an extrusion granulation method, a kneading / crushing granulation method, and the like. In particular, in consideration of a continuous process, it is appropriate to produce the particles by a stirring granulation method. However, the manufacturing method of the granulated material that has been granulated in advance is not limited to the method using the stirring granulation method. The stirring granulation method, the tumbling granulation method, the fluidized bed granulation method, the extrusion granulation method, and the kneading / crushing granulation method itself are already well-known methods. The stirring granulation method will be specifically described below. Further, as the pre-granulated granules, for example, a portion not used for compression molding generated in the classifying step may be added with pre-granulated detergent particles, or the detergent composition may be added in a batch operation. In the case of granulation, a part of the detergent particles of the previous batch may be left in the agitation granulator, and this may be granulated together with the raw material of the new detergent composition as granulated granules in advance. In particular, when manufacturing a briquette detergent, burr pieces generated in the step of removing the burr of the briquette may be used as detergent granules previously granulated.

The pre-granulated material is used in an amount of, for example, 0.1 to 50% by weight, preferably 1 to 30% by weight based on the weight of the total detergent composition to be stirred and granulated. It is appropriate to do so. If this amount is less than 0.1% by weight, the particle size distribution of the detergent particles tends to be widened, the amount of fine powder and coarse powder tends not to decrease, and the granulation time is hardly shortened. On the other hand, if this amount exceeds 50% by weight, the productivity of the method of the present invention tends to decrease. The average particle size of the granulated product in advance is usually 150 to 1200 μm, and preferably 200 to 1000 μm. Further, the bulk density of the granulated granules in advance is usually 0.
It is suitably from 4 to 1.2 g / ml, preferably from 0.6 to 1.2 g / ml.

In the present invention, a detergent composition having the same composition as the pre-granulated granules is stirred and granulated in the presence of the pre-granulated granules to obtain an average particle size of 300-300. 1500μ
m and detergent particles having a bulk density of 0.6 to 1.2 g / ml. In the stirring granulation, as a stirring granulator, a stirring blade is provided inside a granulator such as a high-speed mixer, a sugar mixer, a Loedige mixer, and a distance of 30 mm is provided between the stirring blade and the inner wall of the granulator. By introducing and treating a surfactant, a detergent builder, components that can be optionally added, and / or their spray-dried particles into an internal stirring type granulator having the following clearance, the granulated product is processed. Can be manufactured. The temperature of the stirring granulation is generally 10 to 60.
° C, preferably 20 to 50 ° C, more preferably 35 to 5 ° C.
0 ° C. If the temperature is lower than 10 ° C., granulation hardly proceeds, which is not preferable. On the other hand, if the temperature is higher than 60 ° C., on the contrary, adhesion to the granulator occurs, and the load tends to be excessive, which is not preferable. The processing time in the stirring granulation is usually 1 to 20 minutes, preferably 2 to 1 minute.
5 minutes.

The average particle size of the agglomerated detergent particles is 30.
It is from 0 to 1500 μm, preferably from 400 to 1200 μm. When the average particle size is less than 300 μm, the porosity of the compression-molded product formed by compression molding of the detergent particles is reduced, so that the disintegration in water deteriorates, while the average particle size exceeds 1500 μm If the compression-molded product disintegrates in water, the solubility of the dispersed detergent particles deteriorates, which is not preferable. The bulk density of the agitated and granulated detergent particles is 0.6 to 1.2 g / ml, preferably 0.7 to 1.2 g / ml. Although slightly different depending on the composition,
If the bulk density is less than 0.6 g / ml, the detergent particles are easily crushed during compression molding, and the porosity of the compression molded product is reduced, so that the disintegration in water is deteriorated, while the bulk density exceeds 1.2 g / ml. If the compression-molded product disintegrates in water, the solubility of the dispersed detergent particles deteriorates, which is not preferable.

The detergent particles thus obtained are then classified. By this classification, detergent particles having a uniform particle size range are formed, and the disintegration and dispersibility of a compression-molded detergent such as a tablet or a briquette detergent obtained through compression molding described below are greatly improved. Classification is, for example,
By using a sieve having a predetermined mesh size, it can be easily performed. The degree of classification can be arbitrarily selected according to the desired disintegration, dispersibility and the like.
For example, the particle size can be set to 150 to 3000 μm, preferably 300 to 2000 μm by classification. The classified detergent particles are then subjected to compression molding. Examples of the compression molding method include a tablet method and a briquette method.

In the tablet method, a tableting machine basically comprising a combination of a die and a punch and a compression device is used.
When pressure is applied between the mortar and the punch through the compression device,
A tablet having a shape formed by the mortar and the punch is formed.
Examples of such a tableting machine include a single-shot tableting machine and a rotary tableting machine. As the single-shot tableting machine, for example,
Solid powder molding machines manufactured by Kikusui Seisakusho Co., Ltd., single-shot tableting machines manufactured by Okada Seiko Co., Ltd., standing presses manufactured by Fuji Pharmaceutical Machinery Co., Ltd., and the like. ) Kikusui Seisakusho clean press series, tough press series, FETTE P series, PT series, KORSCH PH series, TRP series, and the like. The shape of the tablet is arbitrary, and is determined in consideration of the convenience of handling by the user. Examples of the shape of the tablet include a cylindrical shape, a cubic shape, and a rectangular parallelepiped shape. As the cylindrical shape, for example, one having a diameter of several mm to 70 mm, preferably 10 to 50 mm is suitable. In the case of a cube or a rectangular parallelepiped, for example, the side (the longest side in a rectangular parallelepiped) has a length of several mm to 70 mm, preferably 10 to 50 mm.

On the other hand, the briquetting method is performed by a roll press. Briquetting machines used for roll pressing are well known and readily available or available to those skilled in the art. A briquetting machine generally has a pair of rolls which are formed at predetermined positions on the outer periphery of the corresponding rolls so as to form a briquette portion having a desired shape and rotate counterclockwise at the same speed. Briquetting machines having a feeder with a hopper and a feed screw for supplying the detergent composition to the clearance formed between the rolls are particularly suitable. In using a briquetting machine having a feeder, the detergent composition is inserted into the clearance from the inlet of the clearance by using the pressing force of the feed screw through the feeder, and the briquette is discharged from the outlet on the side opposite to the feeder side. I do.

The briquette can be obtained as a sheet-shaped primary molded product in which briquettes are connected by a connecting portion or individual briquettes, depending on the clearance between rolls, the pressing pressure between rolls, the insertion pressure, and the like. Can be The shape of the briquette is arbitrary and is determined in consideration of the convenience of handling by the user. As the shape of the briquette, for example, spherical or elliptical, or
The vertical projection image on the sheet surface is circular or elliptical, but the horizontal projection image on the sheet surface is an elliptical or almond-shaped flat sphere or flat elliptical sphere, or the sheet vertical projection image is a square or rectangle. However, the projected image on the sheet surface in the horizontal direction is a circular cylinder, or the projected image on the sheet surface in the vertical direction is a square or a rectangle, but the projected image on the sheet surface in the elliptical or almond shape is a flat cylindrical shape. Things. As the circular or elliptical image projected in the sheet surface vertical direction, for example, the one having a diameter (a major axis in an elliptical shape) of 2 to 40 mm, preferably 3 to 20 mm is suitable. Examples of a square or rectangular image projected in the sheet surface vertical direction include those having a side (long side in a rectangle) of 2 to 40 mm, preferably 3 to 20 mm.
Further, the thickness of the briquette (the length of the briquette portion in the direction perpendicular to the sheet surface) is, for example, 2 to 40 mm, and preferably 3 to 40 mm.
20mm.

The clearance between the pair of rolls is, for example, 0.05 to 2 mm, preferably 0.1 to 1 mm. In this case, the thickness of the connecting portion connecting the briquettes is
Usually, the thickness is the same as the width of the clearance, but a briquette machine of a type in which the roll is retracted according to the molding pressure during the roll pressing and the clearance is widened can also be suitably used, and in this case, it is not limited. The shortest distance between briquettes is, for example, 0.05 to 5 mm, usually 0.1 mm.
３3 mm. If a briquette is obtained as a primary molded body such as a sheet, it may be subjected to a crushing step. Here, “crushing” is an operation of applying an external force to the connecting portion to separate the briquette from the primary molded body and, preferably, substantially remove burr of the briquette. In the crushing step, the type of crusher used in the crushing step is not particularly limited as long as briquettes are individually separated from the primary compact and burrs are removed. A preferred crusher is a crusher equipped with a rotating blade, and a hammer mill type is particularly suitable. As such a crusher, for example, Fitzmill (manufactured by Hosokawa Micron Corp.), Fezamil (manufactured by Hosokawa Micron Corp.), speed mill (manufactured by Okada Seiko Co., Ltd.), Cominuta (Fuji Paudal Corp.) )
And the like.

In the crusher, the peripheral speed of the tip of the blade is generally 0.4 to 15 m / s, preferably 1 to 1 m / s.
0 m / s is mentioned as a suitable thing. If the tip peripheral speed exceeds 15 m / s, the briquette portion is easily broken, which is not preferable. On the other hand, the tip peripheral speed is 0.4 m / s
If it is less than 1, it becomes difficult to separate the briquette portion from the primary molded body, which is not preferable. In addition, in order to further improve the appearance of the briquette detergent product, in order to remove the burr of the briquette portion remaining after crushing, the product was treated with a rolling sizing machine such as a marmelizer (Fuji Paudal Co., Ltd.). You may. However, it is preferable to perform the treatment for a minimum time such that the surface of the obtained briquette detergent does not become smooth. In the crushing step, since a briquette detergent formed from the briquette portion and a crushing residue are generated, the crushing residue is removed and the briquette detergent is collected. The crushed residue may be collected and reused as a detergent composition raw material in the method of the present invention.

The subsequent steps including compression molding are as follows:
Usually, it is appropriate to carry out the reaction at 70 ° C. or lower, preferably 50 ° C. or lower. In particular, when an enzyme is contained in the detergent composition, it is important to maintain the enzyme at a temperature at which the enzyme is hardly deactivated. is there. The compression molded detergent thus obtained generally has a bulk density of 0.7 to 1.6 g / ml, preferably 0.8 to 1.6 g / ml.
Suitably, it is ~ 1.4 g / ml.

[0027]

Hereinafter, the present invention will be described in more detail with reference to Reference Examples, Examples and Comparative Examples.
It is not limited in any way by these examples. [Granulation method A] Spray-dried particles or powder raw materials having the composition shown in Table 1 or 2 described below are charged into a Lodige mixer (M20, manufactured by Matsubo Corporation) (filling ratio: 5
0%), a nonionic surfactant, water and the like were added with stirring, and the mixture was stirred and granulated until the average particle diameter became 700 to 900 μm, and the remaining zeolite was added and stirred for 30 seconds. The operating conditions of the Lödige mixer are 200 rpm spindle.
And the chopper was 3000 rpm. [Granulation method B] Except that a high-speed mixer (Fukae Kogyo Co., Ltd., Model FS-25) was used as the stirring granulator,
By the same operation as in the granulation method A, a granulated product was obtained in advance.
The operating conditions of the high-speed mixer were agitator 200 rpm and chopper 1000 rpm.

[0028]

Table 1 Table 1 Component amount (%) LAS-K 19.4% AOS-K 14.5 Soap 2.0 Zeolite 19.8 Sodium carbonate 21.8 Potassium carbonate 5.5 Sodium sulfite 1.8 Silicic acid Soda 4.0 Fluorescent agent 0.3 Nonionic surfactant 4.7 Water and other small components Remaining amount 100.00

[0029]

[Table 2] Table 2 Formulation amount (%) of nonionic surfactant 23% zeolite 30 light sodium carbonate 17 heavy sodium carbonate 25 water, and other small components remaining amount 100.00

Preparation Example 1 (Pre-granulated granulated material A) Spray-dried particles having the composition shown in Table 1 (excluding some nonionic surfactant and water) were obtained by spray drying. Granules were obtained by the granulation method A. This granulated product has an average particle size of 750 μm (bulk density 0.81 g / ml), 7.0% of particles that do not pass through a 12 mesh sieve (1410 μm opening), and 3%.
Particles 2 passing through a 2-mesh sieve (opening 500 μm)
Had 8.2%. A part of the granulated product was left in the granulator as it was, and the remaining particles were used as granulated product A that had been granulated in advance. Preparation Example 2 (Pre-granulated granules B) By spray-drying, spray-dried particles having the composition shown in Table 1 (excluding some nonionic surfactant and water) were obtained, followed by granulation method B Thus, a granulated product was obtained. This granulated product has an average particle size of 770 μm (bulk density 0.82 g / ml), 7.5% of particles that do not pass through a 12-mesh sieve (aperture 1410 μm),
It had 26.7% of the particles passing through a 32 mesh sieve (500 μm mesh). A part of the granulated material is left in the granulator as it is, and the remaining particles are granulated in the form of a granulated material B which has been granulated in advance.
And Preparation Example 3 (Pre-granulated Granules C) Granules having the composition shown in Table 2 were obtained by the granulation method A. This granulated product has an average particle size of 770 μm (bulk density 0.90 g / ml)
7.3% of particles that do not pass through a 12 mesh sieve (aperture 1410 μm) and a 32 mesh sieve (aperture 50
0 μm). A part of the granulated product was left in the granulator as it was, and the remaining particles were used as a granulated product C that was granulated in advance.

Preparation Example 4 (Pre-granulated granules D) Granules having the composition shown in Table 2 were obtained by granulation method B. This granulated product has an average particle size of 840 μm (bulk density 0.92 g / ml)
8.5% of particles that do not pass through a 12-mesh sieve (aperture 1410 μm) and a 32-mesh sieve (aperture 50
0 μm). A part of the granulated product was left in the granulator as it was, and the remaining particles were used as a granulated product D that had been granulated in advance. Preparation Example 5 (Pre-granulated granules E) Spray-dried particles having the composition shown in Table 1 (excluding some nonionic surfactant and water) were obtained by spray drying, and then granulation method A Thus, a granulated product was obtained. This granulated product had an average particle size of 890 μm and a bulk density of 0.82 g / ml. This granulate is J
IS12 mesh sieve (1410μm mesh) and JIS
Classifying using a 32 mesh sieve (500 μm mesh), particles (8.6%) not passing through a 12 mesh sieve,
Particles (20.9%) were obtained that passed through a 32 mesh screen. Among these, particles that do not pass through the 12 mesh screen are crushed by a crusher, and then mixed with particles that pass through the 32 mesh screen,
Granules E that have been granulated in advance (average particle size 420 μm, bulk density 0.
84 g / ml).

Preparation Example 6 (Pre-granulated granules F) Spray-dried particles having the composition shown in Table 1 (excluding some nonionic surfactant and water) were obtained by spray drying. Granulated product (average particle size 850 μm, bulk density 0.
80 g / ml). The granulated material was classified using a JIS 12 mesh sieve (1410 μm mesh) and a JIS 32 mesh sieve (500 μm mesh), and particles (8.1%) not passing through the 12 mesh sieve and particles (17.2) passing through the 32 mesh sieve. %). Particles that do not pass through the 12-mesh sieve are crushed by a crusher, and then mixed with particles that pass through the 32-mesh sieve, and the granulated product F (average particle size: 340 μm, bulk density: 0.83 g) / ml). Preparation Example 7 (Pre-granulated granules G) By the granulation method A, granules having the compositions shown in Table 2 were obtained. This granulated product had an average particle size of 790 μm and a bulk density of 0.93 g / ml.

The granules are classified using a JIS 12 mesh sieve (1410 μm mesh) and a JIS 32 mesh sieve (500 μm mesh), and particles (8.0%) that do not pass through the 12 mesh sieve and pass through the 32 mesh sieve. Particles (25.3%) were obtained. Particles that do not pass through the 12-mesh sieve are crushed by a crusher, and then mixed with particles that pass through the 32-mesh sieve, and the granulated material G that has been granulated in advance is used.
(Average particle size: 400 μm, bulk density: 0.98 g / ml).

Preparation Example 8 (Pre-granulated Granules H) Granules having the composition shown in Table 2 (average particle size 820 μm, bulk density 0.94 g / ml) were obtained by granulation method B. This granulated product was subjected to JIS 12 mesh sieve (1410 μm opening) and JIS
The particles were classified using an S32 mesh sieve (500 μm opening) to obtain particles (8.3%) not passing through a 12 mesh sieve and particles (20.3%) passing through a 32 mesh sieve.
Particles that do not pass through the 12-mesh sieve are crushed by a crusher, and then mixed with particles that pass through the 32-mesh sieve, and the granulated product H (average particle size: 290 μm, bulk density: 0.95 g) / ml). Preparation Example 9 (Pre-granulated granules I and J) By granulation method A, granules having the composition shown in Table 2 were obtained. This granulated product has an average particle diameter of 800 μm and a bulk density of 0.91 g / ml, and 10.3% of particles that do not pass through a 12 mesh sieve (aperture of 1410 μm) and a 32 mesh sieve (aperture of 50 μm).
0 μm). The granulated material was classified using a JIS 12 mesh sieve and a JIS 42 mesh sieve (mesh size: 350 μm), and the particles passing through the 42 mesh were granulated in advance (average particle diameter 190 μm, bulk density 0.96 g / ml). Particles that do not pass through the 12-mesh sieve are pulverized by a pulverizer to obtain granules J (average particle diameter: 1150 μm, bulk density: 0.15 μm).
91 g / ml).

Examples 1 to 6 In a granulator containing pre-granulated granules A to E,
Subsequently, the raw materials of the same composition as these granulated materials are charged,
Granulation was performed by the same production method to obtain detergent particles. Next, the detergent particles were classified using a JIS 12 mesh screen and a JIS 32 mesh screen, passed through a 12 mesh screen,
Particles that do not pass through a 32 mesh sieve (particle size 500 to 1410μ)
m). To the classified detergent particles, citric acid monohydrate was added as a dissolution accelerator so as to have a concentration of 30%, and the mixture was uniformly mixed. When a tablet detergent is obtained, 25 g of this mixture is taken in a metal cylinder (die) having an inner diameter of 40 mm and pressurized at 40 kgf / cm ² for 1 minute through a metal piston (punch) to obtain a 40 mm diameter, 25 mm weight.
g of tablet detergent was obtained. When a briquette detergent was obtained, this mixture was supplied to a briquetting machine (CS-25, manufactured by Hosokawa Micron Corp.) to obtain a flat elliptical spherical briquette having a height of 4.5 mm and a long diameter of 6 mm. The operating conditions of the briquetting machine were as follows: roll speed 30 rpm, product capacity 170
kg / h and the roll clearance was 0.1 mm. Examples 7 to 14 Along with a pre-granulated product, a raw material having the same composition as that of the pre-granulated product was charged, and granulated by the production method A or B. 700 to 900 μm, bulk density 0.7 to
1.0 g / ml). Next, the detergent particles were subjected to JIS 12
The particles were classified using a mesh sieve and a JIS 32 mesh sieve to obtain particles (particle diameter: 500 to 1410 μm) that passed through a 12 mesh sieve and did not pass through a 32 mesh sieve. To the classified detergent particles, citric acid monohydrate was added as a dissolution accelerator so as to have a concentration of 30%, and mixed uniformly. afterwards,
Tablets or briquette detergents were obtained in the same manner as in Examples 1 to 6.

Comparative Examples 1-2 After spray-dried particles having the composition shown in Table 1 (excluding a nonionic surfactant and a part of water) were obtained by spray-drying, granulated materials previously granulated were added. Instead, granulation was carried out by granulation method A or B to obtain detergent particles (average particle diameter: 700 to 800 μm, bulk density: 0.8 to 0.9 g / ml). Then, the detergent particles are
The particles were classified using an IS 12 mesh sieve and a JIS 32 mesh sieve to obtain particles (particle diameter: 500 to 1410 μm) that passed through the 12 mesh sieve and did not pass through the 32 mesh sieve.
Citric acid 1 was added to the classified detergent particles as a dissolution promoter.
The hydrate was added to 30% and mixed uniformly.
Thereafter, a tablet detergent was obtained in the same manner as in Examples 1 to 6. Comparative Examples 3 to 4 After spray-dried particles having the composition shown in Table 1 (excluding a part of the nonionic surfactant and water) were obtained by spray-drying, the granulated material previously granulated was not added. Granulation was performed by granulation method A or B to obtain detergent particles. Then, without classifying the detergent particles, citric acid monohydrate was used as a dissolution promoter in an amount of 30%.
And mixed uniformly. Thereafter, a tablet detergent was obtained in the same manner as in Examples 1 to 6. Comparative Example 5 Detergent particles having the composition shown in Table 2 were obtained by the granulation method A without adding a granulated material which was previously granulated. Next, without classifying the detergent particles, citric acid monohydrate was added as a dissolution promoter to a concentration of 30% and mixed uniformly. afterwards,
A briquette detergent was obtained in the same manner as in Examples 6 and 12.

Evaluation of Manufacturability / Quality Granulation Time Reduction Rate (%) The granulation time reduction rate (%) was calculated according to the following equation 1. Formula 1: [(granulation time of pre-granulated granules)-(granulation time of detergent particles used for tablet or briquette detergent)] / (granulation time of pre-granulated granules) × 100 Evaluation of the characteristics was performed according to the following criteria. ：: 50% or more ○: 20% or more, less than 50% Δ: 5% or more, less than 20% ×: Less than 5% 12 # on (coarse particles) reduction rate (%) 12 # on (coarse particles) reduction rate ( %) Was calculated by the following equation 2. Formula 2: [(12 # on amount (%) at the time of granulation of pre-granulated granules]-(12 # on amount (%) at the time of granulation of detergent particles used for tablet or briquette detergent) ] / (12 # ON amount (%) at the time of granulation of granulated granules previously) x 1
The evaluation of the characteristics was performed according to the following criteria.
However, the 12 # pass amount (%) indicates the weight of the particles that do not pass through the JIS 12 mesh sieve (mesh size: 1410 μm). ◎: 30% or more ○: 15% or more, less than 30% Δ: 5% or more, less than 15% ×: less than 5%

32 # pass (fine particle) reduction rate (%) The 32 # pass (fine particle) reduction rate (%) was calculated by the following equation 3. Formula 3: [(32 # pass amount (%) at the time of granulation of a granulated product previously granulated)-(32 # pass amount (%) at the time of granulation of detergent particles used for tablet or briquette detergent) ] / (32 # pass amount (%) at the time of granulation of the granulated product granulated in advance) × 1
The evaluation of characteristics was performed according to the following criteria. However, the amount of 32 # pass (%) indicates the weight of particles passing through a JIS 32 mesh sieve (opening 500 μm). ◎: 30% or more ○: 15% or more, less than 30% Δ: 5% or more, less than 15% ×: less than 5%

Solubility test Tap water at a predetermined temperature was placed in a 3000 ml beaker, 25 g of a tablet or briquette detergent was charged, and the mixture was stirred for 10 minutes. Next, the detergent remaining after dissolution was taken out on a nylon cloth, dried at 105 ° C. for 2 hours, and a dissolution residue represented by the following formula was calculated and evaluated according to the following criteria. Dissolution residue (%) = {(dissolved residue at 105 ° C. for 2 hours, dried product (g) / 25 g)} × 100 ：: 0% ≦ dissolution residue <1% ○: 1% ≦ dissolution residue <5% △: 5 % ≦ dissolution residue <10% ×: 10% ≦ dissolution residue

[0040]

Table 3 Example 1 Example 2 Example 3 Example 4 Example 4 Pre-granulated granulated material A B C D Pre-granulated granulated material amount (%) 15 15 15 15 Granulation method A B A B Compressed form Tablet Tablet Tablet Tablet 12 # On reduction rate ◎ ◎ ◎ ◎ 32 # Pass reduction rate ◎ ◎ ◎ ◎ Granulation time reduction rate ◎ ◎ ◎ ◎ Tablet or briquette solubility ◎ ◎ ◎ ◎

[0041]

Table 4 (continued) Example 5 Example 6 Example 7 Example 8 Pre-granulated granules A EF F Pre-granulated granules Amount (%) 45 15 15 15 Granulation Method A A AB Compressed form Tablet Briquette Tablet Tablet 12 # On reduction rate ◎ ◎ ◎ ◎ 32 # Pass reduction rate ◎ ◎ ◎ ◎ Granulation time reduction rate ◎ ◎ ◎ ◎ Tablet or briquette solubility ◎ ◎ ◎ ◎ ◎

[0042]

Table 5 (continued) Example 9 Example 10 Example 11 Example 12 Example 12 Pre-granulated granulated material GHEG Pre-granulated granulated material amount (%) 15 15 0.5 15 Granulation Method A B A A Compressed form Tablet Tablet Tablet Briquette 12 # ON reduction rate ◎ ◎ ○ ◎ 32 # Pass reduction rate ◎ ◎ ○ ◎ Granulation time reduction rate ◎ ◎ ○ ◎ Tablet or briquette solubility ◎ ◎ ○ ◎

[0043]

Table 3 (Continued) Example 13 Example 14 Granulated Material I J Granulated Material Amount Granulated in Pre-Granulation (%) 15 15 Granulation Method A A Compressed Form Tablet 12 # On Reduction Rate ◎ ◎ 32 # Reduction rate of pass ◎ ◎ Reduction rate of granulation time ◎ ◎ Tablet or briquette solubility ◎ ◎

[0044]

Table 7 (Continued) Comparative Example 1 Comparative Example 2 Comparative Example 3 Pre-granulated granulated material---Pre-granulated granulated material amount (%)---Granulation method ABA compression Form Tablet Tablet Tablet 12 # On reduction rate × ¹⁾ × ²⁾ × ¹⁾ 32 # Pass reduction rate × ¹⁾ × ²⁾ × ¹⁾ Granulation time reduction rate × ¹⁾ × ²⁾ × ¹⁾ Tablet or briquette Solubility ◎ ◎ ×

[0045]

Table 8 (Continued) Comparative Example 4 Comparative Example 5 Pre-granulated granules--Pre-granulated granules (%)--Granulation method B A compressed form Tablet Briquette 12 # ON Reduction rate × ²⁾ × ³⁾ 32 # pass reduction rate × ²⁾ × ³⁾ Granulation time reduction rate × ²⁾ × ³⁾ Tablet or briquette solubility × × 1) Formula 1 (Granulation time of granulated material), in equation 2 (at the time of granulation of granulated material
The value at the time of granulation of the granulated material A that has been granulated in advance is used as the (12 # on amount) and the value at the time of granulation of the granulated material A that has been granulated in advance is used for (the amount of 32 # pass at the time of granulating the granulated material that has been granulated in advance). 2) In the equation 1 (granulation time of the pre-granulated material), in the equation 2 (granulation of the pre-granulated product)
The value at the time of granulation of the granulated material B that has been granulated beforehand is used for (12 # on amount) and the value of the granulated material B that has been granulated beforehand is used in Expression 3 (the amount of 32 # pass at the time of granulation of the granulated material previously granulated). 3) In the equation (1) (granulation time of the pre-granulated material) and in the equation (2)
The value at the time of granulation of the granulated material C that has been granulated in advance is used as the (12 # on amount) and the value of the granulated material C that has been granulated in advance is used as the (32 # pass amount at the time of granulation of the granulated material).

[0046]

According to the present invention, a compression molded detergent having excellent disintegration and dispersion characteristics can be produced in a short time and with high productivity.

 ────────────────────────────────────────────────── ─── Continuing on the front page (72) Inventor Takashi Inozuka 1-3-7 Honjo, Sumida-ku, Tokyo F-term in Lion Corporation (reference) 4H003 AB03 AB15 AB19 AB44 AC01 BA10 BA17 CA08 EA12 EA15 EA16 EA28 FA32

Claims (1)

[Claims] 1. A method for producing a compression-molded detergent, comprising: (1) a detergent composition having the same composition as the pre-granulated granules in the presence of the pre-granulated granules. Stir and granulate things
A step of producing detergent particles having an average particle size of 300 to 1500 μm and a bulk density of 0.6 to 1.2 g / ml; (2) a step of classifying the resulting detergent particles; and (3) a compression molding of the resulting detergent particles. A method comprising the steps of: