JP2000352000A - Detergent composition - Google Patents

Abstract

(57) [Problem] To provide a detergent composition which is excellent in solubility and detergency, and has a high soil release effect. Kind Code: A1 A high bulk density detergent particle group containing a surfactant and a soil release agent, wherein the high bulk density detergent particle group has a 95% dissolution time of 120 seconds or less at 10 ° C. by an electric conductivity method. A detergent composition comprising:

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

TECHNICAL FIELD The present invention relates to a detergent composition.

[0002]

2. Description of the Related Art Granular detergent compositions are strongly directed to higher bulk densities and lower usage amounts from the convenience of consumers. However, it is known that a high bulk density detergent composition tends to have a low dissolution rate of detergent particles constituting the composition. In addition, in response to environmental and energy issues and economics, all recent trends in washing machines, such as lowering the temperature of the washing water and shortening the operation time, cause a delay in the dissolving speed of the detergent particles, and as a result, Since the cleaning ability of the detergent composition is remarkably reduced, a great improvement in the dissolution rate of the detergent particles has been desired. On the other hand, the use of soil release agents in detergent compositions has been described in the prior art. However, due to the increase in the bulk density and the reduction in the amount used, a sufficient stain release effect could not be achieved. For example, JP-A-57-65799 and JP-A-61-83298.
Japanese Patent Application Laid-Open Publication No. H11-157550 discloses the use of a stain release agent. However, the solubility of the detergent cannot be said to be sufficient, and a sufficient stain release effect cannot be achieved.

[0003]

SUMMARY OF THE INVENTION An object of the present invention is to provide a detergent composition which is excellent in solubility and detergency and has a high stain-removing effect.

[0004]

That is, the gist of the present invention is as follows.
A detergent composition comprising a high bulk density detergent particle group containing a surfactant and a soil release agent, wherein the high bulk density detergent particle group has a 95% dissolution time of 120 seconds or less at 10 ° C. by an electric conductivity method. About things.

[0005]

DESCRIPTION OF THE PREFERRED EMBODIMENTS High bulk density detergent particles containing a surfactant and a soil release agent (hereinafter also referred to as detergent particles)
The 95% dissolution time at 10 ° C. by the electric conductivity method is 120 seconds or less, preferably 100 seconds or less, more preferably 90 seconds or less, and particularly preferably 80 seconds or less from the viewpoint of improving the cleaning ability. In the present invention, “1”
The 95% dissolution time according to the electric conductivity method at 0 ° C. ”
It is defined as: 1L of cylindrical shape with inner diameter of 105mm
Pour 1 L of distilled water at 10 ° C. into a beaker, and set an electric conductivity meter (CM-60V, manufactured by Toa Denpa Kogyo). Using a cylindrical stirrer with a total length of 35 mm and a diameter of 7.5 mm, 55
Stir at 0 rpm. A 1 g sample at 10 ° C. is introduced into the center of the water vortex. With this time taken as 0 second, the electrical conductivity is measured at 10 second intervals. The value at which the measured value does not increase continuously for 2 minutes or more is defined as the 100% dissolution value, and the time required to reach this value is defined as the 95% dissolution time. A preferred example of the stirrer is “Model SA-35” manufactured by Kagaku Kyoeisha.

The bulk density of the detergent particles is preferably 500 g / L or more, more preferably 500 to 1000.
g / L, more preferably 600 to 1000 g / L, particularly preferably 650 to 850 g / L. The bulk density is
From the viewpoint of economic efficiency, 500 g / L or more is preferable, and from the viewpoint of solubility, 1000 g / L or less is preferable. In addition,
The bulk density of the particle group is measured by a method specified by JIS K3362.

[0007] As one embodiment of the group of high bulk density detergent particles,
Average particle size of 150 to 500 μm, preferably 180 to 5
00 μm, more preferably 180 to 400 μm,
The ratio of the particle group having a particle diameter of 710 μm or more and the particle group having a particle diameter of less than 125 μm is 10% by weight or less, preferably 8% by weight or less, more preferably 5% by weight or less of the entire high bulk density detergent particle group. Detergent particle group (detergent particle group I).

Here, from the viewpoint of preventing dissolution delay due to the formation of the detergent particles I into a paste, the average particle size is 150 μm or more, and the ratio of particles having a particle size of less than 125 μm is 10% by weight or less. Is preferred. Further, from the viewpoint of improving the solubility of the detergent particle group I itself, the average particle size is 50.
It is preferable that the ratio of the particle group of 0 μm or less and 710 μm or more is 10% by weight or less. The average particle diameter of the particle group is the median diameter, and is JIS Z8801.
After shaking the sample for 5 minutes using a standard sieve, the ratio of the particle group of each particle size is measured from the weight fraction based on the size of the sieve opening.

In the composition of the detergent particle group I, the surfactant is preferably 5 to 80% by weight, more preferably 10 to 60% by weight, particularly preferably 15 to 40% by weight. The amount of the soil release agent is preferably 0.05 to 15% by weight, more preferably 0.1 to 10% by weight, particularly preferably 0.3 to 5% by weight. The content of the water-insoluble inorganic substance is preferably 5 to 50% by weight, more preferably 10 to 45% by weight, and particularly preferably 15 to 40% by weight. Of the water-soluble components, the water-soluble polymer is preferably 1 to 30% by weight, more preferably 1 to 30% by weight.
-20% by weight, particularly preferably 1-15% by weight.
The water-soluble salts are preferably 2 to 40% by weight, more preferably 5 to 35% by weight, and particularly preferably 10 to 30% by weight.
% By weight.

In the detergent particle group I, for example, the main component excluding a part of the water-insoluble inorganic substance is kneaded and mixed using a continuous kneader, and the obtained kneaded substance and the remaining water-insoluble inorganic substance are pulverized. It can be obtained by putting it in a machine. Then, by sieving this, a detergent particle group having a predetermined average particle size distribution can be obtained. Preferred examples of the continuous kneader include "KRC2 type" manufactured by Kurimoto Iron Works, and "DKASO6 type" manufactured by Hosokawa Micron as a pulverizer.

In another embodiment, the high bulk density detergent particles comprise a base containing a soil release agent and a water-insoluble inorganic substance, and at least one water-soluble component selected from the group consisting of a water-soluble polymer and a water-soluble salt. A high bulk density detergent particle group in which a surfactant is supported on the granule group (detergent particle group II) is exemplified. The average particle size of the detergent particle group II is preferably from 150 to 600 μm, more preferably from 150 to 500 μm, particularly from the viewpoint of preventing dissolution delay due to the paste formation of the detergent particle group and the solubility of the detergent particle group II itself. Preferably 180
４００400 μm.

In the composition of the base granules, the soil release agent is preferably 0.08 to 22% by weight, more preferably 0.1 to 1% by weight.
The content is 5% by weight, particularly preferably 0.3 to 8% by weight, and the content of the water-insoluble inorganic substance is preferably 20 to 90% by weight, more preferably 30 to 75% by weight, particularly preferably 40 to 70% by weight. Among the water-soluble components, the water-soluble polymer is preferably 2
-30% by weight, more preferably 3-20% by weight, particularly preferably 5-20% by weight. The water-soluble salts are preferably 5-77% by weight, more preferably 10-66% by weight,
Particularly preferably, the content is 20 to 54% by weight.

The structure of the base granule is more preferably a structure in which the water-soluble polymer and / or water-soluble salts are more unevenly distributed near the surface than inside the base granule. Such base granules exhibit a dissolution behavior in which the water-soluble components near the surface are rapidly dissolved in water, thereby promoting the disintegration of the detergent particles II from the surface of the detergent particles II. Therefore, high-speed solubility is realized by such base granules, and detergent particles II having excellent solubility can be obtained. In particular, by blending and supporting an anionic surfactant in the base particles, a large amount of surfactant can be blended while maintaining uneven distribution. Water-soluble polymer in the base granules and / or
Alternatively, the uneven distribution of the water-soluble salts can be confirmed by, for example, Fourier transform infrared spectroscopy (FT-IR) or photoacoustic spectroscopy (PAS)
(FT-IR / PAS). This is APPLIED SPECTROSCOPY vol.47,
As described in 1311-1316 (1993), this is a method for analyzing the distribution state of a substance in the depth direction from the surface of a base granule.

The amount of the surfactant to be carried on the base particles is preferably 5 to 80 parts by weight, more preferably 5 to 60 parts by weight, based on 100 parts by weight of the base particles, in terms of detergency. To 60 parts by weight, more preferably 20 parts by weight.
-60 parts by weight are particularly preferred.

Such a detergent particle group II can be prepared, for example, as follows. First, a slurry containing the components constituting the base granules is prepared. Next, the slurry is subjected to spray drying to obtain a base granule group.
By spray drying, the water-soluble components of the components constituting the base granules move to the surface of the base granules with the evaporation of water, and the base granules exhibit uneven distribution. Next, the obtained base granules and the surfactant are charged into a batch type or continuous mixer to allow the base particles to carry the surfactant.

Further, from the viewpoints of the fluidity and non-caking properties of the detergent particles I and II, the surface modification may be performed by mixing the detergent particles I and II with a surface coating agent. As the surface coating agent, for example, aluminosilicate, calcium silicate, silicon dioxide, bentonite,
Silicate compounds such as talc, clay, amorphous silica derivatives and crystalline silicate compounds, fine powders such as metal soaps and powdered surfactants, carboxymethylcellulose, polyethylene glycol, sodium polyacrylate, copolymers of acrylic acid and maleic acid Or a water-soluble polymer such as a polycarboxylate such as a salt thereof, and a fatty acid.

Next, the components constituting the high bulk density detergent particles will be described. In the present invention, the soil release agent is used to treat a cloth or the like in advance by using this agent to repel the dirt and make it difficult to adhere, or to peel off from the cloth or the like together with the adhered dirt to enhance the cleaning effect. An agent that can be used.

As the soil release agent, one or more selected from polyamines, polyalkylimine derivatives, polyoxyalkylene terephthalates, polyalkylene terephthalates and copolymers thereof are preferably used. From the viewpoints of effect and detergency, polyamine and polyethylene terephthalate-polyoxyethylene terephthalate are preferred.

The polyamine is represented by the formula (1):

[0020]

Embedded image

(Wherein R is a hydrocarbon group having 10 to 22 carbon atoms, R ¹ may be the same or different, and represents a hydrogen atom,-
_{(CH 2 CH 2 O) a} -H, - (CH 2 CH (CH 3)
O) _b -H (a and b are numbers from 1 to 20), R ² is a hydrogen atom, an alkyl group having 1 to 4 carbon atoms or (R ¹ ) _y H
Wherein x, y and z are integers whose sum is in the range of 2 to 25, n is an integer of 1 to 6, and m is an integer of 1 to 9).

In the formula (1), R is a tallowalkyl
Group, coconut alkyl group, palm core alkyl group, par
Alkyl, lauryl, palmityl, stearyl
Or oleyl groups are preferred. R¹Is-(CH_TwoCH
_TwoO)_a-H is preferred. R ^TwoIs an alkyl having 1 to 4 carbon atoms
Kill group (especially methyl group, ethyl group),-(CH_TwoCH
(CH_Three) O)_b-H is preferable (a and b are 3 to 15)
Is the number of ). n is preferably 2 to 4, and 2 or 3 is preferably
More preferred. m is preferably 1 to 3, more preferably 1 or 2.
Is more preferable. x, y and z are 1 to 4 respectively.
It is preferable that the total is 3 to 12.

[0023] As polyalkyl imine derivative of the formula ^{(2): Y- (R 3} NR 4) a - (R 5 NR 6) b -R 7 X (2) ( wherein, a is an integer from 1 to 10 , B is an integer of 0 to 20, X
And Y are each independently a hydrogen atom, —N (R ⁸ )
(R ⁹ ) or a hydroxyl group, R ⁸ and R ⁹ are each independently a hydrogen atom, a hydrocarbon group having 1 to 20 carbon atoms, and R ³ , R ⁵ and R ⁷ are each independently an alkylene having 1 to 6 carbon atoms. The groups R ⁴ and R ⁶ are hydrogen, — (R ¹⁰ O) _pH or —
R ¹¹ N (R ¹² ) (R ¹³ ), R ¹⁰ is an alkylene group having 2 or 3 carbon atoms, p is an integer of 1 to 20, and R ¹¹ is 1 to 2 carbon atoms.
6, an alkylene group, R ¹² and R ¹³ are each independently a hydrogen atom, —CH ₂ CH ₂ NH ₂ or a cyclic structure in which R ¹² and R ¹³ are taken together:

[0024]

Embedded image

R ¹⁴ is a hydrogen atom,-(R ^10-
O) H, an alkyl group having 1 to 12 carbon atoms, R ⁶ represents a hydrogen atom or —R ¹⁵ NH ₂ , and R ¹⁵ represents an alkylene group having 2 or 3 carbon atoms).

In the formula (2), a is preferably 1 or 2. b is preferably 1 to 4. , R ³ , R ⁵ and R ⁷
Is preferably 1 to 3, respectively.

The average molecular weight of the polyalkylimine derivative is preferably less than 1,000, more preferably 100
-600, more preferably 200-400. Further, a low molecular weight polyethyleneimine polymer is preferred.

The weight average molecular weight of polyoxyalkylene terephthalate, polyalkylene terephthalate or a copolymer thereof is preferably 15,000 to 50,000,
19000-43000 is more preferable, and 19000-
25000 is more preferred. Specifically, polyoxyethylene terephthalate, polyethylene terephthalate or a copolymer thereof is preferable, and a copolymer is particularly preferable. The molar ratio of polyoxyethylene terephthalate to polyethylene terephthalate in this copolymer is preferably from 1: 3 to 1: 6, more preferably from 1: 3 to 1: 5, even more preferably from 1: 3 to 1: 4.

As the water-insoluble inorganic substance, those having an average primary particle size of 0.1 to 20 μm are preferable. For example, crystalline or amorphous aluminosilicate, silicon dioxide,
Examples include hydrated silicate compounds, clay compounds such as zeolite, perlite, and bentonite. Among them, crystalline aluminosilicate is preferable in terms of sequestering ability and oil absorbing ability of a surfactant. Examples of the water-soluble polymer include a carboxylic acid polymer, carboxymethyl cellulose, soluble starch, and saccharides. Among them, sequestering ability,
In terms of dispersing ability of solid dirt and particle dirt and prevention of re-contamination,
Carboxylic acid-based polymers having a molecular weight of several thousands to 100,000 are preferred. Particularly, a salt of an acrylic acid-maleic acid copolymer and a polyacrylate are preferred. Examples of the water-soluble salts include water-soluble inorganic salts such as carbonates, bicarbonates, sulfates, sulfites, hydrogensulfates, hydrochlorides, and phosphates, and water-soluble organic acids such as citrates and fumarate salts. Salts. The incorporation of the water-soluble salts allows the bubbles generated from the detergent particles to thermally expand by the heat of hydration and heat of dissolution generated by the reaction between the water-soluble salts and water, thereby promoting the disintegration of the particles. It is more preferable in this respect.

The surfactant is at least one selected from anionic surfactants, nonionic surfactants, amphoteric surfactants and cationic surfactants. Examples of the anionic surfactant include a sulfate of a higher alcohol, a sulfate of an ethoxylated higher alcohol, an alkylbenzene sulfonate, a paraffin sulfonate, α
-Olefin sulfonate, α-sulfo fatty acid salt or its ester salt, or fatty acid salt. In particular,
The alkyl chain has 10 to 18 carbon atoms, more preferably 1 to
A linear alkylbenzene sulfonate having 2 to 14 carbon atoms and an α-sulfofatty acid alkyl ester salt having 10 to 20 carbon atoms are preferred. As the counter ion, an alkali metal ion is preferable from the viewpoint of improving the detergency. In particular, from the viewpoint of improving the dissolution rate, potassium ions are preferable, and potassium ions in all the counter ions are preferably 5% by weight or more, more preferably 20% by weight or more, and particularly preferably 40% by weight or more.

Examples of the nonionic surfactant include an ethylene oxide (hereinafter referred to as EO) adduct of a higher alcohol,
Or EO / propylene oxide adducts, fatty acid alkanolamides, alkyl polyglycosides, and the like. Particularly, EO1 to EO of alcohol having 10 to 16 carbon atoms.
A 0-mol adduct is preferred in terms of removing sebum stains, hard water resistance, biodegradability, and compatibility with linear alkylbenzene sulfonates. Examples of the cationic surfactant include long-chain alkyltrimethylammonium salts, and examples of the amphoteric surfactant include carbobetaine-type and sulfobetaine-type surfactants.

The high bulk density detergent particles include bleaching agents (percarbonates, perborates, bleaching activators, etc.), enzymes, anti-redeposition agents (carboxymethyl cellulose, etc.), softening agents, reducing agents ( Sulfites, etc.), fluorescent dyes, foam inhibitors (silicone, etc.), fragrances and the like can be appropriately contained. Further, the water content of the high bulk density detergent particles is preferably 20% by weight or less, more preferably 10% by weight or less in the detergent particles. The content of the detergent particles is preferably 60 to 100% by weight, more preferably 70 to 100% by weight in the detergent composition,
70-99% by weight is more preferred.

Examples of the enzyme include protease, amylase, pectinase, lipase, cellulase and the like, and a combination of protease and cellulase is particularly preferable.

[0034] High bulk density detergent particles containing a surfactant and a soil release agent, which are highly soluble to the extent specified in the present invention, have not been heretofore known and, of course, such detergent particles. There was no known way to get the group. However, as described in the present specification, a method of sieving the obtained detergent particles to a predetermined degree or a method of spray-drying a slurry in which a specific component is present has a high solubility in the detergent particles. Can be obtained. For this reason, the action of the stain release agent can be sufficiently exerted from an approach that has not been conventionally used, and the effect of improving the detergency is exhibited.

The detergent composition of the present invention is excellent in solubility and detergency, has a high dirt-removing effect, can be fashionably washed with low stirring power, and has a low to medium bath ratio (bath ratio = wash water amount (L)). / Washing in laundry (kg)), especially at low water temperature, and hand washing, pickling and so on.

[0036]

EXAMPLES 1 amine to the flask in Synthesis Example 1 <polyamine> 1L volume with alkyl composition derived from palm kernel oil (R-NH _2; molecular weight 200.95) 20
0 g was added and the temperature was raised to 70 ° C. 52.8 g of acrylonitrile (molecular weight 53.1) was dropped from the dropping funnel over about 1 hour. Then, it was aged at 70 ° C. for 1 hour and cooled. Next, the whole reaction product, 2 g of Raney nickel and 10 g of water were put into a 0.5 L stainless steel autoclave, and after sealing, oxygen in the autoclave was replaced with hydrogen.
The pressure was raised to 120 ° C. by applying pressure to hydrogen to 20 kg / cm ² . While maintaining the hydrogen pressure at 20 kg / cm ² , about 4
The reaction was performed for an hour, and the mixture was cooled. Thereafter, the reaction product is distilled to obtain a polyamine precursor (formula: R—NH—C ₃ H ₆ —N
H ₂₎ was obtained. The yield was 89% and the purity was 94.7% (gas chromatography, area%). Next, 1 part of the polyamine precursor was placed in a 1 L stainless steel autoclave.
After adding 00 g and sealing, oxygen in the autoclave was replaced with nitrogen, and the temperature was raised to 105 ° C. Thereafter, 76.7 g of ethylene oxide was injected over about 1 hour,
Aged at 105 ° C for hours. After cooling, the mixture was extracted with an aqueous alkaline solution having a pH of 10 and hexane, hexane was distilled off from the hexane phase, and the desired polyamine [formula: RN (C ₂ H
₄ OH) -C ₃ was obtained _{H 6 -N (C 2 H 4} OH) 2 ].
The yield was 71% and the purity was 89.2% (measured by high performance liquid chromatography).

Synthesis Example 2 <Polyethylene terephthalate-
Polyoxyethylene terephthalate> Polyethylene terephthalate-polyoxyethylene terephthalate was synthesized such that the molar ratio between polyethylene terephthalate having an average molecular weight of 2200 and polyoxyethylene terephthalate was 3: 1.

Synthesis Example 3 <Polyalkylimine derivative> 21.4 g of diethyl sulfate (0.13 g) was placed in a 2 L flask.
9 mol) and 98.8 g (1.39 mol) of 2-oxazoline were dissolved in 700 g of dehydrated ethyl acetate, and the mixture was refluxed for 5 hours under a nitrogen atmosphere. Next, 444 g (1.11 mol) of a 50% ethyl acetate solution of a primary amine (R-NH ₂ ) having an alkyl composition derived from palm kernel oil was added, and the mixture was refluxed with heating for 10 hours, and then ethyl acetate in the reaction mixture was removed. The solvent was distilled off under reduced pressure. Next, 400 g of the obtained compound was dissolved in 4 L of a 10% aqueous sodium hydroxide solution and reacted at 98 ° C. for 3 hours while heating and mixing. After cooling, the mixture was extracted with hexane, the hexane layer was concentrated, and the unreacted primary amine was distilled off under reduced pressure to obtain a polyalkylimine derivative [R-NH- (C
₂ H ₄ NH) _n -H]. Average degree of polymerization 9.5 mol,
The yield was 78%.

Example 1 [Method for producing detergent composition] 528 kg of water was added to a 1 m ³ mixing tank having stirring blades.
After the water temperature reaches 55 ° C., 40% by weight of acrylic acid
60 kg of a maleic acid copolymer aqueous solution was added. After stirring for 15 minutes, 36 kg of polyamine, 120 kg of sodium carbonate, 108 kg of sodium sulfate, 9 kg of sodium sulfite, and 3 kg of fluorescent dye were added. After stirring for a further 15 minutes, 264 kg of zeolite were added. The mixture was stirred for 30 minutes to obtain a slurry. The final temperature of the slurry was 60 ° C. This slurry was supplied to a spray drying tower, and spraying was performed from the top of the tower at a spray pressure of 25 kg / cm ² to prepare a base granule group. When the uneven distribution of the structure of the base granules was confirmed, the water-soluble polymer and the water-soluble salts were present in large amounts on the surface of the base granules and were unevenly distributed. The composition of the obtained base granules is as follows. Acrylic acid-maleic acid copolymer 4% by weight, polyamine of Synthesis Example 1 6% by weight, sodium carbonate 20% by weight, sodium sulfate 18% by weight, sodium sulfite 1.
5% by weight, 0.5% by weight of fluorescent dye, 44% by weight of zeolite, 6% by weight of water.

The acrylic acid-maleic acid copolymer was a sodium salt (70 mol% neutralized), and the monomer ratio was acrylic acid / maleic acid = 3/7 (molar ratio).
"Tinopearl CBS-X" (manufactured by Ciba Geigy) was used as the fluorescent dye. As the zeolite, 4A type zeolite (manufactured by Tosoh Corporation, average particle size: 3 μm) was used.

Next, a detergent particle group was obtained by adding a surfactant and the like to the base particle group. That is, a nonionic surfactant, an anionic surfactant acid precursor, polyethylene glycol, and an alkaline aqueous solution were heated and mixed at 70 ° C.
Activator mixture was obtained. The composition is as follows. 100 parts by weight of a base granule group, 22 parts by weight of a nonionic surfactant, 22 parts by weight of an anionic surfactant, 2 parts by weight of polyethylene glycol, and 5 parts by weight of water.

Next, a Ladyge mixer (Matsusaka Giken Co., Ltd.)
(With a jacket and a capacity of 20 L) and 100 parts by weight of the above-mentioned base granules were charged, and stirring of the main shaft (150 rpm) was started. The above-mentioned mixture of the activators was added thereto for 3 minutes, and then stirred for 5 minutes to obtain a detergent particle group. Further, 8 parts by weight of the crystalline silicate and 6 parts by weight of the amorphous aluminosilicate were charged into the mixer to coat the surface of the detergent particles. As the nonionic surfactant, a polyoxyethylene alkyl ether having 12 to 16 carbon atoms and an average number of moles of added EO of 7.0 was used. As the anionic surfactant, sodium dodecylbenzenesulfonate was used.
Polyethylene glycol having an average molecular weight of 8,500 was used. The crystalline silicate powder “SKS-6” (crushed by Clariant Tokuyama Co., Ltd., average particle size 50 μm)
Was used. Amorphous aluminosilicate has Al ₂ O ₃ =
29.6% by weight, SiO ₂ = 52.4% by weight, Na ₂ O
= 18.0% by weight (1.0 Na ₂ O.Al ₂ O ₃ .3.
1SiO ₂ ) (based on atomic absorption analysis and plasma emission analysis). The oil absorption capacity is 285
mL / 100 g, water content 11.2% by weight.

Next, the detergent particles were classified using a sieve having an opening of 1000 μm to obtain high bulk density detergent particles having a particle size of less than 1000 μm. 1.5 parts by weight of an enzyme and 0.5 parts by weight of a fragrance were mixed with 100 parts by weight of the obtained detergent particles to obtain a detergent composition. The enzyme was cellulase K (JP-A-63
And lipolase 100T (manufactured by Novo) at a weight ratio of 3: 1.

Example 2 [Method for producing detergent composition] The detergent particles shown in Table 1 were produced by the following method. An aqueous slurry having a water content of 50% is prepared using components other than a part of zeolite (17% by weight), enzymes, flavors, crystalline silicate and amorphous aluminosilicate, and spray-drying is performed. Next, granulation is performed by a screw extrusion granulator to obtain a detergent particle group. The detergent particles were classified with a classifier to a size of 710 μm or more, pulverized with a pulverizer together with a part of zeolite (for 3% by weight), and mixed with the detergent particles having a size of less than 710 μm classified by the classifier. Next, the granulated and pulverized particles were placed in a rotary kiln, a part of zeolite (for 3% by weight), an enzyme, and a crystalline silicate were blended, and simultaneously a fragrance was sprayed to obtain a detergent composition. The polyethylene terephthalate-polyoxyethylene terephthalate obtained in Synthesis Example 2 was used.

Example 3 A detergent composition 3 was obtained in the same manner as in Example 2 except that polyethylene terephthalate-polyoxyethylene terephthalate was replaced with the polyalkylimine derivative of Synthesis Example 3.

Comparative Example 1 Example 2 except that sodium sulfate was used instead of polyethylene terephthalate-polyoxyethylene terephthalate.
As above, a detergent composition was obtained.

Comparative Example 2 The same composition as in Example 2 was used, but the classification and pulverization conditions were changed.
Was changed under different conditions) to obtain a detergent composition.

[0048]

[Table 1]

Table 2 shows the physical properties, 95% dissolution time, and stain release effect of the detergent compositions obtained in Examples 1 to 3 and Comparative Examples 1 and 2. Further, the stain release effect of these detergent compositions was evaluated based on the following method.

<Evaluation of Soil Removal Effect> (1) Preparation of Soiled Cloth A 10 × 10 cm blended cloth [polyester / cotton = 50 /
50 (weight ratio)] at 10 ° C with a targotometer.
After adding 0.6 g of detergent in 1 L of 4 ° DH hard water,
Stir and wash at 100 rpm for 0 minutes. Next, after removing water sufficiently by centrifugation in a centrifugal dehydrator, 10 g
Rinse with 1 L of 4 ° DH hard water at 100 ° C. for 10 minutes. The main rinsing process is repeated twice. Then, after centrifugal dehydrator to remove water sufficiently, 25 ° C, 50% RH
Dry for 1 hour or more in the room. The main washing and rinsing treatment was repeated three times. Next, 60% cottonseed oil, 10% cholesterol, 10% oleic acid, 1 palmitic acid
A sebum soiled cloth was prepared by uniformly applying 2 g of a model sebum soil composed of 0% by weight and 10% by weight of solid paraffin per mixed spinning cloth.

(2) Washing evaluation method Five blended fabrics prepared according to the above method were stirred at 100 rpm for 10 minutes after adding 0.6 g of detergent in 1 L of 4 ° DH hard water at 10 ° C. using a tergotometer. Washed. Next, the mixture was centrifugally dehydrated to sufficiently remove water.
Stirring was performed at rpm. The main rinsing process was repeated twice. Next, after removing water sufficiently with a centrifugal dehydrator,
An iron press treatment was performed. Next, the reflectance at 460 nm of the mixed spinning cloth before the washing treatment, the stained cloth adjusted after the repeated washing, and the stained cloth after the final washing were measured with a self-recording colorimeter (manufactured by Shimadzu Corporation). %) Was calculated. Table 2 shows the average values of the cleaning rates of the five blended fabrics.

Cleaning rate (%) = [(reflectance after final cleaning−
Reflectance after adjustment of stained cloth) / (Reflectance of original cloth−reflectance after adjustment of stained cloth)] × 100

[0053]

[Table 2]

From the results shown in Table 2, the detergent compositions obtained in Examples 1 and 2 have a short dissolution time of 95%, and Comparative Examples 1 and 2
It can be seen that, compared to the detergent composition obtained in 2, the cleaning rate is high and the stain removing effect is high.

[0055]

According to the present invention, it is possible to obtain a detergent composition which is excellent in solubility and detergency, and has a high soil-removing effect.

 ──────────────────────────────────────────────────の Continuing on the front page (72) Inventor Hiroshi Nishimura 1334 Minato, Wakayama-shi F-term in Kao Corporation Research Laboratory 4H003 AB18 AC08 BA10 CA20 DA01 EA12 EA16 EA25 EA28 EB12 EB13 EB32 EB36 EB38 EC01 EC03 ED02 FA04 FA32

Claims (4)

[Claims] 1. A high bulk density detergent particle group containing a surfactant and a soil release agent, wherein the 95% dissolution time at 10 ° C. by an electric conductivity method is 120 seconds or less. A detergent composition comprising: 2. The high bulk density detergent particles have an average particle size of 150
５００500 μm, bulk density 500 g / L or more,
Particles having a particle diameter of 0 μm or more and particles having a particle diameter of less than 125 μm each account for 10% by weight of the entire high bulk density detergent particles.
The detergent composition according to claim 1, which is: 3. The high bulk density detergent particles have an average particle size of 150.
-600 μm, bulk density of 500 g / L or more, and surfactant on a base particle group comprising a soil release agent and a water-insoluble inorganic substance and at least one water-soluble component selected from a water-soluble polymer and a water-soluble salt. The detergent composition according to claim 1, further comprising an agent. 4. A soil release agent comprising a polyamine, a polyalkylimine derivative, a polyoxyalkylene terephthalate,
The detergent composition according to any one of claims 1 to 3, wherein the detergent composition is at least one selected from polyalkylene terephthalates and copolymers thereof.