WO2011074522A1 - Process for producing detergent particles - Google Patents

Abstract

Disclosed is a process for producing detergent particles which comprises the step (B) of mixing an anionic-surfactant paste with an alkyl glyceryl ether to prepare an anionic-surfactant composition and the step (C) of mixing the anionic-surfactant composition prepared in the step (B) with base granules having an oil absorption of 0.2 mL/g or more to prepare the detergent particles. Use of the process produces the effect that detergent particles which are inhibited from agglomerating and have a narrow particle diameter distribution, high solubility, and a high cleaning effect can be produced without requiring a drying step for water removal after the anionic-surfactant composition is mixed with the base granules having an oil absorption of 0.2 mL/g or more. By inhibiting particle agglomeration and imparting a narrow particle size distribution, a detergent having not only an improved appearance but also excellent solubility can be obtained. Furthermore, the content of coarse particles in the detergent particles to be produced can be made low regardless of differences in the content of coarse particles in the base granules.

Description

Method for producing detergent particles

The present invention relates to a method for producing a detergent particle group and a detergent particle group obtained by the production method.

One method for producing detergent particles includes a method of mixing a powdery substance and a liquid surfactant composition. Among them, various methods for using an anionic surfactant in a paste state have been disclosed so far.

For example, Patent Document 1 discloses a method for producing a granular detergent composition in which an alkyl ether sulfate paste is made to absorb oil in silica or silicate, and is granulated and dried. Although such a production method has an advantage that a high amount of an anionic surfactant can be incorporated, in order to facilitate the production of such a granular detergent composition, silica or silicate can be used. An oil-absorbing carrier is required, and further, a drying step is required after the granulation step in order to remove moisture contained in the paste.

Patent Document 2 discloses a production method in which surface modification is performed by mixing a base granule produced by spray-drying and containing a water-soluble inorganic salt and having a support capacity of 20 mL / 100 g or more and an alkyl sulfate paste. Has been. However, in the case of such a production method, there are many aggregates, and dissatisfaction remains from the viewpoint of particle growth. Moreover, although this subject was improved by adding polyoxyethylene alkyl ether, it was necessary to mix in a large amount, and dissatisfaction remained from the viewpoint of composition flexibility.

International Publication No.0031223 Pamphlet JP 2006-137925 A

That is, the present invention
[1] Next step:
Step (B): A step of preparing an anionic surfactant composition by mixing an anionic surfactant paste and an alkyl glyceryl ether, and Step (C): an anionic surfactant composition prepared in the step (B). And a step of preparing a detergent particle group by mixing a base granule group having an oil absorption capacity of 0.2 mL / g or more,
And [2] a detergent particle group obtained by the production method according to [1] above.

The present invention does not require a drying step even when a surfactant composition having a high water content is used, has a particle size distribution that is sharp, has a sharp particle size distribution, and has good powder properties such as solubility. It relates to a manufacturing method.

By using the method for producing detergent particles according to the present invention, a drying step for removing moisture after mixing the anionic surfactant composition and the base granules having an oil absorption capacity of 0.2 mL / g or more is not required. In addition, it is possible to produce a detergent particle group in which particle growth is suppressed, the particle size distribution is sharp, the solubility is high, and the cleaning effect is high. By suppressing particle growth and sharpening the particle size distribution, it is possible to obtain a detergent that not only improves the appearance but also has excellent solubility. Furthermore, regardless of the difference in the coarse particle ratio of the base granule group, the coarse particle ratio of the manufactured detergent particle group can be suppressed.

The method for producing the detergent particle group of the present invention, as described above,
Step (B): a step of preparing an anionic surfactant composition by mixing an anionic surfactant paste and an alkyl glyceryl ether;
Step (C): a step of preparing a detergent particle group by mixing the anionic surfactant composition prepared in the step (B) and a base granule group having an oil absorption capacity of 0.2 mL / g or more,
One major feature is the inclusion of Hereinafter, the production method of the present invention will be described in more detail.

<Process (B)>
Step (B) is a step of preparing an anionic surfactant composition by mixing an anionic surfactant paste and an alkyl glyceryl ether. In this specification, an anionic surfactant paste is a mixture of an anionic surfactant and water. The content of water in the anionic surfactant paste is preferably 15 to 50% by weight, more preferably 25% to 45% by weight, and further preferably 25 to 40% by weight. In addition,% display of content of each component as described in this specification and a compounding quantity is weight% unless there is a prescription | regulation separately.

As the anionic surfactant used in this step, those generally used for garment detergents, vegetable / dishwashing detergents, hair / skin detergents, and the like can be used. For example, alkyl sulfate ester salt, polyoxyethylene alkyl sulfate ester salt, α-sulfo fatty acid ester salt, α-olefin sulfonate, alkyl or hydroxyalkyl ether carboxylate, N-acylated taurine, N-acylated methyl taurine N-acylated glycine, N-acylated aspartic acid, N-acylated sarcosine, N-acylated glutamic acid, higher fatty acid salt, alkylbenzene sulfonate, alkyl sulfate, monoalkyl phosphate ester salt, alkylamide ether sulfate Examples include ester salts, fatty acid monoglyceride sulfates, and alkyliminodicarboxylates. As such an anionic surfactant, one kind can be used alone, or a plurality of kinds can be used in combination.

Among such anionic surfactants, preferred anionic surfactants include alkyl sulfates, alkyl sulfate esters, α-sulfo fatty acid ester salts, α-olefin sulfonates, polyoxyethylene alkyl sulfate salts, and the like. . Alkyl sulfate is more preferable in that a remarkable effect can be obtained.

The content of the anionic surfactant in the anionic surfactant composition prepared in this step is preferably 40 to 80% by weight, more preferably 45 to 75% by weight, still more preferably 50 to 70% by weight. %.

The alkyl glyceryl ether used in this step has the following general formula (3):
R—OCH ₂ —CHOH—CH ₂ OH (3)
(Wherein R represents a linear or branched alkyl or alkenyl group having 1 to 24 carbon atoms, or a cycloalkyl group having 3 to 8 carbon atoms).

By using an anionic surfactant composition obtained by mixing this alkyl glyceryl ether and an anionic surfactant paste, it is possible to obtain a detergent particle group with less aggregates and small particle growth.

In the general formula (3), R is a linear or branched alkyl group or alkenyl group having 1 to 24 carbon atoms, or a cycloalkyl group having 3 to 8 carbon atoms. 18 alkyl groups are preferred, and alkyl groups having 8 to 12 carbon atoms are more preferred. Specifically, R is a straight chain such as hexyl, heptyl, octyl, nonyl, decyl, undecyl, dodecyl, tridecyl, tetradecyl, pentadecyl, hexadecyl, heptadecyl, octadecyl, etc. Chain alkyl group, 2-ethylhexyl group, 2-methylheptyl group, 2-methylnonyl group, 2-octyldecyl group, 3,5,5-trimethylhexyl group, isodecyl group, isostearyl group, etc. branched chain alkyl group, oleyl And an alkenyl group such as a group.

The blending amount of the alkyl glyceryl ether in this step is preferably 10 to 40 parts by weight, more preferably 15 to 40 parts by weight, and more preferably 20 to 40 parts by weight with respect to 100 parts by weight of the anionic surfactant in the anionic surfactant paste. Part is more preferred. From the viewpoint of the particle growth degree of the detergent particle group of the present invention, the blending amount is preferably 10 parts by weight or more, from the viewpoint of the effective amount of the anionic surfactant that can be supported on the base granule group and the cost of the alkyl glyceryl ether. The blending amount is preferably 40 parts by weight or less.

The anionic surfactant composition in this step can be prepared by mixing a predetermined amount of anionic surfactant paste and a predetermined amount of alkyl glyceryl ether. You may add components other than these components as needed.

The viscosity of the anionic surfactant composition in this step is not particularly limited, but the surfactant composition was measured with MCR300 (manufactured by PHYSICA Messtechnik GmbH) at a temperature of 50 ° C. and a shear rate of 10 [1 / s]. In this case, the range of 0.01 to 20 Pa · s is preferable and the range of 0.05 to 15 Pa · s is more preferable from the viewpoint of handling properties in the step of preparing the detergent particle group by mixing with the base granule group.

Specific operations for preparing the anionic surfactant composition include, for example, an operation of mixing a predetermined amount of an anionic surfactant paste and a predetermined amount of alkyl glyceryl ether. You may add and mix components other than these components as needed. As a mixer to be used, a mixer generally used in the detergent field can be used, and as a condition during mixing, a condition generally employed in the detergent field can be employed.

<Process (C)>
Step (C) is a step of preparing a detergent particle group by mixing the anionic surfactant composition prepared in the above step (B) and a base granule group having an oil absorption capacity of 0.2 mL / g or more. is there.

Examples of the base granule group used in the step (C) include a granule group capable of supporting a surfactant. More specifically, the following spray-dried base granule group (a) and non-spray-dried base granule group (b) can be mentioned.

[Preparation of spray-dried base granule group (a): Step (A-1)]
The spray-dried base granule group (a) is a granule group obtained by spray-drying a slurry containing a water-soluble inorganic salt. For example, the spray-dried base granule group (a) can be prepared by spray-drying a slurry containing the following components.

The water-soluble inorganic salt is not particularly limited, but for example, sodium carbonate, potassium carbonate, sodium sulfate, sodium sulfite and sodium chloride are preferable water-soluble inorganic salts. As such a water-soluble inorganic salt, one type can be used alone, or a plurality of types can be used in combination.

In addition to the water-soluble inorganic salt, the following components can be further used. For example, builders generally used in laundry detergents, for example, sequestering agents such as zeolite, citrate and sodium tripolyphosphate, and components having both sequestering ability and alkaline ability such as crystalline silicate And anti-staining agents such as acrylic acid polymer, acrylic acid maleic acid copolymer and carboxymethyl cellulose, and fluorescent brightening agents.

The amount of water in the slurry is not particularly limited, but, for example, 40 to 60% by weight of the slurry is preferable. The conditions for spray drying the slurry (temperature, spray drying apparatus, spraying method, drying method, etc.) may be any known condition and are not particularly limited. By adopting the above raw materials and conditions, a group of base granules having a predetermined oil absorption ability can be obtained.

(Physical properties of spray-dried base granule group (a))
The oil absorption capacity of the spray-dried base granule group (a) is preferably 0.2 mL / g or more, more preferably 0.3 mL / g or more. Moreover, as a preferable upper limit of oil absorption capacity, it is 0.7 mL / g or less. In this range, aggregation between the spray-dried base granule groups (a) is suppressed, which is suitable for suppressing particle growth of the particles in the detergent particle group. Therefore, the oil absorption capacity of the spray-dried base granule group (a) is preferably 0.2 to 0.7 mL / g, more preferably 0.3 to 0.7 mL / g, from the same viewpoint as described above.

The method for measuring the oil absorption capacity of the spray-dried base granule group (a) is as follows. 100 g of a sample (spray-dried base granule group (a)) is placed in a cylindrical mixing tank having an inner diameter of about 5 cm and a depth of about 15 cm equipped with a stirring blade inside. While stirring the stirring blade at 350 r / min, linseed oil at 25 ° C. is added at a rate of about 10 mL / min, and the change over time in the stirring power is measured. The amount of linseed oil input when the stirring power becomes the highest is the oil absorption capacity (mL / g).

The bulk density of the spray-dried base granule group (a) is preferably 200 to 1000 g / L, more preferably 300 to 1000 g / L, further preferably 400 to 1000 g / L, and more preferably 500 to 800 g / L. In the present specification, the bulk density of the spray-dried base granule group (a) is measured by the method defined in JIS K3362 unless otherwise specified.

The average particle size of the spray-dried base granule group (a) is preferably 140 to 600 μm, more preferably 150 to 500 μm, still more preferably 180 to 300 μm. In this specification, the average particle diameter of the detergent particle group, the base granule group, and the like is obtained as follows using a sieve specified in JIS Z 8801 unless otherwise specified.

For example, a 9-stage sieve and a saucer having openings of 2000 μm, 1400 μm, 1000 μm, 710 μm, 500 μm, 355 μm, 250 μm, 180 μm and 125 μm are prepared, and a low tap machine (Tanaka Chemical Machinery Co., Ltd., Tapping: 156 Times / minute, rolling: 290 times / minute). After sieving by shaking a 100 g sample for 10 minutes, the mass frequency under the pan and each sieve is integrated in the order of pan, 125 μm, 180 μm, 250 μm, 355 μm, 500 μm, 710 μm, 1000 μm, 1400 μm, 2000 μm. Go. When the opening of the first sieve with an integrated mass frequency of 50% or more is x _j μm, and the opening of the sieve smaller by one is x _{j + 1} μm, the distance from the tray to the x _j μm sieve When the mass frequency integration is Q _j % and the mass frequency integration from the saucer to the x _{j + 1} μm sieve is Q _{j + 1} %, the average particle size x _a is calculated by the equations (A) and (B). Can be sought.

The moisture content in the spray-dried base granule group (a) is measured by the following infrared moisture meter method. That is, 3 g of a sample (spray-dried base granule group (a)) is weighed on a sample pan of known weight, and the sample is heated and dried for 3 minutes with an infrared moisture meter (Infrared lamp 185W manufactured by Kett Science Laboratory Co., Ltd.). I do. After drying, weigh the sample pan and the dried sample. The difference between the weight of the sample pan and the sample obtained before and after drying obtained by such an operation is divided by the measured amount of the sample, and multiplied by 100 to calculate the amount (%) of moisture in the sample.

The content of the water-soluble inorganic salt in the spray-dried base granule group (a) is preferably 40 to 90% by weight of the granule group (a) from the viewpoint of washing performance and handling of the slurry before spray drying. More preferred is 50 to 90% by weight, and still more preferred is 55 to 90% by weight.

[Preparation of non-spray-dried base granule group (b): Step (A-2)]
Non-spray-dried base granule group (b) is granulated in a container rotary granulator by adding a binder to a detergent powder raw material having an oil absorption capacity of 0.4 mL / g or more using a multi-fluid nozzle. It is a granule group obtained by. Examples of the powder raw material for detergent include the following powder raw materials (referred to as “powder raw material (a)”).

Examples of the powder raw material (a) include soda ash (for example, light ash and dense ash) prepared by baking sodium bicarbonate, mirabilite, porous powder prepared by drying tripolyphosphate hydrate, clay mineral powder Etc. Light ash is preferable from the viewpoint of ease of handling and availability. As the powder raw material (a), one type of component may be used alone, or a plurality of types of components may be used in combination. The powder raw material (a) usually has fine pores of 10 μm or less inside, and a surfactant can be supported on the pores.

Examples of the clay mineral powder include talc, pyrophyllite, smectite (saponite, hectorite, saconite, stevensite, montmorillonite, beidellite, nontronite, etc.), vermiculite, mica (phlogopite, biotite, chinwald mica, muscovite. Mother, paragonite, ceradonite, sea chlorite, etc.), chlorite (clinochlore, chamosite, nimite, penantite, sudite, dombasite, etc.), brittle mica (clinentite, margarite, etc.), sulite, serpentine mineral (antigogo) Light, lizardite, chrysotile, amethyite, clonstedite, burcherin, greenerite, garnierite), kaolin minerals (kaolinite, dickite, nacrite, halloysite, etc.).

From the viewpoint of granulation, the average particle diameter of the powder raw material (a) excluding the clay mineral powder is preferably 10 to 250 μm, more preferably 50 to 200 μm, still more preferably 80 to 200 μm. The particle size of the clay mineral powder is preferably 10 to 100 μm, more preferably 50 μm or less, and more preferably 30 μm or less. From the viewpoint of solubility, the powder raw material (a) is preferably a water-soluble substance.

The oil absorption capacity of the powder raw material (a) used in this step is a value determined by the following evaluation method.

That is, 30 to 35 g of a sample (powder raw material (a)) is put into an absorption measuring device (A410 manufactured by Asahi Research Institute), and the driving blade is rotated at 200 r / m. A liquid nonion (Emulgen 108 manufactured by Kao Corporation) is dropped at a liquid supply rate of 4 mL / min to determine the point at which the maximum torque is obtained. The liquid addition amount at a point where the torque becomes 70% of the point where the maximum torque is reached is divided by the sample input amount to obtain the oil absorption capacity.

In addition, the upper limit of the oil absorption capacity of the powder raw material (a) is not particularly limited, but is preferably 1.0 mL / g or less, for example.

The content of the powder raw material (a) in the non-spray-dried base granule group (b) is preferably 40 to 95% by weight, more preferably 45 to 90% by weight of the granule group (b) from the viewpoint of oil absorption. 50 to 85% by weight is more preferable, and 50 to 80% by weight is more preferable.

The powder raw material (a) may be used alone as a powder raw material for detergent, or a plurality of types may be used.

In addition to the powder raw material (a), non-spray-dried base granule group (b) can be obtained using the following other components. Specific examples include builders generally used for garment detergents, anti-staining agents and fluorescent whitening agents mentioned in the description of the spray-dried base granule group (a).

As the granulation method used in this step, a method of granulating the detergent powder raw material and the binder with a container rotary granulator is employed. As the container rotating granulator, a drum type mixer or a pan type mixer is preferable. The drum-type mixer is not particularly limited as long as the drum-shaped cylinder rotates and performs processing. In addition to the drum-type mixer that is horizontally or slightly inclined, the conical drum-type granulator is used. (Mixer), multi-stage conical drum granulator (mixer), etc. can also be used. These apparatuses can be used in both batch and continuous processes.

Specific examples of the binder to be added include polyethylene glycol, polypropylene glycol, polyoxyethylene alkyl ether and derivatives thereof, polyvinyl alcohol and derivatives thereof, water-soluble cellulose derivatives (these derivatives include ether compounds and the like). ), Organic polymers such as carboxylic acid polymers, starches and saccharides, inorganic polymers such as amorphous silicates, higher fatty acids, alkylbenzene sulfonic acids, general interfaces as described in the well-known collection of conventional techniques Examples include activators. From the viewpoint of caking property and detergency, water-soluble cellulose derivatives, saccharides and carboxylic acid polymers are preferred, and acrylic acid-maleic acid copolymer salts and polyacrylates are more preferred. The salt is preferably a sodium salt, potassium salt or ammonium salt. The weight average molecular weight of the carboxylic acid polymer is preferably from 1,000 to 100,000, more preferably from 2,000 to 80,000.

The added binder may be an aqueous solution. The concentration when added as an aqueous solution is not particularly limited, but the particle size at the time of granulation of the non-spray-dried base granule group (b) is greatly influenced by the volume of the binder. What is necessary is just to determine a density | concentration from the particle size of a desired granule group. For example, the concentration of the binder component when added as an aqueous solution is preferably 20 to 80% by weight.

The binder is added using a multi-fluid nozzle. By using such a nozzle, the droplets of the binder can be made fine and dispersed. A multi-fluid nozzle is a nozzle that mixes and atomizes a liquid and atomizing gas (air, nitrogen, etc.) through an independent flow path to the vicinity of the nozzle tip. A fluid nozzle or the like can be used. Further, the mixing part of the binder and atomizing gas may be either an internal mixing type that mixes within the nozzle tip or an external mixing type that mixes outside the nozzle tip.

As such a multi-fluid nozzle, an internal mixed type two-fluid nozzle such as manufactured by Spraying Systems Japan Co., Ltd., manufactured by Kyoritsu Alloy Manufacturing Co., Ltd., or manufactured by Ikeuchi Co., Ltd., manufactured by Spraying Systems Japan Co., Ltd. And an external mixing type two-fluid nozzle manufactured by Kyoritsu Alloy Mfg. Co., Ltd. and Atmax Co., Ltd., an external mixing type four-fluid nozzle manufactured by Fujisaki Electric Co., Ltd., and the like.

For example, when a two-fluid nozzle is used, for example, it is preferable to supply the binder under the following conditions. The flow rate of the atomizing gas can be easily adjusted by adjusting the atomizing gas spray pressure. From the viewpoint of the dispersibility of the binder, the atomizing gas atomizing pressure is 0.1 MPa (gauge pressure). ) Or more is preferable, and 1.0 MPa (gauge pressure) or less is preferable from the viewpoint of equipment load. Moreover, there is no restriction | limiting in particular as the spraying pressure of a binder, However, 1.0 MPa or less is preferable from a viewpoint of equipment load, for example.

The content of the binder in the non-spray-dried base granule group (b) is preferably 1 to 50% by weight in the non-spray-dried base granule group (b) from the viewpoints of caking property and oil absorption capacity. % By weight is more preferred, 8 to 40% by weight is still more preferred, and 10 to 35% by weight is more preferred.

[Physical properties of non-spray dried base granule group (b)]
The non-spray-dried base granule group (b) is, for example, a group of granules having a structure in which the powder raw material (a) is gently aggregated. In that case, it has (1) a large gap between granules, and (2) a small gap of 10 μm or less in the powder raw material (a) and two supporting sites between layers. By adjusting these two loading sites, a non-spray-dried base granule group (b) having a desired oil absorption capacity can be obtained.

The oil absorption capacity of the non-spray dried base granule group (b) is 0.2 mL / g or more, preferably 0.3 mL / g or more, and more preferably 0.4 mL / g or more. On the other hand, the oil absorption capacity is preferably 0.7 mL / g or less. In such a range, aggregation of the non-spray-dried base granule group (b) is suppressed, which is preferable because the particle growth degree of the particles in the detergent particle group can be suppressed. Accordingly, the oil absorption capacity of the non-spray dried base granule group (b) is preferably 0.2 to 0.7 mL / g, more preferably 0.3 to 0.7 mL / g, from the same viewpoint as described above. The method for measuring the oil absorption capacity of the non-spray dried base granule group (b) is the same as the method for measuring the oil absorption capacity of the spray dried base granule group (a).

The bulk density of the non-spray-dried base granule group (b) is from 200 to 1000 g / from the viewpoint of securing the loading capacity of the surfactant composition and securing the high bulk density after loading the surfactant composition. L is preferable, 300 to 1000 g / L is more preferable, 400 to 550 g / L is still more preferable, and 400 to 500 g / L is still more preferable. In this specification, the method for measuring the bulk density of the non-spray-dried base granule group (b) is the same as the method for measuring the bulk density of the spray-dried base granule group (a).

The average particle size of the non-spray-dried base granule group (b) is preferably 140 to 600 μm, more preferably 150 to 500 μm, still more preferably 200 to 500 μm.

The water content in the non-spray-dried base granule group (b) is preferably 30% by weight or less, more preferably 20% by weight or less, and further preferably 15% by weight or less from the viewpoints of handling properties and oil absorption. The method for measuring the water content in the non-spray-dried base granule group (b) is the same as the method for measuring the water content in the spray-dried base granule group (a).

[Method for mixing anionic surfactant composition and base granule group]
The ratio of the two components when mixing the anionic surfactant composition and the base granule group is not particularly limited as long as it can be uniformly mixed. For example, the anionic surfactant composition with respect to 100 parts by weight of the base granule group The amount of the product is preferably 5 to 100 parts by weight, more preferably 10 to 90 parts by weight, further preferably 20 to 70 parts by weight, and more preferably 25 to 50 parts by weight. From the viewpoint of detergency, the anionic surfactant composition is preferably 5 parts by weight or more, more preferably 10 parts by weight or more, and 20 parts by weight or more with respect to 100 parts by weight of the granule group. Is more preferable, and it is still more preferable that it is 25 parts by weight or more. From the viewpoint of compositional freedom, solubility, etc., the anionic surfactant composition is preferably 100 parts by weight or less, more preferably 90 parts by weight or less, and more preferably 70 parts by weight with respect to 100 parts by weight of the granule group. More preferably, it is more preferably 50 parts by weight or less.

As the mixing condition in the step (C), a mixing condition that substantially maintains the morphology of the base granule group, that is, a mixing condition that does not cause the granule group to collapse may be selected. For example, when mixing a small amount, it may be mixed manually using a spatula or the like, or when using a mixer equipped with a stirring blade, from the viewpoint of suppressing the collapse of the base granules and the efficiency of mixing, When the shape of the mixing blade of the stirring blade provided in the paddle type is a paddle type, the fluid number of the stirring blade is preferably 0.5 to 8.0, more preferably 0.8 to 4.0, still more preferably 0. .5 to 2.0. When the shape of the mixing blade is a screw type, the fluid number of the stirring blade is preferably 0.1 to 4.0, more preferably 0.15 to 2.0. When the mixing blade has a ribbon shape, the fluid number of the stirring blade is preferably 0.05 to 4.0, more preferably 0.1 to 2.0.

Further, the fluid number defined in this specification is calculated by the following equation.
Fluid number = V ² / (R × g)
(Here, V represents the peripheral speed [m / s] of the tip of the stirring blade, R represents the rotational radius [m] of the stirring blade, and g represents the acceleration of gravity [m / s ² ].)

In step (C), powder raw materials other than the base granule group can be blended if desired. The blending amount is preferably 30 parts by weight or less with respect to 100 parts by weight of the base granule group from the viewpoint of solubility.

The powder raw material other than the base granule group referred to in this step means a powder cleaning strength enhancer or oil absorbent at room temperature. Specifically, bases showing sequestering ability such as zeolite and citrate, bases showing alkaline ability such as sodium carbonate and potassium carbonate, sequestering ability and alkaline ability such as crystalline silicate Examples thereof include bases having all of them, amorphous silica and amorphous aluminosilicate having a high sequestering ability but a low sequestering ability. By using this powder raw material in combination with the base granule group as desired, it is possible to achieve a high blending of the anionic surfactant composition and a reduction in the adhesion of the mixture into the mixer, and to improve the cleaning power. it can. As such a powder raw material, one type can be used alone, or a plurality of types can be used in combination.

After mixing the anionic surfactant composition and the base granule group, polyethylene glycol (PEG) and / or fatty acid and / or soapy water is preferably added in an amount of 1 to 10 parts by weight with respect to 100 parts by weight of the base granule group. The surface of the base granule group may be coated by mixing. This coating is preferred because the caking resistance of the detergent particles is improved. Furthermore, by adding PEG and / or fatty acid and / or soapy water, it becomes possible to suppress aggregation and enhance dispersibility when dissolving the detergent particles, resulting in improved solubility of the detergent particles. This is preferable.

The detergent particle group obtained by the present invention may contain a nonionic surfactant. The nonionic surfactant may be oil-absorbed and supported on the base granule group before and / or after the step (C), or may be mixed with the anionic surfactant composition used in the step (B) to form an anionic interface. Oil absorption and loading may be carried out simultaneously with the activator composition, but it is preferable to oil absorption and loading before the step (C) from the viewpoint of suppressing caking due to exudation of the nonionic surfactant. Moreover, as content in the detergent particle group of this nonionic surfactant, 20 weight% or less in a detergent particle group is preferable from a viewpoint of suppression of caking by oozing-out, and 15 weight% or less is more preferable. Moreover, 5 weight% or more is preferable from a viewpoint of detergency, and 10 weight% or more is more preferable.

The type of the nonionic surfactant is not particularly limited, and for example, the nonionic surfactant described in the well-known conventional technique collection (powder detergent for clothing) issued by the Japan Patent Office can be used.

Further, the temperature in the mixer during mixing is preferably a temperature at which the anionic surfactant composition and the base granule group can be efficiently mixed while substantially suppressing the collapse of the base granule group. For example, a temperature equal to or higher than the pour point of the anionic surfactant composition to be mixed is preferable, a temperature equal to or higher than 10 ° C. of the pour point is more preferable, and a temperature equal to or higher than 20 ° C. is more preferable. The mixing time during mixing is preferably about 2 to 20 minutes, more preferably about 2 to 10 minutes. The temperature in the mixer can be adjusted by flowing cold water or hot water through a jacket or the like. Therefore, the apparatus used for mixing preferably has a structure with a jacket.

The mixing method of the anionic surfactant composition and the base granule group may be a batch type or a continuous type. When mixing batchwise, it is preferable to add the anionic surfactant composition after previously charging the base granule group into the mixer. The temperature of the supplied anionic surfactant composition is preferably 70 ° C. or lower, more preferably 60 ° C. or lower, from the viewpoint of the stability of the anionic surfactant composition.

The mixer used for batch mixing is not particularly limited as long as it is a mixer generally used for batch mixing. For example, (1) the mixing blade shape is a paddle type mixer, A mixer with a stirring shaft attached to this shaft and mixing the powder by attaching a stirring blade to this shaft: Henschel mixer (Mitsui Miike Chemical Co., Ltd.), high speed mixer (Fukae Kogyo Co., Ltd.), Vertical granulator (Powrec Co., Ltd.), Redige mixer (Matsubo Co., Ltd.), Proshare mixer (Pacific Kiko Co., Ltd.), TSK-MTI mixer (Tsukishima Kikai Co., Ltd.), JP 10 -296064 and Japanese Patent Laid-Open No. 10-296065, etc. (2) As a mixer having a mixing blade shape of a ribbon type, a cylindrical, semi-cylindrical or conical type solid mixer is used. Mixer that mixes by rotating ribbon-shaped blades that form spirals in a container that has been formed: Ribbon mixer (manufactured by Hiwa Machine Industry Co., Ltd.), batch kneader (manufactured by Satake Chemical Machinery Co., Ltd.) , Ribocorn (manufactured by Daishun Seisakusho Co., Ltd.), Julia mixer (manufactured by Tokuju Kosakusho Co., Ltd.), etc. There are mixers that mix by revolving while rotating around an axis parallel to the wall of the wall: for example, Nauter mixer (manufactured by Hosokawa Micron Corporation), SV mixer (manufactured by Shinko Pantech Co., Ltd.), etc. .

In addition, when mixing in a continuous manner, it is not particularly limited as long as it is a continuous mixer generally used for continuous mixing, but for example, the base granule group using a continuous device among the above mixers. An anionic surfactant composition may be mixed.

<Surface modification>
It is desirable to further modify the surface of the detergent particles obtained in the step (C). By performing the surface modification, it is possible to obtain a detergent particle group having improved fluidity and caking resistance. When performing surface modification, it is preferable to use fine powder. When the fine powder is used, surface modification can be performed by mixing the detergent particles obtained in the step (C) and the fine powder under predetermined conditions.

The fine powder is not particularly limited, but has an average primary particle size of 20 μm or less in terms of improving the coverage of the detergent particles and improving the fluidity and caking resistance of the detergent particles. Is preferred. The average particle diameter is measured by a method using light scattering, for example, a particle analyzer (manufactured by Horiba, Ltd.) or microscopic observation.

Specific examples of the fine powder include inorganic fine powders such as silicate compounds such as crystalline silicate compounds, aluminosilicate, calcium silicate, silicon dioxide, bentonite, sodium tripolyphosphate, talc, clay, and amorphous silica derivatives. Body and metal soap with primary particles of 20 μm or less. As such a fine powder, one kind can be used alone, or a plurality of kinds can be used in combination. Furthermore, it is preferable in terms of detergency that the fine powder has high ion exchange ability and alkali ability. Among these, preferable fine powders include silicate compounds such as crystalline silicate compounds and aluminosilicates.

The amount of the fine powder used is preferably 0.5 to 40.0 parts by weight, more preferably 1 to 30 parts by weight, based on 100 parts by weight of the base granule group, from the viewpoint of fluidity and feeling of use.

As a mixing condition in the surface modification, a mixing condition capable of substantially maintaining the form of the base granule group carrying the anionic surfactant composition may be selected. For example, when mixing a small amount, it may be mixed manually using a spatula or the like, or it is preferable to use a mixer equipped with both a stirring blade and a crushing blade. In the case of using such a mixer, from the viewpoint of suppressing the collapse of the base granule group, the fluid number of the stirring blade provided in the machine is preferably 10 or less, more preferably 7 or less. From the viewpoint of efficiency of mixing with fine powder and dispersion with fine powder, the fluid number is preferably 2 or more, more preferably 3 or more. Furthermore, from the viewpoint of the efficiency of mixing with fine powder and dispersion of fine powder, the fluid number of the crushing blade is preferably 8000 or less, and more preferably 5000 or less. When the fluid number is within this range, a detergent particle group having excellent fluidity can be obtained.

As a preferable mixer in this step, among the mixers used in the step (C), those equipped with both a stirring blade and a crushing blade can be mentioned. Further, by performing the step (C) and the surface modification using different mixers, it is easy to adjust the temperature of the substance to be mixed. For example, when a non-heat resistant component such as a fragrance or an enzyme is added during or after the surface modification, it is preferable to adjust the temperature of the mixture when the surface modification is performed. Such temperature adjustment can be performed by setting the jacket temperature or venting. In order to transfer the detergent particles obtained in the step (C) to an apparatus for efficiently modifying the surface, it is also a preferable aspect that a part of the fine powder is added to the detergent particles at the end of the step (C). .

<Detergent particle group>
The detergent particle group of the present invention can be obtained by the production method of the present invention as described above.

[Physical properties of detergent particles]
In the present invention, the detergent particle group is not particularly limited, but is a detergent particle group produced using the base granule group as a core, and substantially one base granule in one detergent particle. A group of detergent particles having the characteristic of having as a core is preferred.

As an index representing such characteristics of the detergent particles, the following formula (1):
Particle growth degree = [average particle size of detergent particles] / [average particle size of base granules] (1)
Can be used. Specifically, a detergent particle group having a particle growth degree of 1.25 or less is preferable, one having 1.20 or less is more preferable, and one having 1.15 or less is more preferable. The lower limit of the degree of grain growth is not particularly limited, but is preferably 1.0 or more. Accordingly, the degree of particle growth is preferably 1.0 to 1.25, more preferably 1.0 to 1.20, and still more preferably 1.0 to 1.15 from the viewpoint of suppressing aggregation of the detergent particle group.

Since the detergent particles of the present invention are prevented from agglomerating between detergent particles, the amount of particles outside the desired particle size range (aggregated particles) is less, and the detergent particles have excellent solubility. And the particle size distribution of the detergent particles is sharp.

The average particle diameter of the detergent particle group of the present invention is preferably 150 μm or more, more preferably in the range of 150 to 500 μm, and still more preferably in the range of 180 to 350 μm.

In the present specification, the coarse particle ratio is defined by the weight percentage of the proportion of particles having a size of 500 μm or more in the base granule group or the detergent particle group. Specifically, the coarse particle ratio of the detergent particle group or the base granule group in the present invention is preferably 35% by weight or less, preferably 25% by weight or less, more preferably 15% by weight or less, and further preferably 10% by weight or less. Preferably, 5% by weight or less is even more preferable.

One of the features of the present invention is that the coarse particle ratio of the detergent particle group to be produced does not increase greatly even when the base granule group having a relatively high coarse particle ratio is used. This feature can be manifested by the “difference in the coarse particle rate of the detergent particles” defined below. In this specification, the increase in the coarse particle ratio of the detergent particle group is defined as the coarse particle ratio of the detergent particle group minus the coarse particle ratio of the base granule group. Specifically, the difference in increase in the coarse particle ratio of the detergent particle group of the present invention is preferably smaller, but is preferably 15% by weight or less, and more preferably 10% by weight or less.

The bulk density of the detergent particles is preferably 300 to 2000 g / L, more preferably 500 to 1500 g / L, and still more preferably 600 to 1000 g / L. The method for measuring the bulk density of the detergent particles is the same as the method for measuring the bulk density of the spray-dried base granules (a).

As described above, the detergent particle group obtained by the production method of the present invention having the above-described structure has a suppressed particle growth and a sharp particle size distribution, which improves not only the appearance but also the solubility. It is an excellent detergent particle group.

As the solubility index of the detergent particle group in the present invention, the dissolution rate of the detergent particle group for 60 seconds can be used. The dissolution rate for 60 seconds is preferably 80% or more, more preferably 90% or more.

The dissolution rate of the detergent particles for 60 seconds is calculated by the following method.
1 liter of hard water (Ca / Mg molar ratio 7/3) corresponding to 71.2 mg CaCO ₃ / liter cooled to 5 ° C. is a 1 liter beaker (inner diameter 105 mm, height 150 mm cylindrical type, for example, manufactured by Iwaki Glass Co., Ltd. 1 In a state where the water temperature of 5 ° C. is kept constant in a water bath, the stirring bar (length: 35 mm, diameter: 8 mm, for example, model: manufactured by ADVANTEC, trade name: Teflon (registered trademark)) In SA (round thin type)), stirring is performed at a rotational speed (800 r / m) at which the spiral depth with respect to the water depth is approximately 1/3. The detergent particles, which have been reduced and weighed to 1.000 ± 0.0010 g, are added and dispersed in water with stirring, and stirring is continued. 60 seconds after charging, the detergent particle group dispersion in the beaker is filtered through a standard sieve (diameter: 100 mm) having an opening of 74 μm as defined in JISZ8801 of known weight, and the water-containing detergent particle groups remaining on the sieve are collected together with the sieve. Collect in an open container of known weight. The operation time from the start of filtration until the sieve is collected is 10 ± 2 seconds. The collected residue of detergent particles is dried in an electric dryer heated to 105 ° C. for 1 hour, and then cooled in a desiccator (25 ° C.) containing silica gel for 30 minutes. After cooling, the total weight of the dissolved residue of the dried detergent, the sieve, and the collection container is measured, and the dissolution rate (%) of the detergent particle group is calculated by Equation (4).

Dissolution rate (%) = {1- (T / S)} × 100 (4)
S: input weight of detergent particles (g)
T: When the aqueous solution obtained under the above stirring conditions is subjected to the sieve, the dry weight (g) of the residue of the detergent particles remaining on the sieve

Moreover, the detergent particle group of the present invention is excellent in detergency. Unless otherwise specified, the following method is used as an index of detergency in the present specification.

(Preparation of artificially contaminated cloth)
An artificially contaminated cloth is prepared by attaching an artificially contaminated liquid having the following composition to the cloth. The artificial contamination liquid is attached to the cloth by printing the artificial contamination liquid on the cloth using a gravure roll coater. The process of making an artificially contaminated cloth by adhering an artificially contaminated liquid to the cloth is performed under the conditions of a gravure roll cell capacity of 58 cm ³ / cm ² , a coating speed of 1.0 m / min, a drying temperature of 100 ° C., and a drying time of 1 minute. Do. As the cloth, a cotton gold cloth 2003 cloth (manufactured by Tanigami Shoten) is used.

Artificial contamination liquid composition:
Lauric acid: 0.44% by weight
Myristic acid: 3.09% by weight
Pentadecanoic acid: 2.31% by weight
Palmitic acid: 6.18% by weight
Heptadecanoic acid: 0.44% by weight
Stearic acid: 1.57% by weight
Oleic acid: 7.75% by weight
Triolein: 13.06% by weight
N-hexadecyl palmitate: 2.18% by weight
Squalene: 6.53% by weight
Egg white lecithin liquid crystal: 1.94% by weight
Kanuma red soil: 8.11% by weight
Carbon black: 0.01% by weight
Tap water: Balance

(Cleaning conditions)
Using a tartometer, the rotation speed is 85 r / m, the washing time is 10 minutes, the temperature is 20 ° C., the water used is 4 ° DH (Ca / Mg = 3/1), and the concentration of the detergent particles is 0.0667 wt%. Do laundry. Usually, the hardness component of washing water is represented by Ca ²⁺ and Mg ²⁺ , and the weight ratio is about Ca / Mg = (60 to 85) / (40 to 15). Mg = 3/1 is used. 4 ° DH is the hardness when an equimolar amount of Mg ions is replaced by Ca.

(Calculation of cleaning rate)
The reflectance at 550 mμ before and after washing is measured with a self-recording color meter (manufactured by Shimadzu Corporation), and the washing rate D (%) is calculated by the following formula. The higher the cleaning rate, the better the detergent particles.
D = (L2-L1) / (L0-L1) × 100 (%)
L0: Reflection rate of raw cloth L1: Reflection rate of contaminated cloth before washing L2: Reflectivity of contaminated cloth after washing

The present invention will be further described based on the following examples. This example is merely illustrative of the invention and is not meant to be limiting in any way. In the following examples and the like, the following components were used unless otherwise specified.

Sodium polyacrylate: weight average molecular weight 10,000 (manufactured by Kao Corporation)
Zeolite: Zeobuilder (type 4A, manufactured by Zeobuilder: median diameter: 3.0 μm)
Clay mineral powder: Round rosyl DGA powder; Oil absorption capacity 0.44 mL / g (manufactured by Zude Chemi)
Light ash: average particle size 100 μm; oil absorption capacity 0.45 mL / g (manufactured by Central Glass Co., Ltd.)
Sodium alkyl sulfate: Alkyl group having C12: C14: C16 = 67: 28: 5 (weight ratio) Crystalline silicate: Pre-feed granule (manufactured by Tokuyama Siltech Co., Ltd.)
Polyoxyethylene alkyl ether: Emulgen 106KH (manufactured by Kao Corporation)

Production Example 1: Production of spray-dried base granule group (a) The spray-dried base granule group (a) was produced by the following procedure.
<Process (A-1)>
405 kg of water was added to a 1 m ³ mixing tank equipped with a stirring blade, and after the water temperature reached 55 ° C., 110 kg of sodium sulfate, 123 kg of sodium carbonate, and 4.4 kg of sodium sulfite were added to this mixing tank. After stirring for 10 minutes, 137 kg of 40% by weight aqueous sodium polyacrylate was added to the mixing vessel. After further stirring for 10 minutes, 37 kg of sodium chloride and 120 kg of zeolite were added to this mixing tank, and further stirred for 30 minutes to obtain a homogeneous slurry. The final temperature of this slurry was 58 ° C.

The slurry was sprayed at a spray pressure of 2.5 MPa from a pressure spray nozzle installed near the top of the spray-drying tower to produce a spray-dried base granule group (a). The hot gas supplied to the spray-drying tower was supplied at a temperature of 235 ° C. from the bottom of the tower and discharged at 119 ° C. from the top of the tower. The water content of the obtained spray-dried base granule group (a) was 0.15% by weight.

The physical properties of the resulting spray-dried base granule group (a) were an average particle size of 257 μm, a bulk density of 538 g / L, a coarse particle ratio of 0.2% by weight, and an oil absorption capacity of 0.45 mL / g.

Production Example 2: Production of non-spray-dried base granule group (b-1) A non-spray-dried base granule group (b-1) was produced by the following procedure.
<Process (A-2)>
As a powder raw material (a), clay mineral powder 2.1 kg and light ash 4.2 kg in a 75 L drum granulator (φ40 cm × L60 cm, rotation speed 30 r / m, fluid number 0.2) having a baffle plate Mixed with. After mixing for 2 minutes, 3.8 kg of a 25 wt% sodium polyacrylate aqueous solution was added to a two-fluid nozzle (manufactured by Spraying Systems Japan Co., Ltd .: binder spray pressure 0.15 MPa / air spray pressure for atomization 0.3 MPa. However, all are gauge pressures) and added to the granulator over 5 minutes. After the addition, the mixture was further mixed and granulated for 3 minutes, and then the obtained granule was discharged from the drum type granulator. The granules were then dried for 3 hours at 200 ° C. using an electric dryer. The water content in the dried granule group (non-spray-dried base granule group (b-1)) was 1.3% by weight.

The physical properties of the obtained non-spray-dried base granule group (b-1) were as follows: the average particle size was 289 μm, the bulk density was 511 g / L, the coarse particle ratio was 12.2 wt%, and the oil absorption capacity was 0.51 mL / g. there were.

Production Example 3: Production of non-spray dried base granule group (b-2) A non-spray dried base granule group (b-2) was produced by the following procedure.
<Process (A-2)>
As a powder raw material (a), 4.55 kg of light ash was mixed in a 75 L drum granulator (φ40 cm × L60 cm, rotation speed 30 r / m, fluid number 0.2) having a baffle plate. After mixing for 2 minutes, 2.45 kg of a 40 wt% sodium polyacrylate aqueous solution was added to a two-fluid nozzle (manufactured by Atmax Co., Ltd .: binder spray pressure 0.15 MPa / air spray pressure for atomization 0.3 MPa; All are gauge pressures) and added to the granulator over 3.7 minutes. After the addition, the mixture was further mixed and granulated for 3 minutes, and then the obtained granule was discharged from the drum type granulator. The granules were then dried for 3 hours at 200 ° C. using an electric dryer. The water content in the dried granule group (non-spray-dried base granule group (b-2)) was 1.8% by weight.

The physical properties of the non-spray-dried base granule group (b-2) obtained were as follows: the average particle size was 270 μm, the bulk density was 484 g / L, the coarse particle ratio was 20.4% by weight, and the oil absorption capacity was 0.52 mL / g. there were.

Examples 1-6
<Process (B)>
20 parts by weight (Example 1), 30 parts by weight (Example 2) or 40 parts by weight of 100 parts by weight of sodium alkyl sulfate in an anionic surfactant paste comprising 75% by weight of sodium alkyl sulfate and 25% by weight of water A mixture of 90% by weight of isodecyl glyceryl ether and 10% by weight of water of Example 3 or 20 parts by weight (Example 4), 30 parts by weight (Example 5) or 40 parts by weight (Example 6) The mixture of 90% by weight of 2-ethylhexyl glyceryl ether and 10% by weight of water was added and mixed at a temperature of 60 ° C. for 1 minute to obtain an anionic surfactant composition.

The viscosity of the anionic surfactant composition of Example 1 and Example 4 was measured at a temperature of 50 ° C. and a shear rate of 10 [1 / s] using MCR300 (manufactured by PHYSICA Messtechnik GmbH). s (Example 1) 10.1 Pa · s (Example 4).

<Process (C)>
33.9 parts by weight (Examples 1 and 4) of the anionic surfactant composition prepared in the step (B) with respect to 100 parts by weight (50 g) of the spray-dried base granule group (a) produced in Production Example 1 ), 36.1 parts by weight (Examples 2 and 5) and 38.3 parts by weight (Examples 3 and 6) were added and mixed for 10 minutes using a spatula to obtain respective mixtures. When the obtained mixture was observed, no liquid was observed in any of the mixtures, and the mixture formed a granulated product without agglomerates.

Each granulated product obtained by the above operation is placed in a plastic bag containing 4.2 parts by weight of crystalline silicate and 23.1 parts by weight of zeolite with respect to 100 parts by weight of spray-dried base granules (a). added. The plastic bag was shaken 30 times up and down to modify the surface of the granulated product (mixture), and each detergent particle group was obtained.

Comparative Example 1
<Process (C)>
29.5 parts by weight of an anionic surfactant paste composed of 75% by weight of sodium alkyl sulfate and 25% by weight of water is added to 100 parts by weight (50g) of the spray-dried base granule group (a) produced in Production Example 1. And mixing for 10 minutes using a spatula to obtain a mixture. When the obtained mixture was observed, the presence of liquid was not observed, but many aggregates were observed.

The granulated product obtained by the above operation was added to a plastic bag containing 4.2 parts by weight of crystalline silicate and 23.1 parts by weight of zeolite with respect to 100 parts by weight of the spray-dried base granule group (a). . The plastic bag was shaken up and down 30 times to carry out surface modification of the granulated product (mixture) to obtain detergent particles.

Comparative Example 2
<Process (B)>
25 parts by weight of polyoxyethylene alkyl ether with respect to 100 parts by weight of sodium alkyl sulfate was added to a mixture comprising 75% by weight of sodium alkyl sulfate and 25% by weight of water, and mixed for 1 minute at a temperature of 60 ° C. An activator composition was obtained. When the viscosity of the obtained anionic surfactant composition was measured at a temperature of 50 ° C. and a shear rate of 10 [1 / s] using MCR300 (manufactured by PHYSICA Messtechnik GmbH), it was 11.2 Pa · s.

<Process (C)>
35.0 parts by weight of the anionic surfactant composition prepared in step (B) is added to 100 parts by weight (50 g) of the spray-dried base granule group (a) produced in Production Example 1, and a spatula is used. For 10 minutes to obtain a mixture. When the obtained mixture was observed, the presence of liquid was not observed, but many aggregates were observed.

The mixture obtained by the above operation was added to a plastic bag containing 4.2 parts by weight of crystalline silicate and 23.1 parts by weight of zeolite with respect to 100 parts by weight of the spray-dried base granule group (a). The plastic bag was shaken up and down 30 times to carry out surface modification of the granulated product (mixture) to obtain detergent particles.

Table 1 shows the physical properties of the detergent particles obtained in Examples 1 to 6 and Comparative Examples 1 and 2.

Examples 7 to 10
<Process (B)>
In an anionic surfactant paste comprising 75% by weight sodium alkyl sulfate and 25% by weight water, 20 parts by weight (Example 8) or 30 parts by weight (Example 7) of isodecylglyceryl per 100 parts by weight of sodium alkyl sulfate A mixture consisting of 90% by weight of ether and 10% by weight of water or 20 parts by weight (Examples 9, 10) of 90% by weight of 2-ethylhexyl glyceryl ether and 10% by weight of water was added, and the temperature 60 The mixture was mixed at 1 ° C. for 1 minute to obtain an anionic surfactant composition.

<Process (C)>
With respect to 100 parts by weight (50 g) of the non-spray-dried base granule group (b-1) or (b-2) produced in Production Example 2 or 3, the anionic surfactant composition prepared in Step (B) is used. Add 36.1 parts by weight (Example 7), 36.2 parts by weight (Examples 8 and 9), 50.7 parts by weight (Example 10), mix using a spatula for 10 minutes, A mixture was obtained. When the obtained mixture was observed, no liquid was observed in any of the mixtures, and the mixture formed a granulated product without agglomerates.

Each granulated product obtained by the above operation is prepared by using 4.2 parts by weight of crystalline silicate and 23. It was added to a plastic bag containing 1 part by weight. The plastic bag was shaken 30 times up and down to modify the surface of the granulated product (mixture), and each detergent particle group was obtained.

Comparative Examples 3-5
<Process (C)>
Anion comprising 75% by weight of sodium alkyl sulfate and 25% by weight of water with respect to 100 parts by weight (50 g) of the non-spray-dried base granules (b-1) or (b-2) produced in Production Example 2 or 3. 29.5 parts by weight of surfactant paste (Comparative Example 3), 31.5 parts by weight (Comparative Example 4) and 44.1 parts by weight (Comparative Example 5) were added and mixed for 10 minutes using a spatula. Each mixture was obtained. When the obtained mixture was observed, no liquid was observed in any of the mixtures, but many aggregates were observed.

Each granulated product obtained by the above operation is used with 100 parts by weight of the non-spray-dried base granule group (b-1) or (b-2), 4.2 parts by weight of crystalline silicate, and 23. of zeolite. It was added to a plastic bag containing 1 part by weight. The plastic bag was shaken 30 times up and down to modify the surface of the granulated product (mixture), and each detergent particle group was obtained.

Table 2 shows the physical properties and the like of the detergent particles obtained in Examples 7 to 10 and Comparative Examples 3 to 5.

Table 1 summarizes the results using the spray-dried base granule group (a). From Table 1, as compared with those of Comparative Examples 1 and 2, all of the detergent particle groups obtained in Examples 1 to 6, the coarse particle ratio, the difference in the coarse particle ratio of the detergent particle group, the degree of particle growth, It can be seen from the observation results of the obtained detergent particles that the solubility and detergency are good that the detergent particles having few aggregates can be produced by the production method of the present invention. From comparison between Examples 1 to 6 and Comparative Example 2, it was found that the predetermined effect was not exhibited simply by mixing nonionic surfactant (polyoxyethylene alkyl ether in Comparative Example 2) and anionic surfactant paste. It was found that a predetermined effect was exhibited for the first time by using an alkyl glyceryl ether as defined in the present application.

Further, Table 2 summarizes the results using the non-spray-dried base granule group (b-1) or (b-2). From Table 2, the detergent particle groups obtained in Examples 7 to 10 were compared with those in Comparative Examples 3 to 5, all of the coarse particle ratio, the difference in the coarse particle ratio of the detergent particle group, the degree of particle growth, It can be seen from the observation results of the obtained detergent particles that the solubility and detergency are good that the detergent particles having few aggregates can be produced by the production method of the present invention. Furthermore, the non-spray-dried base granule group (b-1) or (b-2) tended to have a higher coarse particle ratio than the spray-dried base granule group (a), but such (b-1) Or even if it was a case where (b-2) was used, it turned out that the coarse particle rate raise difference of a detergent particle group is small. From this, according to the manufacturing method of this invention, it was shown that the detergent particle group by which the raise of the coarse particle rate was suppressed irrespective of the difference in the coarse particle rate of the base granule group to be used can be manufactured.

Since the detergent particle group of the present invention has a sharp particle size distribution, few aggregates and excellent solubility, it can be suitably used, for example, for the production of clothing detergents and dishwasher detergents.

Claims (13)

Next step:
Step (B): A step of preparing an anionic surfactant composition by mixing an anionic surfactant paste and an alkyl glyceryl ether, and Step (C): an anionic surfactant composition prepared in the step (B). And a step of preparing a detergent particle group by mixing a base granule group having an oil absorption capacity of 0.2 mL / g or more,
A method for producing a detergent particle group. The following formula (1) of the detergent particle group to be produced:
Particle growth degree = [average particle size of detergent particles] / [average particle size of base granules] (1)
The production method according to claim 1, wherein the grain growth rate defined by the formula (1) is 1.25 or less. The production method according to claim 1 or 2, wherein 10 to 40 parts by weight of alkyl glyceryl ether is mixed with 100 parts by weight of the anionic surfactant in the anionic surfactant paste. The production method according to any one of claims 1 to 3, wherein 5 to 100 parts by weight of an anionic surfactant composition is mixed with 100 parts by weight of the base granule group. The base granule group is one of the following steps:
Step (A-1): A step of obtaining a base granule group by spray-drying a slurry containing a water-soluble inorganic salt, or Step (A-2): Oil absorption capacity 0.4 mL / g in a container rotary granulator A step of adding a binder to the above powder raw material for detergent using a multi-fluid nozzle and granulating to obtain a base granule group,
The production method according to any one of claims 1 to 4, which is a group of base granules prepared by a method comprising: The anionic surfactant is represented by the following formula (2):
R—O—SO ₃ M (2)
(In the formula, R represents an alkyl group or alkenyl group having 10 to 18 carbon atoms, and M represents an alkali metal atom or an amine.)
The production method according to any one of claims 1 to 5, which is an anionic surfactant represented by the formula: The production method according to any one of claims 1 to 6, wherein the alkyl glyceryl ether is isodecyl glyceryl ether and / or 2-ethylhexyl glyceryl ether. The production method according to any one of claims 1 to 7, wherein the content of water in the anionic surfactant paste is 15 to 50% by weight. The production method according to any one of claims 1 to 8, wherein the viscosity (50 ° C) of the anionic surfactant composition is 0.01 to 20 Pa · s. The production method according to any one of claims 1 to 9, wherein the oil absorption capacity of the base granule group is 0.7 mL / g or less. The production method according to any one of claims 1 to 10, wherein the average particle size of the base granule group is 140 to 600 µm. The production method according to any one of claims 5 to 11, wherein the oil absorption capacity of the detergent powder raw material is 1.0 mL / g or less. A detergent particle group obtained by the production method according to any one of claims 1 to 12.