JP2002180098A - Tablet type detergent and method for producing the same - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a tablet type detergent excellent in detergency and solubility and easy to use. SOLUTION: This tablet type detergent comprises an activator particle (I) containing (a) an anionic surfactant, (b) a nonionic surfactant, (c) a water-soluble inorganic salt and (d) a water-insoluble inorganic compound and 3-20 wt.% of a disintegrator particle (II) and has the following ratios of (a) to (d): (a)+(b) is 15-50 wt.%; (c)+(d) is 40-70 wt.%; (a)/(b) is (6/1) to (50/1) (weight ratio); (c)/(d) is (1/3) to (3/1) (weight ratio); and [(a)+(b)+(c)]/(d) is (10/1) to (1/1) (weight ratio).

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to a tablet detergent and a method for producing the same. The tablet detergent of the present invention is particularly suitable for clothing.

[0002]

2. Description of the Related Art At present, powdery and granular forms of laundry detergent are mainly used. However, these detergents need to be weighed at the time of use, and furthermore, powder may be scattered, which has a drawback of causing discomfort to the user.

Recently, attempts have been made to develop tablet detergents to solve these problems. However, while tablet detergents are simple and easy to use, it is extremely difficult to satisfy the seemingly contradictory factors of high tablet strength and rapid solubility in water to maintain their shape in the manufacturing and transport processes. Technical challenges. Furthermore, when tableted, it is generally impossible to develop exactly the same solubility as a general granular or powdered detergent. In other words, if the washing time is short, the tableted detergent may result in inferior washing performance due to the time constraint required for dissolution. For this reason, detergents in the form of tablets are required to exhibit sufficient washing performance in a shorter time in addition to the above-mentioned solubility and strength. Therefore, it is a necessary condition that the detergency exceeds the conventional granular or powdered detergent.

[0004]

SUMMARY OF THE INVENTION An object of the present invention is to provide a tablet-type detergent which is excellent in detergency and solubility and is easy to use, and a method for producing the same.

[0005]

The present invention relates to an activator containing (a) an anionic surfactant, (b) a nonionic surfactant, (c) a water-soluble inorganic salt and (d) a water-insoluble inorganic substance. A tablet detergent containing particles (I) and 3 to 20% by weight of disintegrant particles (II), wherein the ratio of (a) to (d) is:
(A) + (b) = 15-50% by weight, (c) + (d) =
40 to 70% by weight, (a) / (b) = 6/1 to 50/1
(Weight ratio), (c) / (d) = 1/3 to 3/1 (weight ratio), [(a) + (b) + (c)] / (d) = 10/1
１／1/1 (weight ratio).

Further, the present invention provides (a) an anionic surfactant [hereinafter, (a)] having the following steps A, B, C and D:
Component)], (b) a nonionic surfactant [hereinafter, referred to as
(B) component), (c) water-soluble inorganic salt [hereinafter, referred to as
(Referred to as component (c)) and (d) a water-insoluble inorganic substance [hereinafter, referred to as
(Referred to as "d) component") and a tablet detergent containing 3 to 20% by weight of disintegrant particles (II), wherein the ratio of (a) to (d) is as follows: (A) + (b) =
15 to 50% by weight, (c) + (d) = 40 to 70% by weight, (a) / (b) = 6/1 to 50/1 (weight ratio),
(C) / (d) = 1/3 to 3/1 (weight ratio), [(a)
+ (B) + (c)] / (d) = 10/1 to 1/1 (weight ratio). Step A: Step of producing activator particles (I) containing component (a), component (b), component (c) and component (d) and having an average particle size of 300 to 1500 μm Step B: average particle size of 200 to Step of preparing 1500 μm disintegrant particles (II) Step C: mixing activator particles (I) and disintegrant particles (II) Step D: mixing the mixture obtained in Step C at 20 to 50 ° C.
At a temperature of 20 to 100 kgf / cm ² (1.96 to
Forming with a molding pressure of 9.81 MPa)

[0007]

BEST MODE FOR CARRYING OUT THE INVENTION In the activator particles (I) of the tablet detergent of the present invention, the total amount of the components (a) and (b) is as follows:
In terms of cleaning performance and solubility, 15 to 50 in tablet detergents
%, Preferably 25 to 48% by weight, and 30 to 4% by weight.
5% by weight is more preferred.

The weight ratio of component (a) / component (b) is from 6/1 to 50/1 in terms of washing performance and tablet formability.
6.5 / 1 to 25/1 are preferred, and 7/1 to 15/1 are more preferred.

[0009] The total amount of the components (c) and (d) is from 40 to 40 in the tablet type detergent in terms of washing performance and solubility.
70% by weight, preferably 45-60% by weight,
~ 55 wt% is more preferred.

The weight ratio of component (c) / component (d) is from 1/3 to 3/1 in terms of solubility and tablet formability.
3 to 3/2 are preferable, and 1/1 to 3/2 are more preferable.

[(A) component + (b) component + (c)
Component / (d) is 10/10 in terms of solubility.
1-1 / 1, preferably 5 / 1-3 / 2, and 3/1
２2/1 is more preferable.

The amount of the activator particles (I) is from 80 to 97% by weight, more preferably from 8 to 97% by weight in the tablet type detergent in view of the washing performance and solubility.
It is preferably from 5 to 95% by weight, especially from 85 to 93% by weight.

The amount of the disintegrant particles (II) is 3 to 20% by weight in the tablet detergent in terms of washing performance and solubility,
-15% by weight is preferred, and 7-15% by weight is more preferred.

[0014] By mixing the active agent particles (I) and the disintegrant particles (II) and compression molding into tablets, sufficient strength and solubility can be obtained.

The active agent particles (I) preferably have an average particle size of 300 to 1500 μm from the viewpoint of solubility and tablet formability.
400-1200 μm is more preferable, and 500-100
0 μm is more preferable, and 600 to 900 μm is particularly preferable. Further, the ratio of particles having a particle size of less than 125 μm is preferably 15% by weight or less, more preferably 10% by weight or less, and even more preferably 5% by weight or less.

The disintegrant particles (II) preferably have an average particle size of 200 to 1500 μm in view of solubility and tablet formability.
200 to 1000 μm is more preferable, and 250 to 750
μm is more preferred.

The water content of the tablet detergent of the present invention is
In terms of tablet formability and storage stability, the content is preferably 10% by weight or less, more preferably 8% by weight or less, further preferably 6% by weight or less, and particularly preferably 4% by weight or less. In addition, the water content is measured by a method defined by JIS K 3362: 1998 heating loss method.

<Component (a)> The tablet detergent of the present invention comprises:
(A) It contains an anionic surfactant. Examples of the anionic surfactant include an alkylbenzene sulfonate, an alkyl or alkenyl sulfate, an alkyl or alkenyl ether sulfate, an α-olefin sulfonate, an α-sulfofatty acid salt or an ester thereof, an alkyl or alkenyl ether carboxylate, Amino acid type surfactants, N-acyl amino acid type surfactants and the like are exemplified. Especially 1 carbon
0-14 straight-chain alkyl benzene sulfonates, alkyl sulfates having 10 to 18 carbon atoms or alkyl ether sulfates, and examples of the counter ion include alkali metals such as sodium and potassium, and amines such as monoethanolamine and diethanolamine. preferable. Alkali metals such as sodium and potassium are preferred in view of tablet formability. From the viewpoint of dissolution rate, it is also preferable to use sodium ion and potassium ion in combination, and potassium ion in all counter ions is 5%.
% By weight or more, preferably 20% by weight or more, and particularly preferably 40% by weight or more.

Further, a fatty acid salt can be used in combination to obtain a defoaming effect. Preferred fatty acids have 12 carbon atoms.
~ 18.

<Component (b)> The tablet detergent of the present invention comprises:
(B) It contains a nonionic surfactant. As the nonionic surfactant, polyoxyethylene alkyl or alkenyl ether, polyoxyethylene alkyl or alkenyl phenyl ether, polyoxyethylene polyoxypropylene alkyl or alkenyl ether, polyoxyethylene polyoxypropylene glycol, polyoxyethylene alkylamine, Higher fatty acid alkanolamides, alkylglucosides, alkylglucoseamides, alkylamine oxides and the like can be mentioned. Among them, those having high hydrophilicity and those having low ability to form liquid crystal or not generating liquid crystal when mixed with water are preferable, and polyoxyalkylene alkyl or alkenyl ether is particularly preferable. Ethylene of an alcohol having preferably 10 to 18, preferably 12 to 14 carbon atoms and an average addition mole number of 5 to 30, preferably 7 to 30, more preferably 9 to 30, and more preferably 11 to 30. Oxide (hereinafter referred to as EO) adducts, and other 8 carbon atoms
EO adducts and propylene oxide (hereinafter, referred to as PO) adducts of alcohols Nos. To 18 are preferable. As the order of addition, a sequence obtained by adding PO after adding EO, a sequence obtained by adding EO after adding PO, or a sequence obtained by randomly adding EO and PO can be used. Is a general formula in which EO is added, PO is added in a block, and EO is further added in a block: R—O— (EO) _X — (PO) _Y — (EO) _Z —H wherein R is A hydrocarbon group, preferably an alkyl group or an alkenyl group, EO represents an oxyethylene group, PO represents an oxypropylene group, and X, Y and Z each represent an average number of moles. And the most preferred relationship among the average number of moles added is X> 0, Z> 0,
X + Y + Z = 6 to 14, X + Z = 5 to 12, and Y = 1 to 4.

The tablet detergent of the present invention may contain a cationic surfactant or an amphoteric surfactant as a surfactant other than the components (a) and (b). Examples of the cationic surfactant include a quaternary ammonium salt such as an alkyltrimethylammonium salt. Examples of the amphoteric surfactant include a carbobetaine type and a sulfobetaine type.

<Component (c)> The tablet detergent of the present invention comprises:
(C) It contains a water-soluble inorganic salt. The term "water-soluble" means that the solubility in 100 g of water at 25 ° C is 0.5 g or more. Examples of the water-soluble inorganic salt include water-soluble inorganic salts having a carbonate group, a sulfate group, a hydrogen carbonate group, a sulfite group, a hydrogen sulfate group, a phosphate group and the like (for example, alkali metal salts, ammonium salts,
Or amine salt). Also, halides such as chlorides, bromides, iodides, fluorides and the like of alkali metals (for example, sodium or potassium) and alkaline earth metal salts (for example, calcium or magnesium) can be mentioned. Further, double salts containing these (for example, burkeite, sodium sesquicarbonate, etc.) are also included.

Of these, carbonates, sulfates and sulfites are preferred. Carbonates are preferred as an alkaline agent exhibiting a suitable pH buffer region in the washing liquor, and salts having a high degree of dissociation, such as sulfates and sulfites, increase the ionic strength of the washing liquor and work well for sebum dirt washing and the like. . Sulfite also has the effect of reducing hypochlorite ions contained in tap water and preventing oxidative deterioration of detergent components such as enzymes and fragrances due to hypochlorite ions. The water-soluble inorganic salt may be composed of a single component, or a plurality of components such as a carbonate and a sulfate may be used in combination.

<Component (d)> The tablet detergent of the present invention comprises:
(D) It contains a water-insoluble inorganic substance. Water insoluble is 25
It has a solubility in water of 100 ° C. of less than 0.5 g. As the water-insoluble inorganic substance, a crystalline aluminosilicate, an amorphous aluminosilicate, silicon dioxide, a hydrated silicate compound, a perlite, a clay compound such as bentonite, or the like can be used, and for supporting a liquid surfactant composition. Crystalline aluminosilicates and amorphous aluminosilicates are preferred because of their contribution and the reason that they do not promote the generation of undissolved residues.
The average particle size of the aluminosilicate is 0.1 to 10 μm.
Is preferable, and 0.5 to 5 μm is more preferable.

Preferred as the crystalline aluminosilicate is A-type zeolite, which is also preferable in terms of sequestering ability and economy. Other examples include a P-type and an X-type. Further, a hybrid zeolite described in WO9842622 is also mentioned as a suitable crystalline aluminosilicate.

As the amorphous aluminosilicate, for example, JP-A-62-191417, page 2, lower right column, line 19 to page 5, upper left column, line 17; Amorphous aluminosilicates described on page 2, lower right column, line 20 to page 5, lower left column, line 11, and JP-A-9-132794
No. 17, line 46 to column 18, line 38;
No. 10526, column 3, line 3 to column 5, line 9, JP-A-6-227811, column 2, line 15 to column 5, second
And the amorphous aluminosilicates described in JP-A-8-119622, column 2, line 18 to column 3, line 47. In particular, the oil absorbing carrier is disclosed in
No. 179899, column 12, line 12 to column 13, first
Lines, column 17, line 34 to column 19, line 17 are preferred. The water-insoluble inorganic substance may be composed of a single component or a plurality of components.

<Other Components> The tablet detergent of the present invention can use water-soluble organic acid salts having a low molecular weight in terms of solubility. For example, carboxylate salts such as citrate and fumarate can be used. Is mentioned. Further, from the viewpoint of detergency, methyliminodiacetic acid, iminodisuccinate, ethylenediaminedisuccinate, taurine diacetate, hydroxyethyliminodiacetate, β-alanine diacetate, hydroxyiminodisuccinate, methylglycine diacetate Salt, glutamic acid diacetate, asparagine diacetate, serine diacetate and the like are preferred.

The tablet detergent of the present invention comprises a dispersant or a color transfer inhibitor such as carboxymethyl cellulose, polyethylene glycol, polyvinylpyrrolidone and polyvinyl alcohol, a compound described in JP-A-6-316700, and a bleaching activity such as tetraacetylethylenediamine. An agent such as an agent such as protease, cellulase, amylase, or lipase, a biphenyl-type or stilbene-type fluorescent dye, an antifoaming agent, an antioxidant, a bluing agent, or a fragrance can be added. still,
Separately granulated particles such as enzymes, bleach activators, defoamers, etc. may be after blended.

<Activator Particles (I)> The activator particles (I) used in the present invention can be obtained by the following method. After kneading and kneading the raw material powder and binder component,
The extrusion granulation method of extruding and granulating, or kneading and kneading, after kneading and kneading, crushing and granulating the obtained solid detergent
Crushing granulation method, stirring granulation method in which a binder component is added to raw material powder and agitated with stirring blades to granulate, or rolling granulation method in which raw material powder is tumbled while spraying binder component to granulate And the like. As the raw material powder, a powdered surfactant or a detergent builder can be used in combination, or, if necessary, a slurry is prepared by adding water to part or all of the detergent components in advance, and spraying is performed according to a conventional method. Dry and dried powder may be used. The activator particles obtained by these methods are passed through a sieve after granulation, if necessary, to adjust the particle size distribution.

From the viewpoint of solubility, a particularly preferable production method is to spray-dry a slurry containing (c) a water-soluble inorganic salt and (d) a water-insoluble inorganic substance, and to obtain (a) There is a method in which an ionic surfactant and (b) a nonionic surfactant are supported, and the surface is coated with (c) a water-soluble inorganic salt and (d) a water-insoluble inorganic substance as necessary. At this time, it is more preferable that the operation is performed so that the particles obtained by spray drying are not broken as much as possible.

<Disintegrant particles (II)> The tablet detergent of the present invention contains disintegrant particles (II). Among them, particles containing (II ₁ ) a water-insoluble substance (preferably 70% by weight or more, more preferably 80% by weight or more) and (II ₂ ) a water-soluble substance (preferably 70% by weight or more, more preferably 80% by weight) It is preferable to contain disintegrant particles containing the above-mentioned particles in view of solubility and detergency. In particular (II ₁₎ content of the particles containing particles and (II ₂₎ water-soluble substance includes a water-insoluble substance, in the detergent tablet, the particles (II ₁₎ + particle (I
I ₂ ) = 5 to 15% by weight is preferred. In addition, in terms of solubility and detergency, the particles (II ₁ ) /
The weight ratio of the particles (II ₂ ) is preferably 5/1 to 1/2, and
/ 1 to 2/3 are more preferable, and 3/1 to 1/1 are more preferable.

Examples of the water-insoluble substance include one or more selected from cellulose, starch, polyvinylpyrrolidone and polyvinyl alcohol. Specifically, powdered cellulose, crystalline cellulose, low etherified carboxymethyl cellulose, cross-linked carboxymethyl cellulose, carboxymethyl cellulose calcium, cellulose derivatives such as hydroxypropyl cellulose, starch such as corn starch, starch derivatives such as hydroxypropyl starch, cross-linked Polyvinylpyrrolidone, polyvinyl alcohol having a low degree of etherification, and the like can be mentioned, and those having swellability are preferable.

The water-insoluble substance is extruded by granulation, kneading,
The particles (II ₁ ) are formed by using a granulation method such as a crushing granulation method, a stirring granulation method, a tumbling granulation method, and a compression granulation method. At the time of granulation, water, a liquid surfactant, a surfactant aqueous solution, or a polymer aqueous solution may be added as a binder to promote granulation. After granulation, post-treatments such as drying, pulverization, sizing, and sieving are performed as necessary.

Examples of the water-soluble substance include inorganic peroxides and solid acids, with inorganic peroxides being preferred. Examples of the inorganic peroxide include percarbonate, perborate, perphosphate, and persulfate. Of these, sodium percarbonate and sodium perborate are preferable. From the viewpoint of storage stability, it is preferable to form particles (II ₂ ) by coating. As the coating agent, boric acid and / or an alkali metal silicate are preferred. Examples of boric acid include orthoboric acid, metaboric acid, and tetraboric acid. Examples of the alkali metal silicate include sodium metasilicate, sodium orthosilicate, sodium salts of water glass Nos. 1, 2 and 3, potassium metasilicate, potassium orthosilicate and the like. Among them, water glass Nos. 1, 2, and 3 are liquid, and are preferable from the viewpoint of convenience in use. In addition to the above-mentioned coating agent, a conventionally known stabilizer such as a chelating agent may be used in combination with the coating agent.

<Tablet-type detergent> The tablet-type detergent of the present invention is formed after mixing the activator particles (I) and the disintegrant particles (II) obtained in Step A and Step B (Step C), respectively (Step C). It is obtained by step D). In the step C, in addition to the activator particles (I) and the disintegrant particles (II), other components can be mixed as required. In the tablet detergent of the present invention, various additives for improving the performance and function may be present in the activator particles by uniformly mixing and granulating with the surfactant and the builder. Alternatively, it may be added independently from the activator particles from the viewpoint of storage stability. In step D, 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 upper punch and the lower punch in the mortar via the compression device, a tablet having a shape formed by the mortar and the punch is formed. As such a tableting machine, a generally known single-shot tableting machine for tableting one tablet at a time can be used, or a rotary with high production efficiency equipped with a plurality of dies along a rotating disk. A tableting machine can also be used. In addition, it is also possible to make the tablet easier to use by dividing by putting a score line.

In the step D, the mixture is mixed with 20
At a temperature of ５０50 ° C., preferably 20-40 ° C.
00 kgf / cm ² (1.96 to 9.81 MPa), preferably 20 to 80 kgf / cm ² (1.96 to 7.8 MPa)
4 MPa), more preferably 20-60 kgf / cm ²
(1.96 to 5.88 MPa).

The compressed tablet detergent is commercialized by surrounding it with a suitable material, preferably a water-soluble material. For example, the packaging or surface is covered with one or more pieces.
As a packaging material, an aluminum laminate film, a PET two-layer film, a PP two-layer film, and the like are preferable in terms of moisture resistance, but are preferably packaged in a water-soluble material in terms of convenience.

The tablet-type detergent of the present invention is preferably in a form of being packaged separately with a water-soluble material from the viewpoint of convenience. It is preferable in terms of convenience to divide the amount of detergent used for one washing.

The water-soluble material is defined as a columnar 1 L beaker having an inner diameter of 105 mm, into which 1 L of distilled water at 40 ° C. is added.
5 mm, a stirrer with a maximum diameter of 7.5 mm (manufactured by Kagaku Kyoeisha,
Stirring is performed at 550 rpm using a model SA-35 or the like as a preferred example), and the material (3 cm × 3 cm, 4 sheets) is charged. After stirring is continued for 8 minutes, the mixture is passed through a sieve having an aperture of 125 μm. Is less than 5% by weight of the input material. Preferably, when the same operation is performed using distilled water at 10 ° C., the residue is 5% by weight or less;
It is more preferably at most 2% by weight.

Examples of the water-soluble material include polyvinyl alcohol, polyvinylpyrrolidone, pullulan, polyacrylamide, polyacrylic acid or a salt thereof, polymethacrylic acid or a salt thereof, polyitaconic acid or a salt thereof, polyethylene oxide, polyvinyl methylene ether and xanthan gum. , Guar gum, collagen, carboxymethylcellulose, hydroxyethylcellulose, and hydroxypropylcellulose.

In particular, polyvinyl alcohol is preferable from the viewpoint of solubility in cold water, and partially saponified polyvinyl alcohol having a degree of saponification of less than 96 mol%, or a degree of saponification of 96 mol% or more, preferably from the point of deterioration resistance. Modified polyvinyl alcohol of 98 mol% or more is more preferable.

Examples of the modifying group include an anionic group, a cationic group and a nonionic group, and an anionic group and a nonionic group are more preferred.

From the viewpoint of productivity, anionic modification is preferred. Examples of the monomer having an anionic group include unsaturated carboxylic acids such as acrylic acid, crotonic acid, maleic acid, fumaric acid, and itaconic acid, unsaturated sulfonic acids, and the like. These esters or anhydrides are mentioned, and maleic acid, itaconic acid and 2-acrylamido-methylpropanesulfonic acid are particularly preferable.

From the viewpoint of flexibility at low temperatures, nonionic modification is more preferable, and EO modification is more preferable.

The modification ratio is preferably from 0.1 to 20 mol%, preferably from 0.5 to 15 mol%, based on the total amount of monomer units in all molecules.
More preferably, the molar percentage is more preferably 1 to 10 mol%. 0.1 mol% or more is preferable in view of solubility in water,
The amount is preferably 20 mol% or less from the viewpoint of preventing the formation of a gel-like substance upon introduction into water to prevent the solubility from being lowered.

From the viewpoint of solubility, the weight average molecular weight of the modified polyvinyl alcohol is preferably 5000 to 1,000,000, as measured by gel permeation chromatography using polyethylene glycol as a standard.
10,000 is more preferable.

As other water-soluble films, JP-A-10-72599, column 5, line 47 to column 6, line 31
The ones described in the line are mentioned.

The thickness of the water-soluble material of the present invention can be arbitrarily set according to the purpose of use, but is preferably from 10 to 100 μm, and more preferably from 15 to 50 μm, from the viewpoint of mechanical strength and rapid water solubility.
m is more preferred.

In addition, processability, feel when touched, solubility,
In order to improve the prevention of blocking during storage of the material, the prevention of blocking during storage of the tablet-type detergent, and the like, it is preferable that the water-soluble material is provided with lattice-like or turtle-like irregularities by embossing or the like.

By being packaged separately in a water-soluble material,
Since the aroma imparted to the tablet detergent no longer smells, it is preferable to include a compounded flavor in the water-soluble material in masking the specific odor of the water-soluble material. The fragrance contained in the water-soluble material is more preferably 0.05 to 5% by weight in the water-soluble material, from the viewpoints of masking and physical properties of the water-soluble material.
5 to 3% by weight is more preferred.

It is preferable to add a surfactant to the water-soluble material from the viewpoints of stabilizing and releasing the fragrance. Examples of the surfactant include a cationic surfactant, an anionic surfactant, a nonionic surfactant, and the like, and a nonionic surfactant is more preferable. Surfactant in a water-soluble material,
It is preferably contained in an amount of 0.01 to 5% by weight, more preferably 0.05 to 3% by weight, and still more preferably 0.1 to 5% by weight.
1 to 2% by weight. It is 0.01% by weight or more in terms of the releasability, and 5% by weight or less in terms of the strength of the water-soluble material.

The water-soluble material may contain a plasticizer in order to improve processability, flexibility, hydrophilicity when dissolved in water, prevention of blocking during storage of the material, prevention of blocking during storage, and the like.
The water-soluble material preferably contains 1 to 50% by weight, more preferably 2 to 40% by weight. Examples of the plasticizer include ethylene glycol, propylene glycol, glycerin, diglycerin, polyglycerin, low molecular weight polyethylene glycol (molecular weight: 600 or less),
Polyhydric alcohol plasticizers such as trimethylolpropane are preferred, and glycerin is more preferred. Further, a colorant, a release agent, and the like can be blended or applied within a range that does not impair the purpose of the present invention.

In order to increase the strength of the water-soluble material and improve the water-solubility, it has an average particle diameter of 0.1 to 10 μm, more preferably 0.1 to 5 μm, and still more preferably 0.2 to 3 μm. Soluble powder to water-soluble material 0.05
The content is preferably 5 to 5% by weight, more preferably 0.1 to 4% by weight, and still more preferably 1 to 3% by weight. This makes it possible to reduce the amount of the water-soluble material used.

Examples of the water-insoluble or hardly water-soluble powder include titanium dioxide, calcium carbonate, talc, insoluble silica, clay mineral, aluminosilicate, aluminum hydroxide, barium sulfate, silicate, pulp, cellulose and the like.
These can be used alone or in combination of two or more as necessary. Of these, titanium dioxide, calcium carbonate, talc, insoluble silica, and clay minerals are preferred in terms of storage stability and good appearance, and titanium dioxide and combination use with titanium dioxide are more preferred.

As a method for producing a water-soluble material, for example,
If necessary, an aqueous solution of the material resin can be mixed with a surfactant, a plasticizer, a fragrance, and the like, cast on a drum or an endless belt, and dried to form a water-soluble film.

[0056]

[Example] [Average particle diameter] After oscillating for 5 minutes using a standard sieve according to JIS Z 8801, the average particle diameter was determined from the weight fraction based on the sieve size.

[Water content] JIS K 3362: 199
8 Measured according to the method specified by the heating weight loss method.

[Detergency] (Preparation of stained cloth for evaluation) Bilirubin (C ₃₃ H ₃₆ N ₄ O ₆ ,
(MERK) 0.061 g in chloroform 100 ml
Dissolve in 0.4 ml of this solution is dropped on a 10 cm × 10 cm cotton cloth # 2003 cloth per sheet and air-dried to obtain a stained cloth for evaluation.

(Evaluation method) 5 sheets of cloth for evaluation and 2 kg of clothing (50% by weight of cotton underwear, 50% by weight of polyester / cotton blend, polyester / cotton Y-shirt 50) were put on a fully automatic washing machine "Aizuma-go NA-F42Y1" manufactured by Matsushita Electric Industrial Co., Ltd. % By weight), and then a tablet detergent (25 g) was charged.
Of tap water and washed for 5 minutes in a standard water flow. Next, the evaluation cloth was rinsed with tap water for 5 minutes.

The reflectivity at 460 nm of the original stained cloth for evaluation and the stained cloth before and after washing was measured with an automatic colorimeter (manufactured by Shimadzu Corporation), and the washing rate (%) was determined by the following equation.
The measured average value of the sheets was determined and evaluated according to the evaluation criteria.

[0061]

(Equation 1)

(Evaluation Criteria) A: Cleaning rate is 60% or more. A: Cleaning rate is 55% or more and less than 60%. X: Cleaning rate is less than 55%.

[Dispersibility] The pulsator 6 of the fully automatic washing machine "Aizuma NA-F42Y1" manufactured by Matsushita Electric Industrial Co., Ltd.
A tablet detergent (25 g) is placed on a portion near the outer periphery of one of the divided fan-shaped depressions, and 1.5 kg of clothing (50% by weight of cotton underwear, 50% by weight of polyester / cotton blend Y-shirt) is put into a washing tub, 10L / m so that water does not directly hit the detergent
22 L of tap water at 5 ° C. was injected at a flow rate of “in”, and allowed to stand still after the injection.

After 10 minutes from the start of water injection, stirring was started with a weak water flow (hand washing mode), and after stirring for 3 minutes, drainage was performed.
The state of the detergent remaining in the clothes and the washing tub was visually determined according to the following evaluation criteria.

The “aggregates” described in the following evaluation criteria
"Lump" refers to a lump having a diameter of 3 mm or more in which the detergent is aggregated.

(Evaluation Criteria) A: There is no aggregate of detergent. ：: Almost no aggregates of the detergent. ×: A large amount of detergent aggregates remained.

[Solubility] After putting 2 kg of clothing (50% by weight of cotton underwear, 50% by weight of polyester / cotton blended Y-shirt) into a fully automatic washing machine “Aizumago NA-F42Y1” manufactured by Matsushita Electric Industrial Co., Ltd. , A tablet detergent (25 g) was charged, tap water at 5 ° C. was set at a medium water level (40 L), and washing was performed for 5 minutes in a standard water flow.

The washing drainage discharged after the washing process
After filtration through a 00 μm sieve, the amount of detergent remaining on the sieve was visually determined based on the following evaluation criteria.

(Evaluation Criteria) A: No detergent remains. ：: Detergent hardly remains. ×: A large amount of detergent remains.

Examples 1 to 4 and Comparative Examples 1 to 4 Based on the weight in the tablet detergent of Table 1, 7% by weight of the zeolite of the activator particles (I), carbonate, and components other than the fragrance, A slurry having a solid content of 50% by weight was prepared and spray-dried to obtain a spray-dried composition. The carbonate was added to the ribbon mixer and mixed. The obtained mixture was extruded into a cylindrical shape having a diameter of 10 mm by a pre-extrusion type twin-screw extrusion granulator (pelleter double: manufactured by Fuji Paudal Co., Ltd.) and compacted. The obtained pellets were pulverized and granulated with a flash mill (manufactured by Fuji Paudal Co., Ltd.) together with 5% by weight of zeolite to perform surface coating. After removing coarse substances from the granulated product, the granulated product was transferred to a V blender, and the remaining zeolite, flavor, and the like were mixed to obtain activator particles (I).

Next, the obtained activator particles (I), disintegrant particles (II) and other particles were mixed, and 12.5 g
Into a tableting mold having a diameter of 35 mm, 25 ° C., 40 kg
A tablet detergent was molded by pressing at f / cm ² (3.92 MPa) for 1 minute. Table 1 shows the results of the above-mentioned evaluation performed on the obtained tablet detergent.

[0072]

[Table 1]

AOS-K: potassium α-olefin sulfonate having 14 to 18 carbon atoms. AOS-Na: sodium α-olefin sulfonate having 14 to 18 carbon atoms. LAS-K: linear chain having 10 to 14 carbon atoms. LAS-Na: linear alkylbenzene sulfonate having 10 to 14 carbon atoms α-SFE-Na: α-sulfofatty acid methyl ester sodium having 14 to 18 carbon atoms Fatty acid Na: 14 to 18 carbon atoms -Nonionic surfactant 1: secondary alcohol having 12 to 14 carbon atoms and an average of 12 mol of EO added-Nonionic surfactant 2: linear first chain having 10 to 14 carbon atoms
5 mol of EO on average, 2 mol of PO on average,
EO added in the order of 3 moles on average.-Zeolite: 4A-type zeolite (average particle size: 3 µm)-Cellulose-containing particles [disintegrant particles (II ₁ )]: Mix 60% by weight of powdered cellulose and 40% by weight of water Then, it was extruded from a screen having an opening diameter of 1.4 mm to obtain an extruded granulated product. Next, after drying in a dryer (80 ° C.)
%), Ground with a ball mill ・ Na-percarbonate-containing particles [disintegrant particles (II ₂ )]: Granules containing 84% by weight of sodium percarbonate surface-coated with water glass No. 1 sodium salt AA / MA copolymer: sodium salt of acrylic acid / maleic acid copolymer (neutralized by 70 mol%), monomer ratio: acrylic acid / maleic acid = 3/7 (molar ratio), weight average molecular weight: 50,000 AOBS particles: alkanoyl (C12) Granulated product of 70% by weight of sodium oxybenzenesulfonate. Enzyme particles: Cellulase K (JP-A-63-264699)
Publication No.), Lipolase 100T (manufactured by Novo):
• Fluorescent dye: Tinopearl CBS-X and Tinopearl AMS
-A mixture of GX (manufactured by Ciba Specialty Chemicals) at a weight ratio of 1/1.

Examples 5 to 8 Combinations of the tablet detergent and the water-soluble material shown in Table 2
The same evaluation as in Example 1 was performed on the tablet detergent obtained by separately packing the tablet detergent. Table 2 shows the results. The water-soluble materials 1 to 5 are as follows.

(Water-soluble material 1) 100 parts by weight of maleic acid-modified (modification ratio: 2 mol%) polyvinyl alcohol (99 mol% of saponification degree), 550 parts by weight of water, 10 parts by weight of glycerin, Emulgen 120 (nonionic surfactant) 0.2 parts by weight), 0.5 parts by weight of a compounded flavor, and 2 parts by weight of titanium dioxide (average particle size: 0.3 μm) are dispersed and defoamed, and then cast on a 120 ° C. drum. 14
Dry with hot air at 0 ° C (drying residence time: 2 minutes), water content 7
% By weight, and a long film having a thickness of 30 μm was obtained.

(Water-soluble material 2) The water-soluble material 1 was embossed with 40 mesh silk (roller 120 ° C., linear pressure 30
kg / cm).

(Water-soluble material 3) A polyvinyl alcohol fiber having a degree of saponification of 88 mol% and a degree of polymerization of 1700 was crimped and cut to obtain a 2 denier × 51 mm stable, which was then spread to obtain a basis weight of 20 g / m 2. ² webs. The obtained web is superimposed on the water-soluble material 1, and the compression area ratio is 25.
% Of the embossed roller with a deformed square pattern with a side of 2 mm
The temperature was set to 20 ° C., and thermocompression bonding was performed at a linear pressure of 30 kg / cm to form a composite. The grammage was 46 g / m ² .

(Water-soluble material 4) While unwinding the same film as the water-soluble material 1, a gravure coating machine (gravure roll 2)
00 mesh, manufactured by Hirano Lecseed, cellulose powder (W-400G, manufactured by Nippon Paper, average fiber length 27 μm)
m) A dispersion of 50 g of ethyl cellulose (K-200, Hercules), 890 g of isopropyl alcohol, and 50 g of water was applied while stirring. Continue 1
Hot air drying was performed at 10 ° C. for 20 seconds. This composited the cellulose powder with the water-soluble material. 2.5g /
m ² .

(Water-soluble material 5) After polymerization of vinyl acetate and polyoxyethylene (EO average addition mole number: 7) monoallyl ether, a saponification reaction was carried out to obtain polyoxyethylene (EO average addition mole number: 7) monoallyl ether. An ether / vinyl acetate copolymer was obtained. This copolymer had 0.5 mol% of unsaponified vinyl acetate, 4 mol% of polyoxyethylene (EO average addition mole number: 7) monoallyl ether, and a weight average molecular weight of about 20,000.

100 parts by weight of the copolymer, 2 parts by weight of titanium dioxide (average particle size: 0.3 μm), 550 parts by weight of water, 10 parts by weight of glycerin, Emulgen 120 (nonionic surfactant, manufactured by Kao) 0.2 After dispersing and defoaming 0.5 part by weight of the prepared flavor, the mixture was dried on a 140 ° C. hot air while drying on a drum at 120 ° C. (dry residence time: 2 minutes) to give a water content of 6% by weight. A long film having a thickness of 30 μm was obtained. Next, a 40 mesh silk embossing (roller 120 ° C., linear pressure 30 kg / cm) was performed to obtain a water-soluble material.

[0081]

[Table 2]

Examples 9 to 12 Based on the weight in the tablet detergent of Table 1 (Examples 1 to 4), the components (a) and (b) of the activator particles (I), 7% by weight of zeolite and A 50% by weight solids slurry composed of components other than the fragrance was prepared and spray-dried to obtain a spray-dried composition. This is put into a Loedige mixer, and the component (a)
The components (b) and (b) were charged, mixed and carried. Next, the remaining zeolite, perfume and the like were mixed to obtain activator particles (I).

Next, the obtained activator particles (I), the disintegrant particles (II) and other particles were mixed,
g into a 35 mm diameter tableting mold, 25 ° C, 40 kg
A tablet detergent was molded by pressing at f / cm ² (3.92 MPa) for 1 minute. Next, the obtained tablet-type detergent was divided and packaged in a water-soluble material. The same evaluation as in Example 1 was performed for the obtained tablet detergent. Table 3 shows the results.

[0084]

[Table 3]

──────────────────────────────────────────────────の Continued on the front page (51) Int.Cl. ⁷ Identification symbol FI Theme coat ゛ (Reference) C11D 3/38 C11D 3/38 F term (Reference) 4H003 AB03 AB15 AB19 AB21 AB42 AB44 AC08 AC09 AC23 BA17 CA08 CA20 DA01 EA20 EA28 EB22 EB32 EC01 EC03 ED02 EE05 FA32

Claims (7)

[Claims] 1. An activator particle (I) containing (a) an anionic surfactant, (b) a nonionic surfactant, (c) a water-soluble inorganic salt and (d) a water-insoluble inorganic substance, and a disintegrant A tablet detergent containing 3 to 20% by weight of particles (II), wherein the ratio of (a) to (d) is (a) + (b) = 15 to
50% by weight, (c) + (d) = 40-70% by weight,
(A) / (b) = 6/1 to 50/1 (weight ratio), (c)
/ (D) = 1/3 to 3/1 (weight ratio), [(a) +
(B) + (c)] / (d) = 10/1 to 1/1 (weight ratio). 2. The tablet detergent according to claim 1, wherein the disintegrant particles (II) contain (II ₁ ) particles containing a water-insoluble substance and (II ₂ ) particles containing a water-soluble substance. (II ₁ ) The water-insoluble substance is cellulose,
3. The tablet detergent according to claim 2, which is at least one selected from starch, polyvinylpyrrolidone and polyvinyl alcohol. 4. The tablet detergent according to claim 2, wherein (II ₂ ) the water-soluble substance is at least one selected from percarbonate, perborate, perphosphate and persulfate. 5. A tablet detergent obtained by surrounding the tablet detergent according to claim 1 with a water-soluble material. 6. It has the following steps A, B, C and D.
Activator particles (I) containing (a) an anionic surfactant, (b) a nonionic surfactant, (c) a water-soluble inorganic salt and (d) a water-insoluble inorganic substance, and disintegrant particles (II) 3 ~ 20
% By weight of a tablet detergent comprising (a)
(D) is (a) + (b) = 15 to 50% by weight,
(C) + (d) = 40-70% by weight, (a) / (b) =
6/1 to 50/1 (weight ratio), (c) / (d) = 1/3
３3/1 (weight ratio), [(a) + (b) + (c)] /
(D) A method for producing a tablet-type detergent in which 10/1 to 1/1 (weight ratio). Step A: Step of producing activator particles (I) containing (a), (b), (c) and (d) and having an average particle diameter of 300 to 1500 μm Step B: disintegrant having an average particle diameter of 200 to 1500 μm Step of producing particles (II) Step C: step of mixing activator particles (I) and disintegrant particles (II) Step D: mixing the mixture obtained in step C at 20 to 50 ° C
At a temperature of 20 to 100 kgf / cm ² (1.96 to
Forming with a molding pressure of 9.81 MPa) 7. The step A comprises spray-drying a slurry containing (c) a water-soluble inorganic salt and (d) a water-insoluble inorganic substance, and adding (a) an anionic surfactant and (b) The production method according to claim 6, further comprising a step of supporting a nonionic surfactant.