JP2003193096A - Tablet detergent composition - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To obtain a tablet detergent composition that can inhibit the disintegration in water from deteriorating after long-term storage in the composition wherein the content of a straight-chain alkylbenzenesulfonate is reduced. <P>SOLUTION: This tablet detergent composition comprises (a) 10-50 mass % of a surfactant, (b) 0-5 mass % of the straight-chain alkylbenzenesulfonate salt, (c) 0.1-3 mass % of a polycarboxylate salt and (d) 0.1-5 mass % of a reductant. <P>COPYRIGHT: (C)2003,JPO

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a tablet detergent composition, and more particularly to a composition which prevents deterioration of disintegration properties of tablets in water during long-term storage.

[0002]

2. Description of the Related Art Generally, a tablet detergent composition is obtained by compression-molding detergent granules. In order to promote the disintegration property of the tablet detergent in water, a tablet disintegrating agent or a gas generating substance has been conventionally added. Is known (Table 20
01-514690, WO98 / 54283, WO98
/ 55575, etc.). Such detergent compositions include
Linear alkyl benzene sulfonate, which has excellent cost performance, is used as a general-purpose anionic surfactant. In recent years, to reduce the environmental impact of detergents,
A detergent containing a small amount of the linear alkylbenzene sulfonate has been desired.

[0003]

However, it has been found that when the compounding amount of the linear alkylbenzene sulfonate is reduced, the disintegrating property of the tablet detergent in water deteriorates with time. The present invention has been made in view of the above circumstances, and an object thereof is to provide a tablet detergent composition in which deterioration of disintegration in water after long-term storage of the tablet detergent is prevented.

[0004]

Means for Solving the Problems As a result of intensive studies to solve the above problems, the present inventors have found that in a tablet detergent composition containing 0 to 5% by mass of a linear alkylbenzene sulfonate, a polycarboxylic acid salt is used. It was found that the disintegration property of the tablet detergent in water can be prevented from being deteriorated by adding a specific amount of the reducing agent and the reducing agent, and the present invention has been completed.

That is, the tablet detergent composition of the present invention is
It is characterized by containing the following components (a) to (d). (A) Surfactant: 10 to 50% by mass, (b) Linear alkylbenzene sulfonate: 0 to 5% by mass,
(C) Polycarboxylic acid salt: 0.1 to 3 mass%, (d) reducing agent: 0.1 to 5 mass%.

[0006]

BEST MODE FOR CARRYING OUT THE INVENTION The present invention will be described in more detail below. Examples of the surfactant as the component (a) include various surfactants such as anionic surfactants, nonionic surfactants, cationic surfactants and amphoteric surfactants, which may be used alone or in combination of two kinds. The above can be used in appropriate combination. The total amount of these surfactants in the composition is 10 to 50% by mass, preferably 20 to 40% by mass. However, among the above anionic surfactants, the linear alkylbenzene sulfonate of the component (b) is
From the viewpoint of environmental load, it is 0 to 5% by mass, preferably 0 to 3% by mass in the composition.

The component (b) has 8 to 18 carbon atoms.
Linear alkylbenzene sulfonate, preferably linear sodium alkylbenzenesulfonate having 10 to 14 carbon atoms and potassium linear alkylbenzenesulfonate having 10 to 14 carbon atoms.

As the anionic surfactant other than the above-mentioned component (b), sulfo fatty acid lower alkyl ester salt, alkyl sulfate ester salt, soap, olefin sulfonate and the like can be used, but from the viewpoint of environmental load, it is preferable. , An anionic surfactant selected from sulfo fatty acid lower alkyl ester salt, alkyl sulfate ester salt, and soap.
Specifically, α-sulfofatty acid lower alkyl (C1 to C3) ester salt having 13 to 19 carbon atoms, C10 to C2
An alkyl sulfate ester salt of 0, a saturated or unsaturated fatty acid salt of 12 to 22 carbon atoms, and the like can be preferably used. As these salts, alkali metal salts such as sodium salts and potassium salts, amine salts, ammonium salts and the like can be used.

Specific examples of the nonionic surfactant used as the component (a) include the following. (1) An EO-added nonionic surfactant (alkyl ether ethoxylate) in which ethylene oxide (EO) is added in an average of 5 to 30 mol to an alcohol having an average of 10 to 20 carbon atoms. (2) Ethylene oxide (EO) and propylene oxide (PO) in alcohol having an average carbon number of 10 to 20
An EO-PO-added nonionic surfactant having an average of 5 to 30 moles added. (3) A fatty acid ester type nonionic surfactant represented by the following chemical formula 1. [Chemical Formula 1] R1-CO (OR2) nOR3 (In the formula, R1 has 5 to 21 carbon atoms, preferably 9 to 9 carbon atoms.
17 alkyl group or alkenyl group, R2 has 2 carbon atoms
˜4, and it is preferable that EO is independently added or EO and PO are mixed and added to form OR2.
Is an alkyl group having 1 to 4 carbon atoms, preferably 1 to 2 carbon atoms
, An n is the average number of moles of OR2 added, and
Indicates a number of -30, preferably a number of 5-20. (4) A fatty acid alkanolamide having an average carbon number of 10 to 20. (5) An alkylamine oxide having an average carbon number of 10 to 20. (6) The sugar residue is a monosaccharide such as glucose, galactose, xylose, mannose, lyxose, or arabinose,
Alternatively, a sugar fatty acid ester-based surfactant that is a polysaccharide such as maltose, xylopyose, lactose, sucrose. (7) Alkyl glycoside represented by the following Chemical Formula 2 [Chemical Formula 2] R1O (R2O) y (z) x (wherein, z is a residue derived from a reducing sugar having 5 to 6 carbon atoms, R
1 is an alkyl group, an alkenyl group, a hydroxyalkyl group, a hydroxyalkylphenyl group or a mixture thereof, wherein the alkyl group or the alkenyl group has 8 carbon atoms.
~ 20, R2 is an alkylene group having 2 to 4 carbon atoms, y
Indicates a number of 0 to 30, and x indicates a number of 1.0 to 1.42. Among the above nonionic surfactants, the nonionic surfactants (1) to (3) above are preferable. In the nonionic surfactants of (1) to (3) above, the number of moles of EO added is 10 to 10.
The 20 nonionic surfactants are particularly preferable because they enhance the effects of the present invention. EO addition mole number is 10-20
The amount of the nonionic surfactant is 1 to 15 in the composition.
Mass%, especially 3 to 10 mass% is preferred.

Examples of the cationic surfactant used in the present invention include dilong-chain alkyldishort-chain alkyl-type quaternary ammonium salts, mono-long-chain alkyltri-short-chain alkyl-type quaternary ammonium salts, and imidazoline derivatives. Examples of the amphoteric surfactant include lauric acid amidopropyl betaine, stearic acid amidoethyl betaine, betaines such as 2-alkyl-N-carboxymethyl-N-hydroxyethylimidazolinium betaine, lecithin (phosphatidylcholine), and the like. .

As the polycarboxylic acid salt of the component (c),
Polyacrylic acid, acrylic acid-maleic acid copolymer, acrylic acid-allyl alcohol copolymer, hydroxyacrylic acid polymer, polysaccharide-acrylic acid copolymer and other acrylic acid polymers and salts of copolymers, maleic acid Acid, itaconic acid, fumaric acid, tetramethylene 1,2-dicarboxylic acid,
Examples thereof include salts of polymers or copolymers such as succinic acid and aspartic acid. The compounding amount of the polycarboxylic acid salt is 0.1 to 3% by mass, preferably 0.2 to 2% by mass from the viewpoint of effects and environmental load. Among the above polycarboxylic acid salts, sodium polyacrylate, maleic acid (MA)
/ Sodium salt of acrylic acid (AA) copolymer is preferred. The weight average molecular weight of sodium polyacrylate is preferably 500 to 100,000, and MA / AA
The sodium salt of the copolymer has a mass average molecular weight of 500 to
100,000, MA / AA in mass ratio 80/20 to 3
0/70 is preferred.

Examples of the reducing agent as the component (d) include sulfite and bisulfite. As these salts, alkali metal salts such as sodium salt and potassium salt are preferable. The compounding amount of the component (d) is 0.1 to 5% by mass, preferably 0.3 to 3% by mass.

In the tablet detergent of the present invention, in addition to the above components, a disintegrating agent and a lubricant which are components peculiar to the tablet detergent are used. The lubricant is used for favorably performing compression molding and has a particle size of 10 μm or less, preferably 0.1 to
5 μm, 0.1 to 10% by mass in the particle mixture. Specific examples of the lubricant include fine powders of zeolite, talc, silica and the like, and zeolite is particularly preferably used. The disintegrant is used to accelerate the disintegration of the tablet detergent in water, and a water-swellable granular substance that absorbs water to increase the volume and physically disintegrates the tablet can be suitably used (swelling property). Disintegrant). The swelling disintegrating agent is preferably a highly swelling disintegrating agent having a swelling property of 10 mL / g or more. For example, ARBOCEL T manufactured by Rettenmeier Co., Ltd.
Granulated product of powdered cellulose such as F30HG, crosslinked carboxymethyl cellulose (trade name: Ac-di-so
1, manufactured by FMC Corporation, carboxymethylcellulose calcium (trade name: ECG-505,
Nichirin Kagaku Co., Ltd., etc., and especially ARB
A granulated product of powdered cellulose such as OCEL TF30HG is preferably used. The average particle size of the disintegrant particles is preferably 500 to 1000 μm, particularly 700 to 900.
μm is preferred. Further, the swelling disintegrant includes a high swelling disintegrant and a low swelling disintegrant (swellability of 10 mL / g
Less than) may be combined. As a low swelling disintegrant, powdered cellulose (trade name: KC Flock, manufactured by Nippon Paper Industries Co., Ltd.), crystalline cellulose (trade name: Avicel, manufactured by Asahi Kasei Co., Ltd.), crosslinked polyvinylpyrrolidone (trade name: poly) Plasdon, manufactured by ISP) and the like.
The high swelling disintegrant / low swelling disintegrant is preferably 3/7 to
7/3, particularly preferably 4/6 to 6/4 are used in the range of ratio.

The average particle size of the disintegrant particles obtained by combining the high swelling disintegrant and the low swelling disintegrant is preferably 2
50 to 1000 μm, particularly 355 to 710 μm are preferable. The disintegrating agent of the present invention further includes a disintegrating agent that disintegrates tablets by foaming (effervescent disintegrating agent).
Foaming, as defined herein, means the generation of gas bubbles from a liquid as a result of the chemical reaction of a soluble acid source with an alkali metal carbonate to produce carbon dioxide gas. In the detergent composition containing the alkali metal carbonate of the present invention, the effervescent disintegrant means a soluble acid source. As an example of the effervescent disintegrating agent, an acid salt of an organic acid such as citric acid, succinic acid, tartaric acid or the like and an inorganic acid such as a bisulfate salt is preferably used.

The tablet detergent composition of the present invention may contain various components usually contained in a detergent composition within a range that does not impair the effects of the present invention. For example, an alkaline agent (sodium carbonate, potassium carbonate, Sodium silicate,
Monoethanolamine, diethanolamine, etc.), calcium scavenger (A-type zeolite, P-type zeolite, layered silicate, citrate, etc.), bleaching agent (coated percarbonate, perborate), bleaching activation Agents (organic peracid precursors, metal ions, metal ion complex catalysts, etc.), enzyme granules (protease, amylase, lipase, cellulase, pectinase, etc.), enzyme stabilizers, fluorescent agents, rinse agents, Perfumes, solvents (polyethylene glycol, alcohol, etc.), hydrotropes, anti-redeposition agents and the like can be added in a usual dose within a range that does not impair the effects of the present invention.

A preferred method for producing the tablet detergent composition of the present invention is shown below. First, the surfactant-containing particles containing the components (a) to (d) and the builder are prepared by a known method for producing a high-density granular detergent. The particles have a mass average particle diameter of 500 to 1500 μm, preferably 550 to 1200 μm, and more preferably 600 to 10 μm.
It is 00 μm. The proportion of particles having a particle size of 75 to 355 μm is 10 to 30% by mass, preferably 10 to 20% by mass, and more preferably 15 to 20% by mass.
The fine powder having a particle size of less than 5 μm is preferably 5% by mass or less, particularly 3% by mass or less. The bulk density of the particles is 0.6 to 0.9.
g / mL, preferably 0.7 to 0.8 g / mL. Next, as the surfactant-containing particles, the disintegrant particles, and the optional component particles, enzyme particles, bleaching agent particles, bleaching activator particles, builder particles, lubricants, etc. are mixed to prepare a particle mixture, which is then compressed. Mold to form a tablet detergent composition.

The bulk density of the particle mixture is from 0.6 to
It is 0.9 g / mL, preferably 0.7 to 0.8 g / mL.

The tablet detergent composition obtained by compression molding the particle mixture has a bulk density of 0.9 to 1.6 g / mL,
It is preferably 1.0 to 1.5 g / mL, more preferably 1.2 to 1.4 g / mL.

In the above particle mixture, the proportion of the surfactant-containing particles is preferably 50 to 95% by mass, preferably 70 to 95, of the total particles having a particle size of 75 to 355 μm.
Mass%, and more preferably 80 to 92 mass% is suitable. Further, in the particle mixture, fine powder having a particle size of less than 75 μm is
5 mass% or less, especially 3 mass% or less are suitable.

By compressing and molding the above-mentioned particle mixture, it is possible to provide a tablet detergent which is not broken by vibration during transportation, but quickly disintegrates in water.

In the compression molding of the particle mixture, a tableting machine basically composed of a combination of a die and a punch and a compression molding device is used. Examples of the tableting machine include a vertical powder molding machine manufactured by Kikusui Seisakusho Co., Ltd., a single-shot tableting machine manufactured by Okada Seiko Co., Ltd., and a single-shot tableting machine such as a standing press manufactured by Fuji Chemical Machinery Co., Ltd. ) Kikusui clean press series, tough press series, FETTE P series,
PT Series, KORSCH PH Series, TRP
Examples include rotary tablet presses such as series. The tableting pressure is not particularly limited, but is preferably 3 to 10 kN, particularly 4 to 8 kN. If the tableting pressure is too high, sufficient low temperature disintegration may not be obtained, and if it is too low, the desired strength may be difficult to obtain. For the same reason, the compression strength of the compression molded product immediately after molding has a tablet strength of 30 to 70 according to the measuring method described in Examples described later.
Tableting is preferably performed so as to have N, particularly 40 to 60 N. The temperature for compression molding is not particularly limited, but is preferably 15 to 35 ° C.

[0022]

According to the present invention, the load on the environment is low,
It is possible to provide a tablet detergent composition that prevents deterioration of disintegration in water after long-term storage.

[0023]

EXAMPLES Next, the present invention will be described in detail with reference to examples, but the present invention is not limited to these examples.

Preparation Example I (Examples 1 to 12, Comparative Examples 1 to 1)
3) Immediately after production (within 1 hour after tableting) using a tablet detergent composition having the composition shown in Tables 1 to 3 prepared by the following method
And the disintegration property after storage according to the following storage method were evaluated by the following measurement methods. The results of these evaluations are shown together in Tables 1 to 3. In addition, the numerical value in Tables 1-3 is the mass% of the pure content of each component except an enzyme granulated material and a fragrance | flavor.

(1) Method for preparing detergent composition (1-1) Granulation of detergent granules Among the detergent compositions shown in Tables 1 to 3, nonionic surfactant,
A detergent slurry having a solid content of 40% by mass was prepared using a part of zeolite (granular A-type zeolite and fine powder A-type zeolite for coating), disintegrant, enzyme, fragrance, and dye, and the slurry was prepared. Hot air temperature 3 using a flow-type drying tower
Spray drying was carried out under the condition of 00 ° C. to obtain spray dried particles having a water content of 3% by mass. Zeolite for detergent slurry is fine powder A
Type zeolite (Shilton B, Mizusawa Chemical) was used. Along with these dried particles, the nonionic surfactants shown in Tables 1 to 3 and water for water content adjustment were put into a continuous kneader (KRC-S4 type, manufactured by Kurimoto Iron Works Co., Ltd.), and a kneading capacity of 120 kg /
The mixture was kneaded under the conditions of h and a temperature of 70 ° C. to obtain an amorphous solid detergent. This irregular solid detergent is a pelleter double equipped with a die with a hole diameter of 10 mm (Fuji Paudal Co., Ltd., EXD
While extruding using FJS-100 type, cutting with a cutter (cutter peripheral speed is 5 m / s), a pellet-like solid detergent having a length of about 5 to 30 mm was obtained. Then, 3.2% of granule A-type zeolite (average particle diameter 200 μm) as a grinding aid was added to the obtained solid detergent, and cold air (10
Fitzmill (DKA-3, manufactured by Hosokawa Micron Co., Ltd.) arranged in three stages in series in the coexistence of (° C, 15 m / s) was used to adjust the number of revolutions so that the average particle diameter was 800 μm and pulverized (screen. Hole diameter: 1st step / 2nd step / 3rd step = 8mm / 6mm / 3mm). Finally, fill with a horizontal cylindrical rolling mixer (a cylinder having a diameter of 585 mm, a cylinder length of 490 mm, a drum inner wall surface of the container 131.7 L having a clearance of 20 mm from the inner wall surface, and two baffle plates having a height of 45 mm). 0.5% by mass of fine powder A-type zeolite was added under the conditions of a rate of 30%, a rotation speed of 22 rpm, and 25 ° C., and the mixture was rolled for 1 minute for surface modification to obtain a detergent granulated product. The detergent granules were classified using a sieve having a mesh size of 425 μm to obtain detergent granules (88% of the detergent granules) having an average particle diameter of 900 μm that did not pass through the sieve. In addition, the fine powder (12% in the detergent granules) that has permeated through a sieve having an opening of 425 μm was supplied again to the continuous kneader and reused. (1-2) Coloring A of Detergent Granules In order to color a part of the obtained detergent granules, a portion of the detergent granules was mixed with a Ledige mixer (Matsubo Co., Ltd., M20).
It was charged into the mold (filling rate 50%), and stirring of the main shaft (200 rpm) and the chopper (3000 rpm) was started. Immediately after the stirring was started, a 20% aqueous dispersion was gradually added as a solid content of the dye A over about 5 minutes, and after the addition, the mixture was stirred for 20 seconds to obtain a colored granular detergent.

The colored detergent granules were reduced by mixing 1% with the uncolored detergent granules. The amount of the pigment added was set so that, when the colored detergent granules were reduced by 1% with respect to the uncolored detergent granules, the tablet detergent compositions had the compositions shown in Tables 1 to 3.

(2) Addition of enzyme granules To the partially-colored detergent granules, the enzyme granules were added in the amounts shown in Tables 1 to 3, and a horizontal cylindrical rolling mixer (cylindrical diameter 585 m) was added.
m, cylinder length 490 mm, clearance of the inner wall surface of the drum of the container 131.7L of 20 mm, height 45
mm baffle plate), the mixture was mixed at a filling rate of 30%, a rotation speed of 22 rpm, and 25 ° C. to obtain a mixture of detergent granules and enzyme granules.

(3) Preparation of tablets The above mixture obtained was mixed with a horizontal cylindrical tumbling mixer (cylinder diameter 585 mm, cylinder length 490 mm, the inner wall surface of the container 131.7 L had a clearance of 20 mm from the inner wall surface,
It was filled in (having two baffle plates with a height of 45 mm) (filling rate 30%) and started rolling under the conditions of a rotation speed of 22 rpm and 25 ° C. The fragrances shown in Tables 1 to 3 were sprayed there, and then finely divided A type zeolite (Silton B, Mizusawa Chemical Co., Ltd.)
Mass% was added and mixed for 30 seconds. A, which is a disintegrant
RBOCEL TF30HG (Rettenmeyer) was added and mixed for 30 seconds to obtain a mixture before compression molding. 20 g of the mixture before compression molding was placed in a tableting die (flat shape: round shape, side surface shape: flat edge) having a diameter of 34 mm, and the mixture for tableting was mixed with a single-shot tableting machine (N60E: Okada Seiko). Temperature 2
Tableting was performed at 5 ° C., and the tableting pressure was adjusted so that the tablet strength immediately after molding was 45 N in the following evaluation method, and compression molding was performed to obtain a tablet detergent composition having a mass of 20 g. With respect to each tablet detergent composition, the disintegration property and the disintegration property after long-term storage were evaluated according to the following evaluation methods. The results are shown in Table 1.
It is also described in ~ 3. The strength of the obtained tablets was confirmed according to the following method for measuring the strength of tablets.

(4) Evaluation method (4-1) Method for measuring tablet strength The tablets prepared by the above method were measured with a tablet strength meter (TD-
50: Okada Seiko), the pressure arm was moved at a speed of 20 mm per minute, and a force was applied in the diameter direction of the tablet, and the maximum stress until the tablet collapsed was defined as the tablet strength. (4-2) Method of measuring disintegration About 800 mL of water at 5 ° C was put into a 1-liter glass beaker, and a small mesh (circular shape with a diameter of 75 mm, mesh opening 4
mm, the wire diameter of the mesh is 1.08 mm), 1 tablet is gently put in water and kept at a position of a depth of about 3 cm from the water surface. The time required for the tablet to disintegrate in water and disintegrate until it completely dropped from the net was taken as the disintegration time. The disintegration time was evaluated according to the following criteria, and ◯ and ⊚ were evaluated as good.

<Evaluation Criteria> ⊚: Disintegration time 30 seconds or less ○: Disintegration time more than 30 seconds to 60 seconds Δ: Disintegration time more than 60 seconds to 120 seconds ×: Disintegration time more than 120 seconds (4-3) Long-term storage Measurement of Disintegration Property of Later Tablet Detergent Composition The obtained tablet detergent composition was composed of an unstretched polypropylene (CPP) film and a stretched polypropylene (OPP) film.
A pillow film, which is a two-layer film with a PP) film, was used as a packaging material and was pillow-packaged as follows.

A film of 80 mm × 120 mm size made of the following materials was first used to form a cylinder having a size of 80 mm × 100 mm circumference, and one of the tablets prepared above was placed in the cylinder. A gusset (folded) was put into a pillow package having a short side width of 35 mm. The length of the long side was changed by adjusting the seal position, and the outside of the seal portion was cut after bonding.

Next, the pillow package was filled in a rectangular carton container made of mini cardboard. The size of the packaging container is length x width x height = 115 mm x 95 mm x
The length of the pillow package was 140 mm, and the pillow package was placed with the long side of the pillow package in the height direction and the short side of the pillow package in the horizontal direction. The stacked pillow packages are packed vertically and horizontally in 3 rows x 5 rows, and a partition for coated cardboard is introduced on top of them, and the pillow packages stacked in the same direction are also placed vertically and horizontally. Pillow packages were filled so as to have 3 rows × 5 rows, and a total of 30 pillow packages were filled in the packaging container. The tablet detergent composition filled in this packaging container was kept at 45 ° C. and 85% RH for 16 hours and 25 hours.
The tablet detergent composition after being stored in a constant temperature and humidity chamber in which the condition of 65 ° C RH for 8 hours is alternately repeated for 1 month, and the tablet detergent composition after the storage is completed, the disintegration property of the tablet detergent composition of (4-2) is measured. It carried out and it judged by the same judgment standard.

Preparation Example II (Examples 13 to 24, Comparative Example 4)
~ 6) Immediately after production (within 1 hour after tableting) using the tablet detergent composition having the composition shown in Tables 4 to 6 prepared by the following method
And the disintegration property after storage according to the following storage method were evaluated by the following measurement methods. The results of these evaluations are shown together in Tables 4-6. In addition, the numerical value in Tables 4-6 is the mass% of the pure content of each component except enzyme granules and a fragrance | flavor.

(1) Method for preparing detergent composition (1-1) Granulation of detergent granules Detergent granules having the compositions shown in Tables 4 to 6 were prepared in the same manner as in Preparation Example I to form detergent granules having an average particle diameter of 900 μm ( 8 of detergent granules
2%) was obtained. The fine powder (18% in the detergent granules) that had passed through a sieve with an opening of 425 μm was supplied again to the continuous kneader for reuse. (1-2) Coloring of Detergent Granules In order to color a part of the obtained detergent granules, the detergent granules are transported at a speed of 0.5 m / s on a belt conveyor (the detergent granule layer height on the belt conveyor is 30 mm. , Layer width 300m
m) A 20% aqueous dispersion as a solid content of Dye B was sprayed on the surface as a tablet detergent composition so as to have the compositions shown in Tables 4 to 6.

(2) Addition of enzyme granules The same amounts of enzyme granules as shown in Tables 4 to 6 were added in the same manner as in the method of adding enzyme granules in Preparation Example I.

(3) Preparation of tablets As in Preparation Example I, fragrance, fine powder A-type zeolite, and ARBOCEL, which is a disintegrant, are used so as to have the compositions shown in Tables 4 to 6.
TF30HG (Rettenmeyer) was added and mixed to obtain a mixture before compression molding.

The mixture before compression molding was compression molded under the same conditions as in Preparation Example I to obtain a tablet detergent composition having a mass of 20 g. Preparation Example I for each tablet detergent composition
The disintegration property and the disintegration property after long-term storage were evaluated according to the method described in (4) Evaluation method. The results are also shown in Tables 4-6.

Preparation Example III (Examples 25 to 36, Comparative Examples 7 to 9) Using tablet detergent compositions having the compositions shown in Tables 7 to 9 prepared by the following method, immediately after production (1 hour after tableting Within)
The disintegration property in water and the disintegration property in water after storage by the following storage method were evaluated by the following measurement methods. The results of these evaluations are shown together in Tables 7-9. Table 7-
The numerical value in 9 is the mass% of the pure content of each component excluding enzyme granules and fragrances.

(1) Method for preparing detergent composition (1-1) Granulation of detergent granules Among the detergent compositions shown in Tables 7 to 9, nonionic surfactant,
A detergent slurry having a solid content of 40% by mass was prepared using each component excluding a part of zeolite (fine powder A type zeolite for coating), a disintegrant, an enzyme, a fragrance, and a dye, and the slurry was applied to a countercurrent drying tower. It was spray-dried under the conditions of a hot air temperature of 300 ° C. to obtain spray-dried particles having a water content of 3% by mass. As the zeolite for the detergent slurry, fine powder type A zeolite (Silton B, Mizusawa Chemical Co., Ltd.) was used. The spray-dried particles were put into a high speed mixer (FS-25 type, manufactured by Fukae Industry Co., Ltd.) (filling rate 50%), and agitator 200 rpm,
The nonionic surfactant and water for adjusting the water content were added while stirring under the conditions of a chopper of 1000 rpm, and stirring granulation was carried out under the conditions of 35 ° C. until the average particle size became about 550 μm. Finally, 1% by mass of fine powder A-type zeolite (Shilton B, Mizusawa Chemical Co., Ltd.) was added, and the mixture was stirred for 30 seconds to coat the surface to obtain a detergent granule. The detergent granules were classified using a sieve with an opening of 1400 μm and a sieve with an opening of 150 μm, and the opening was 14
Detergent granules having an average particle diameter of 600 μm (8% in detergent granules)
9%) was obtained. The coarse powder (1% in the detergent granules) that did not pass through the 1400 μm sieve was fitted with a Fitzmill (Hosokawa Micron Co., Ltd., D
KA-3) crushed at a rotation speed of 4700 rpm and passed through a sieve with an opening of 150 μm (10% of detergent granules)
In the state as it was, it was supplied again to the stirring granulator and reused. (1-2) Partially colored detergent granules were obtained in the same manner as in Preparation Example 1 except that the coloring pigment of the detergent granules was changed to the pigment C.

(2) Addition of enzyme granules The same amounts of enzyme granules as shown in Tables 7 to 9 were added in the same manner as in the method of adding enzyme granules in Preparation Example 1.

(3) Preparation of tablet As in Preparation Example I, a layered silicate was added and mixed together with the fragrance, the finely divided A-type zeolite, and the disintegrating agent citric acid so as to have the compositions shown in Tables 7 to 9, A pre-compression molding mixture was obtained. The above-mentioned mixture before compression molding was compression-molded under the same conditions as in Preparation Example I except that the tablet strength immediately after molding was adjusted so that the tablet strength immediately after molding was 25 N, and then about 1
The above compression molded product was immersed in adipic acid dissolved at a temperature of 70 ° C. and air dried to obtain a final tablet detergent composition. The total weight of this tablet was 20 g and the tablet strength was 45N. For each tablet detergent composition, the disintegration property and the disintegration property after long-term storage were evaluated according to the method described in Preparation Example I (4) Evaluation method. The results are shown in Table 7-
It is also described in 9.

[0042]

[Table 1]

[0043]

[Table 2]

[0044]

[Table 3]

[0045]

[Table 4]

[0046]

[Table 5]

[0047]

[Table 6]

[0048]

[Table 7]

[0049]

[Table 8]

[0050]

[Table 9]

The components used in the examples and comparative examples are
It is as follows. LAS-Na: straight-chain alkyl (carbon number 10 to 14) sodium benzenesulfonate (when producing a composition, Lypon LH-200 (LAS-H pure content 96, manufactured by Lion Corporation)
%) Was neutralized with a 48% sodium hydroxide aqueous solution) LAS-K: straight-chain alkyl (C 10-14) potassium benzene sulfonate (in the production of the composition, Lion Co., Ltd.) Made Ripon LH-200 (LAS-H Pure 96
%) Prepared by neutralizing 48% potassium hydroxide aqueous solution) AOS-K: α having an alkyl group having 14 to 18 carbon atoms
-Potassium olefin sulfonate (manufactured by Lion Corporation)
70% pure aqueous slurry) -α-SF-Na: sodium salt of α-sulfo fatty acid methyl ester having an alkyl group having 14 and 16 carbon atoms (mass ratio C14 / C16 = 2/8), pure 65% , Solids 7
3%, α-sulfofatty acid disodium salt 3%, methyl sulfate 3%, sodium sulfate 2%, methanol 2
%, Lion Corporation AS-Na: sodium lauryl sulfate, 95% pure,
Lion Co., Ltd., Sannor LM-1100NT Soap: Sodium fatty acid having an alkyl group having 12 to 18 carbon atoms (Lion Co., C12: 0.9%, C
18: 80.2%, unsaturated fatty acid 80.2%, molecular weight 289, pure 67-68%, titer 47.0 ° C) -Nonionic surfactant species: Nonion 1: Oxidation of Dyadol 13 (Mitsubishi Chemical). 15 mol ethylene adduct (manufactured by Lion Corporation, 90% pure,
AAO-90) Nonion 2: 25 mol of ethylene oxide adduct of Dyador 13 (Mitsubishi Chemical) (Lion Co., Ltd., net content: 84%,
AAY-13) Nonion 3: Fatty acid methyl ester (Pastel M-181 manufactured by Lion Corporation, main component methyl oleate) 15 mol ethylene oxide adduct Nonion 4: Fatty acid methyl ester (Pastel M-12 manufactured by Lion Corporation) , Main component methyl laurate) ethylene oxide 15 mol adduct nonion 5: dovanol 23 (Mitsubishi Chemical) ethylene oxide 8 mol adduct (Lion Co., Dovanox 23)
H) -Reducing agent type: reducing agent A: sodium sulfite (manufactured by Mitsui Chemicals, Inc., anhydrous sodium sulfite) reducing agent B: potassium sulfite reducing agent C: sodium bisulfite reducing agent D: potassium bisulfite-zeolite: A type Zeolite (Silton B manufactured by Mizusawa Chemical Co., Ltd. and granules manufactured by Cosmo: average particle size 200 μm) Sodium carbonate: heavy sodium carbonate, Asahi Glass Co., Ltd.
Made, soda ash, potassium carbonate: Asahi Glass Co., Ltd., potassium carbonate (powder), sodium silicate: JIS No. 1 sodium silicate (Osaka silicate Soda Co., Ltd., sodium silicate) layered silicate: crystalline layered sodium silicate (SKS-6 manufactured by Hoechst Co.) MA / AA copolymer: sodium salt of acrylic acid / maleic acid copolymer, trade name Sokaran CP7 (BAS
F) Sodium polyacrylate: Sodium polyacrylate MW = 10000 (manufactured by Nippon Pure Chemical Co., Ltd., Aronbis
S) -Fluorescent brightener: Chinopearl CBS-X (Ciba Specialty Chemicals) / Chinopearl AMS-GX (Ciba Specialty Chemicals) = 4/1 (mass ratio) mixture-Enzyme species: Enzyme A: Proteolytic enzyme (Canase 24 manufactured by Novozyme
T) / lipolytic enzyme (Novozymes Lipolase Ultra 50T) / cellulose degrading enzyme (Novozymes Cellzyme 0.7T) / starch degrading enzyme (Novozymes Termamyl 60T) = 5/1/3/1 (mass ratio) Mixture enzyme B: Proteolytic enzyme (Evalase 8 manufactured by Novozyme)
T) / lipolytic enzyme (Novozymes Lipolase Ultra 50T) / cellulose degrading enzyme (Novozymes Cellzyme 0.7T) / starch degrading enzyme (Novozymes Termamyl 60T) = 5/1/3/1 (mass ratio) Mixture enzyme C: Proteolytic enzyme (Sabinase 12 manufactured by Novozyme)
T) / lipolytic enzyme (Novozymes Lipolase Ultra 50T) / cellulose degrading enzyme (Novozymes Cellzyme 0.7T) / starch degrading enzyme (Novozymes Termamyl 60T) = 7/1/1/1 (mass ratio) Mixture enzyme D: Proteolytic enzyme 1 (Cannase 2 manufactured by Novozyme)
4T) / Proteolytic enzyme 2 (Savinase 1 manufactured by Novozyme)
2T) / lipolytic enzyme (Novozymes Lipolase Ultra 50T) / cellulose degrading enzyme (Novozymes Cellzyme 0.7T) / starch degrading enzyme (Novozymes Termamyl 60T) = 5/1/1/2/1 (mass) Ratio) Mixture / Disintegrant type: Disintegrant A: ARBOCEL TF30HG (manufactured by Rettenmeyer) Disintegrant B: Citric acid / Dye type: Dye A: Acrylonitrile / styrene / acrylic acid as a constituent monomer, radical emulsification in water dispersion system Spherical resin particles having an average particle diameter of 0.35 μm obtained by polymerization,
About 1% by mass of C.I. I. BASIC RE
An aqueous dispersion of a pink fluorescent pigment obtained by adding D-1 to a suspension of polymerized resin and heat-treating it. Dye B: Ultramarine (Dainichi Seika Kogyo KK, Ultramari
ne Blue) Pigment C: Pigment Green 7 (manufactured by Dainichiseika Kogyo Co., Ltd.)-Perfume compositions A to D: Japanese Patent Application No. 2000-346626 Compositions shown in Tables 11 to 18.

   ─────────────────────────────────────────────────── ─── Continued front page    F-term (reference) 4H003 AB15 AB19 AB21 AB27 AB32                       AB44 DA01 EA12 EA15 EA16                       EA28 EB08 EB30 EC01 EC02                       EC03 ED02 EE02 FA12 FA16                       FA26 FA32

Claims (2)

[Claims] 1. A surfactant is contained in an amount of 10 to 50% by mass, and a linear alkylbenzene sulfonate of (b) is included in an amount of 0 to 5.
Mass%, (c) polycarboxylic acid salt: 0.1 to 3 mass%,
(D) Reducing agent: 0.1 to 5 mass%, a tablet detergent composition characterized by the above. 2. The tablet detergent composition according to claim 1, further comprising a nonionic surfactant having an average number of moles of ethylene oxide added of 10 to 20 moles.