TWI502063B - Method for manufacturing cleaning agent particles - Google Patents

Description

Method for producing detergent particle group

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

One of the methods for preparing the detergent particle group is a method of mixing a powdery substance with a liquid surfactant composition. Among them, a method of using an anionic surfactant in a state of a paste has been disclosed so far.

For example, Patent Document 1 discloses a method for producing a particulate detergent composition in which a paste of an alkyl ether sulfate is absorbed into cerium oxide or cerium salt and granulated and dried. In such a production method, although it has an advantage of being able to achieve a high degree of blending of an anionic surfactant, in order to facilitate the production of such a granular detergent composition, an oil-absorbing carrier such as cerium oxide or ceric acid salt is required, and further, After the granulation step, in order to remove the moisture contained in the above paste, a drying step is required.

Further, in Patent Document 2, it is disclosed that a base granule having a water-soluble inorganic salt produced by spray drying and having a holding ability of 20 mL/100 g or more is mixed with an alkyl sulfate paste, and surface modification is carried out. Quality manufacturing method. However, in the case of such a manufacturing method, there are many agglomerates, and there are still disadvantages in terms of the length of the particles. Further, although this problem is improved by the addition of polyoxyethylene alkyl ether, it requires a large amount of blending, and there are still disadvantages in terms of the degree of freedom of composition.

Prior technical literature Patent literature

Patent Document 1: International Publication No. 0031223

Patent Document 2: Japanese Patent Laid-Open No. 2006-137925

That is, the present invention relates to:

[1] A method for producing a detergent particle group, comprising the steps of: (B): mixing an anionic surfactant paste with an alkyl glyceryl ether to prepare an anionic surfactant composition; and step (C): Preparing the anionic surfactant composition prepared in the step (B) and mixing the base particle group having an oil absorption capacity of 0.2 mL/g or more to prepare a detergent particle group;

[2] A detergent particle group obtained by the production method of the above [1].

The present invention relates to a method for producing a detergent particle group, which does not require a drying step even when a surfactant composition having a high water content is used, and can produce powder characteristics such as suppression of particle growth, steep particle size distribution, and solubility. A good detergent particle group.

By using the method for producing a detergent particle group of the present invention, it is possible to exhibit an effect of mixing the anionic surfactant composition with a base particle group having an oil absorption capacity of 0.2 mL/g or more, without a drying step of removing moisture, that is, It is possible to produce a detergent particle group in which particle growth is suppressed, a particle size distribution is steep, a solubility is high, and a cleaning effect is high. By suppressing the growth of the particles and making the particle size distribution steep, it is possible to obtain a cleaning agent which is not only excellent in appearance but also excellent in solubility. Further, regardless of the difference in the coarse particle ratio of the base particle group, the coarse particle ratio of the detergent particle group to be produced can be suppressed.

The method for producing the detergent particle group of the present invention is as described above, and is characterized in that it comprises the following steps: Step (B): mixing an anionic surfactant paste with an alkyl glyceryl ether to prepare an anionic surfactant composition; And the step (C): mixing the anionic surfactant composition prepared in the step (B) with a base particle group having an oil absorption capacity of 0.2 mL/g or more to prepare a detergent particle group.

Hereinafter, the production method of the present invention will be described in further detail.

<Step (B)>

Step (B) is to prepare an anionic surfactant composition by mixing an anionic surfactant paste with an alkyl glyceryl ether. In the present specification, the term "anionic surfactant paste" means a mixture of an anionic surfactant and water. The content of water in the anionic surfactant paste is preferably from 15 to 50% by weight, more preferably from 25% to 45% by weight, still more preferably from 25 to 40% by weight. In addition, the content of each component and the % of the compounding amount described in the present specification are represented by weight % unless otherwise specified.

As the anionic surfactant used in this step, generally, a detergent for clothing, a vegetable, a dishwashing detergent, a hair, a skin cleansing agent, or the like can be used. For example, an alkyl sulfate salt, a polyoxyethylene alkyl sulfate salt, an α-sulfo fatty acid ester salt, an α-olefin sulfonate, an alkyl or hydroxyalkyl ether carboxylate, and N-fluorene may be mentioned. Taurine, N-deuterated methyl taurine, N-deuterated glycine, N-deuterated aspartic acid, N-deuterated sarcosine, N-deuterated glutamic acid, higher fatty acids Salts, alkylbenzenesulfonates, alkyl sulfates, monoalkyl phosphates, alkylguanamine ether sulfates, fatty acid monoglyceride sulfates, and alkylimidodicarboxylates. As the anionic surfactant, one type may be used alone or a plurality of types may be used in combination.

Among the anionic surfactants, preferred are anionic surfactants, alkyl sulfates, alkyl sulfates, α-sulfofatty acid ester salts, α-olefin sulfonates, and polyoxyethylene alkyl sulfates. Ester salts and the like. More preferably, it is an alkyl sulfate in terms of obtaining a remarkable effect.

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

The alkyl glyceryl ether used in this step can be represented by the following 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 the alkyl glyceryl ether and an anionic surfactant paste, a detergent particle group having less aggregates and a smaller particle length can be obtained.

In the formula (3), R is a linear or branched alkyl or alkenyl group having 1 to 24 carbon atoms or a cycloalkyl group having 3 to 8 carbon atoms, preferably a linear or branched carbon number of 6 The alkyl group of ~18 is more preferably an alkyl group having 8 to 12 carbon atoms. Specifically, examples of R include hexyl, heptyl, octyl, decyl, decyl, undecyl, dodecyl, tridecyl, tetradecyl, pentadecyl, and ten. a linear alkyl group such as hexaalkyl, heptadecyl or octadecyl, 2-ethylhexyl, 2-methylheptyl, 2-methylindenyl, 2-octyldecyl, 3,5, A branched alkyl group such as 5-trimethylhexyl, isodecyl or isostearyl, or an alkenyl group such as an oleyl group.

The amount of the alkyl glyceryl ether in the step is preferably 10 to 40 parts by weight, more preferably 15 to 40 parts by weight, based on 100 parts by weight of the anionic surfactant in the anionic surfactant paste. Good is 20~40 parts by weight. From the viewpoint of the length of the particles of the detergent particle group of the present invention, the compounding amount is preferably 10 parts by weight or more, and the effective component of the anionic surfactant supported on the base particle group and the alkyl glyceryl ether The blending amount is preferably 40 parts by weight or less from the viewpoint of cost.

The anionic surfactant composition of this step can be prepared by mixing a specific amount of an anionic surfactant paste, a specific amount of an alkyl glyceryl ether. Ingredients other than these ingredients may also be added as needed.

The viscosity of the anionic surfactant composition in this step is not particularly limited, and the surfactant composition is measured by MCR300 (manufactured by PHYSICA Messtechnik GmbH) at a temperature of 50 ° C and a shear rate of 10 [1/s]. In the case of the operability in the step of preparing the detergent particle group in combination with the base particle group, it is preferably in the range of 0.01 to 20 Pa‧s, more preferably in the range of 0.05 to 15 Pa‧s.

Specific examples of the operation for preparing the anionic surfactant composition include an operation of mixing a specific amount of an anionic surfactant paste and a specific amount of alkyl glyceryl ether. It is also possible to add ingredients other than the ingredients as needed. As the mixer to be used, a mixer generally used in the field of detergents can be used, and as conditions for mixing, conditions generally employed in the field of detergents can be employed.

<Step (C)>

The step (C) is a step of preparing the detergent particle group by mixing the anionic surfactant composition prepared in the above step (B) with a base particle group having an oil absorption capacity of 0.2 mL/g or more.

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

[Preparation of spray-dried base particle group (a): step (A-1)]

The spray-dried base particle group (a) is a particle group obtained by spray-drying a slurry containing a water-soluble inorganic salt. The spray-dried base particle group (a) can be prepared by spray drying, for example, a slurry containing the following components.

The water-soluble inorganic salt is not particularly limited, and for example, sodium carbonate, potassium carbonate, sodium sulfate, sodium sulfite, sodium chloride or the like is preferred as the water-soluble inorganic salt. As the water-soluble inorganic salt, one type may be used alone or a plurality of types may be used in combination.

In addition to the water-soluble inorganic salt, the following components may be further used. For example, a builder which is generally used for a detergent for clothing, such as a metal ion blocker such as zeolite, citrate or sodium tripolyphosphate, and a crystalline citrate having a metal ion blocking ability ‧ alkaline A component of the ability, such as an acrylic polymer, an acrylic acid maleic acid copolymer, a re-contamination inhibitor such as carboxymethyl cellulose, a fluorescent whitening agent, and the like.

The amount of water in the slurry is not particularly limited, and for example, it is preferably 40 to 60% by weight of the slurry. The conditions (temperature, spray drying device, spray method, drying method, and the like) when the slurry is spray-dried may be a known condition, and are not particularly limited. By using the above materials or conditions, a base particle group having a specific oil absorbing ability can be obtained.

[Physical properties of spray-dried base particle group (a)]

The oil absorbing ability of the spray-dried base particle group (a) is preferably 0.2 mL/g or more, more preferably 0.3 mL/g or more. Further, as a preferred upper limit of the oil absorption capacity, it is 0.7 mL/g or less. Within this range, it is suitable for suppressing aggregation of the spray-dried base particle group (a) and suppressing particle growth of particles in the detergent particle group. Therefore, from the same viewpoint as described above, the oil absorption capacity of the spray-dried base particle group (a) is preferably from 0.2 to 0.7 mL/g, more preferably from 0.3 to 0.7 mL/g.

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

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

The average particle diameter of the spray-dried base particle group (a) is preferably from 140 to 600 μm, more preferably from 150 to 500 μm, still more preferably from 180 to 300 μm. In the present specification, the average particle diameter of the detergent particle group and the base particle group is determined by the following method using a sieve specified in JIS Z 8801 unless otherwise specified.

For example, prepare sieves and trays with meshes of 2000 μm, 1400 μm, 1000 μm, 710 μm, 500 μm, 355 μm, 250 μm, 180 μm, and 125 μm, installed in a Rota-Turbo screen (Ro-Tap) Machine) (Tanzhong Chemical Machinery Manufacturing Co., Ltd., slap: 156 times / minute, shaking: 290 times / minute). After 100 g of the sample was shaken for 10 minutes for sieving, the tray and each sieve were stacked in the order of tray, 125 μm, 180 μm, 250 μm, 355 μm, 500 μm, 710 μm, 1000 μm, 1400 μm, and 2000 μm. The quality frequency below. The mesh of the initial sieve with the cumulative mass frequency of 50% or more is set to x _j μm, and when the mesh of the sieve of the smaller one is set to x _j+1 μm, the sieve from the tray to x _j μm The cumulative mass frequency is set to Q _j %, and when the total mass frequency of the sieve from the tray to x _j+1 μm is set to Q _j+1 %, it can be obtained according to formulas (A) and (B). Average particle size x _a :

[Number 1]

x _a =10 ^z (A)

z=log ₁₀ x _j+1 +(log ₁₀ x _j -log ₁₀ x _j+1 )×(50-Q _j+1 )/(Q _j -Q _j+1 ) (B).

The measurement of the moisture in the spray-dried base particle group (a) was carried out by the following infrared moisture meter method. That is, 3 g of the sample (spray-dried base particle group (a)) was weighed into a sample dish of known weight by an infrared moisture meter (Kett Scientific Research Institute Co., Ltd. (Infrared Lamp 185 W)) The sample was heated and dried for 3 minutes. After drying, the weight of the sample dish and the dried sample was measured. The difference between the weight of the sample dish before and after drying obtained by the operation and the weight of the sample is divided by the 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 particle group (a) is preferably from 40 to 90% by weight of the particle group (a) from the viewpoints of the cleaning performance and the workability of the slurry before spray drying. More preferably, it is 50 to 90% by weight, and further preferably 55 to 90% by weight.

[Preparation of non-spray dried base particle group (b): step (A-2)]

The non-spray-dried base particle group (b) is obtained by adding a binder to a powder raw material for a detergent having an oil absorption capacity of 0.4 mL/g or more by using a multi-fluid nozzle in a container rotary granulator, and obtaining granulation. The particle group. The powder raw material for detergents is, for example, a powder raw material (hereinafter referred to as "powder raw material (a)").

Examples of the powder raw material (a) include a caustic soda (for example, light soda ash and heavy ash) produced by calcining sodium hydrogencarbonate, a mirabilite, and a porous powder obtained by drying water and a substance of sodium tripolyphosphate. Clay mineral powder, etc. From the viewpoint of easiness of handling and ease of acquisition, light soda ash is preferred. As the powder raw material (a), one component may be used alone or a plurality of components may be used in combination. The powder raw material (a) usually has fine pores of 10 μm or less inside, and the surfactant can be supported on the micropores.

Examples of the clay mineral powder include talc, pyrophyllite, bentonite (saponite, lithium bentonite, zinc bentonite, strontite, montmorillonite, aluminum bentonite, iron bentonite, etc.), vermiculite, Mica (phlogopite, sericite, iron lithium mica, muscovite, orange sapphire glass, squama, sea green stone, etc.), chlorite (sloping chlorite, chlorite, nickel chlorite, manganese aluminum) Chlorite, aluminum chlorite, bismuth aluminite, etc., crisp mica (green crisp mica, pearl mica, etc.), manganese zoisite, serpentine mineral (leaf serpentine, serpentine, serpentine, magnesium Aluminum serpentine, gram iron serpentine, iron-aluminum serpentine, iron serpentine, dark nickel serpentine, etc.), kaolin minerals (kaolin, dickite, pearl clay, watery kaolin, etc.).

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

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

In other words, the sample (powder material (a)) was placed in an amount of 30 to 35 g in an absorption amount measuring device (S410 manufactured by Asahi Co., Ltd.), and the driving blade was rotated at 200 r/m. A liquid nonionic surfactant (Emulgen 108, manufactured by Kao Corporation) was added dropwise at a liquid supply rate of 4 mL/min, and the point of maximum torque was determined. The liquid addition amount at the point of the torque which is 70% of the point of the maximum torque is divided by the sample input amount, and is set as the oil absorption capacity.

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

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

The powder raw material (a) may be used alone as a powder raw material for detergents, or may be used in combination.

In addition to the powder raw material (a), the non-spray-dried base particle group (b) may be further obtained by using other components as follows. Specific examples thereof include a builder, a recontamination preventing agent, a fluorescent whitening agent, and the like which are generally used for a detergent for clothing, which are mentioned in the description of the spray-dried base particle group (a).

As a granulation method used in this step, a method of granulating a powder raw material for a detergent and a binder by a container rotary granulator is employed. As the container rotary granulator, a drum type mixer or a disc type mixer is preferred. The drum type mixer is not particularly limited as long as it is rotated by a drum-shaped cylinder, and a drum type granulator (mixer) may be used in addition to a drum type mixer which is horizontally or slightly inclined. Multi-stage cone drum granulator (mixer), etc. These devices can be used in either batch or 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, and water-soluble cellulose derivatives (as Examples of such derivatives include an organic polymer such as an carboxylic acid polymer, a starch or a saccharide, an inorganic polymer such as an amorphous phthalate, a higher fatty acid, an alkylbenzenesulfonic acid, or the like. A general surfactant or the like which is widely described in the conventional technique. From the viewpoint of the adhesion and the cleaning power, a water-soluble cellulose derivative, a saccharide, and a carboxylic acid-based polymer are preferable, and a salt of a acrylate-maleic acid copolymer or a polyacrylate is more preferable. As the salt, a sodium salt, a potassium salt or an ammonium salt is preferred. Further, the weight average molecular weight of the carboxylic acid-based polymer is preferably from 1,000 to 100,000, more preferably from 2,000 to 80,000.

The binder added may also be an aqueous solution. The concentration at the time of addition in an aqueous solution is not particularly limited, but the particle size at the time of granulation by the non-spray-dried base particle group (b) is greatly affected depending on the volume of the binder, and therefore, depending on the amount of the binder required The particle size of the desired particle group is determined to determine the concentration. For example, the concentration of the component of the binder when added as an aqueous solution is preferably 20 to 80% by weight.

The binder is added using a multi-fluid nozzle. By using the nozzle, the droplets of the binder can be made fine and dispersed. The multi-fluid nozzle is a nozzle that allows a liquid and a gas for atomization (air, nitrogen, etc.) to flow through a separate flow path to the vicinity of the tip end of the nozzle, and to mix and atomize the nozzle, and a 2-fluid nozzle or a 3-fluid nozzle can be used. Fluid nozzles, etc. Further, the mixing portion of the binder and the gas for atomization may be either an internal mixing type mixed in the tip end portion of the nozzle or an external mixing type mixed outside the nozzle tip end portion.

As such a multi-fluid nozzle, an internal mixing type 2-fluid nozzle manufactured by Spraying Systems Japan Co., Ltd., Kyoritsu Alloy Co., Ltd., and Ikei Co., Ltd., manufactured by Spraying Systems Japan Co., Ltd., and a common alloy An external hybrid type 2 fluid nozzle manufactured by Fujisawa Electric Co., Ltd., an external hybrid type 2 fluid nozzle manufactured by Fujisawa Electric Co., Ltd., etc.

For example, in the case of using a two-fluid nozzle, it is preferred to supply the binder, for example, under the following conditions. The adjustment of the flow rate of the gas for atomization is easy by the adjustment of the spray pressure of the gas for atomization, and the spray pressure of the gas for atomization is preferably 0.1 MPa from the viewpoint of the dispersibility of the binder. The pressure is more than 1.0 MPa (gauge pressure) from the viewpoint of equipment load. Further, the spray pressure of the binder is not particularly limited, and is preferably, for example, 1.0 MPa or less from the viewpoint of equipment load.

The content of the binder in the non-spray-dried base particle group (b) is preferably from 1 to 50% by weight, more preferably from 1 to 50% by weight, based on the viewpoint of adhesion and oil absorption ability. 5 to 45% by weight, further preferably 8 to 40% by weight, more preferably 10 to 35% by weight.

[Physical properties of non-spray dried base particle group (b)]

The non-spray-dried base particle group (b) is, for example, a group of particles of a structure in which the powder raw material (a) is slowly agglomerated. In this case, there are (1) a large gap between the particles, (2) a small void of 10 μm or less or a two holding point between the layers in the powder raw material (a). By adjusting the two holding points, a non-spray-dried base particle group (b) having a desired oil absorption capacity can be obtained.

The oil absorption capacity of the non-spray dried base particle group (b) is 0.2 mL/g or more, preferably 0.3 mL/g or more, more preferably 0.4 mL/g or more. On the other hand, as the oil absorbing ability, it is preferably 0.7 mL/g or less. Within this range, the aggregation of the non-spray-dried base particle groups (b) is suppressed, and therefore, it is preferable to suppress the particle length of the particles in the detergent particle group. Therefore, from the same viewpoint as described above, the oil absorption capacity of the non-spray-dried base particle group (b) is preferably from 0.2 to 0.7 mL/g, more preferably from 0.3 to 0.7 mL/g. The method for measuring the oil absorption capacity of the non-spray dried base particle group (b) is the same as the method for measuring the oil absorption capacity of the spray-dried base particle group (a).

The bulk density of the non-spray-dried base particle group (b) is preferably 200 to be considered from the viewpoint of ensuring the capacity of the surfactant composition and ensuring a higher bulk density after the surfactant composition is carried. 1000 g/L, more preferably 300 to 1000 g/L, further preferably 400 to 550 g/L, and more preferably 400 to 500 g/L. In the present specification, the method for measuring the bulk density of the non-spray-dried base particle group (b) is the same as the method for measuring the bulk density of the spray-dried base particle group (a).

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

The content of the water in the non-spray-dried base particle group (b) is preferably 30% by weight or less, more preferably 20% by weight or less, still more preferably 15% by weight or less, from the viewpoint of workability or oil absorption ability. The method for measuring the moisture in the non-spray dried base particle group (b) is the same as the method for measuring the water content in the spray-dried base particle group (a).

[Method of mixing anionic surfactant composition with basic particle group]

The ratio of the two components in the case of mixing the anionic surfactant composition to the base particle group is not particularly limited as long as it can be uniformly mixed. For example, the anionic surfactant composition is preferably used in an amount of 100 parts by weight based on the base particle group. 5 to 100 parts by weight, more preferably 10 to 90 parts by weight, still more preferably 20 to 70 parts by weight, still more preferably 25 to 50 parts by weight. From the viewpoint of the cleaning power, the anionic surfactant composition is preferably 5 parts by weight or more, more preferably 10 parts by weight or more, still more preferably 20 parts by weight or more, and furthermore, based on 100 parts by weight of the particle group. It is preferably 25 parts by weight or more. The anionic surfactant composition is preferably 100 parts by weight or less, more preferably 90 parts by weight or less, still more preferably 70 parts by weight, based on 100 parts by weight of the particle group, from the viewpoints of composition degree of freedom, solubility, and the like. Hereinafter, it is more preferably 50 parts by weight or less.

As the mixing conditions in the step (C), the mixing conditions for substantially maintaining the form of the base particle group, that is, the mixing conditions for not disintegrating the particle group, may be selected. For example, in the case of a small amount of mixing, a spatula or the like may be used for manual mixing, or when a mixer having a stirring blade is used, from the viewpoint of suppressing the disintegration of the base particle group and the mixing efficiency, When the shape of the mixing wing of the stirring wing provided in the machine is a paddle type, the froude number of the stirring wing is preferably set to 0.5 to 8.0, more preferably 0.8 to 4.0, and further It is preferably set to 0.5 to 2.0. Further, when the shape of the mixing blade is a propeller type, the Froude number of the agitating blade is preferably 0.1 to 4.0, more preferably 0.15 to 2.0. Further, when the shape of the mixing blade is a belt type, the Froude number of the stirring blade is preferably 0.05 to 4.0, more preferably 0.1 to 2.0.

Further, the Froude number system defined in the present specification is calculated by the following formula:

Froude number = V ² / (R × g)

(here, V represents the peripheral speed [m/s] of the front end of the stirring blade, R represents the radius of rotation [m] of the stirring blade, and g represents the gravitational acceleration [m/s ² ]).

In the step (C), the powder raw materials other than the base particle group may be blended as needed. In terms of solubility, the amount thereof is preferably 30 parts by weight or less based on 100 parts by weight of the base particle group.

The powder raw material other than the base particle group referred to in this step means a cleaning power enhancer or an oil absorbing agent which is a powder at normal temperature. Specific examples thereof include a base exhibiting a metal ion blocking ability such as zeolite or citrate, a base exhibiting basic ability such as sodium carbonate or potassium carbonate, and a crystalline bismuth salt having a metal ion seal. Resistance, ‧ basic ability, etc., or amorphous cerium oxide or amorphous aluminum lanate with low metal ion blocking ability but high oil absorption capacity. By using the powder raw material in combination with the base particle group as needed, it is possible to achieve high formulation of the anionic surfactant composition and reduction of adhesion of the mixture to the mixer, and also to improve the cleaning power. As the raw material of the powder, one type may be used alone or a plurality of types may be used in combination.

After the anionic surfactant composition is mixed with the base particle group, preferably 1 to 10 parts by weight of polyethylene glycol (PEG) and/or fatty acid and/or is added with respect to 100 parts by weight of the base particle group. The soap water is further mixed to coat the surface of the base particle group. By this coating, the blocking resistance of the detergent particle group is improved, which is preferable. Further, by adding PEG and/or a fatty acid and/or soap water, when the detergent particle group is dissolved, aggregation can be suppressed and the dispersibility can be improved, and as a result, the solubility of the detergent particle group can be improved, which is preferable.

Further, the detergent particle group obtained by the present invention may also contain a nonionic surfactant. The nonionic surfactant may be adsorbed in the base particle group before and/or after the step (C), or may be mixed into the anionic surfactant composition used in the step (B), and the anionic surfactant is active. The composition is simultaneously absorbed by oil ‧ carried in the base particle group, and from the viewpoint of suppressing the agglomeration caused by the exudation of the nonionic surfactant, it is preferred to absorb the oil before the step (C) In the group. Further, the content of the detergent particle group of the nonionic surfactant is preferably 20% by weight or less, more preferably 15% by weight in the detergent particle group from the viewpoint of suppressing agglomeration due to bleeding. %the following. Further, from the viewpoint of the cleaning power, it is preferably 5% by weight or more, and more preferably 10% by weight or more.

The type of the nonionic surfactant is not particularly limited. For example, a nonionic surfactant described in a conventionally known technique set (powder cleaner for clothing) issued by the Japan Patent Office can be used.

Further, as the temperature in the mixer at the time of mixing, it is preferred to substantially suppress the disintegration of the base particle group, and at the same time, the temperature of the anionic surfactant composition and the base particle group can be effectively mixed. For example, it is preferred that the temperature above the pour point of the mixed anionic surfactant composition is more preferably 10 ° C or more of the pour point, and further preferably 20 ° C or more of the pour point. Further, the mixing time at the time of mixing is preferably about 2 to 20 minutes, more preferably about 2 to 10 minutes. The temperature adjustment in the mixer can be performed by circulating cold water or warm water in a casing or the like. Therefore, the means for mixing is preferably a structure having a casing.

As a method of mixing the anionic surfactant composition and the base particle group, it may be either a batch type or a continuous type. In the case of batch mixing, it is preferred to add an anionic surfactant composition after the base particle group is previously placed in a mixer. The temperature of the anionic surfactant composition to be supplied is preferably 70 ° C or lower, and more preferably 60 ° C or lower from the viewpoint of stability of the anionic surfactant composition.

The mixer which is used in the case of batch mixing is not particularly limited as long as it is generally used for batch mixing, and for example, (1) a mixer having a paddle type as a shape of a mixing blade, A mixing machine having a stirring shaft in the mixing tank, and a stirring wing is mounted on the shaft to carry out mixing of powders: for example, a Henschel mixer (manufactured by Mitsui Miike Chemical Co., Ltd.) and a high-speed mixer (Shenjiang Industrial Co., Ltd.) Company system), vertical granulator (made by Powrex Co., Ltd.), Loedige mixer (made by Matsubo Co., Ltd.), coulter mixer (made by Pacific Machine Co., Ltd.), TSK-MTI mixing A mixing device described in Japanese Laid-Open Patent Publication No. Hei 10-296064, and Japanese Patent Application Laid-Open No. Hei No. Hei 10-296065, and the like. There is a mixer in which a spiral-shaped belt-like wing is rotated and is mixed by a cylindrical, semi-cylindrical or conical type fixed container: a belt mixer (made by Rihe Machinery Co., Ltd.) ), Batch type kneading machine (made by Satake Chemical Industry Co., Ltd.), ribbon type mixer (manufactured by Dashun Seisakusho Co., Ltd.), Julia mixer (made by Deshou Co., Ltd.), etc. (3) As a propeller type hybrid mixer, the propeller rotates on one side of the conical container and rotates around the axis parallel to the wall of the container, thereby revolving, thereby performing mixing in the form of mixing. Machine: For example, a conical spiral mixer (manufactured by Hosokawa Micron Co., Ltd.), an SV mixer (manufactured by Shinko Pantec Co., Ltd.), or the like.

Further, in the case of continuous mixing, there is no particular limitation as long as it is a continuous mixer which is generally used for continuous mixing. For example, the basic particle group and the anionic surfactant can be used by using a continuous device in the above mixer. The composition is mixed.

<surface modification>

It is desirable to further surface modify the detergent particle group obtained in the step (C). By performing surface modification, it is possible to obtain a detergent particle group in which fluidity and blocking resistance are further improved. It is preferred to use a fine powder when performing surface modification. In the case of using a fine powder, surface modification can be carried out by mixing the detergent particle group obtained in the step (C) with the fine powder under specific conditions.

The fine powder is not particularly limited, and the average particle diameter of the primary particles is preferably 20 μm in terms of improvement in the coverage of the detergent particle group, improvement in fluidity of the detergent particle group, and improvement in blocking resistance. The following. The average particle diameter is measured by a method using light scattering, for example, a particle analyzer (manufactured by Horiba, Ltd.) or a microscope.

Specific examples of the fine powder include a phthalate compound such as a crystalline citrate compound, an aluminosilicate, calcium citrate, cerium oxide, bentonite, sodium tripolyphosphate, talc, clay, and amorphous. An inorganic fine powder such as a cerium oxide derivative or a metal soap having a primary particle of 20 μm or less. As the fine powder, one type may be used alone or a plurality of types may be used in combination. Further, the fine powder has a high ion exchange capacity or a basic ability, so that it is preferable in terms of cleaning power. Preferred fine powders among these include a phthalate compound such as a crystalline phthalate compound and an aluminosilicate.

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

As a mixing condition in the surface modification, a mixing condition in which the form of the base particle group holding the anionic surfactant composition is substantially maintained may be selected. For example, in the case of a small amount of mixing, it is preferable to use a spatula or the like to manually mix, or to use a mixer having both a stirring blade and a crushing wing. In the case of using the mixer, from the viewpoint of suppressing the collapse of the base particle group, it is preferable to set the number of the Froude of the stirring blade provided in the machine to 10 or less, and more preferably to 7 or less. From the viewpoint of the efficiency of mixing with the fine powder and the dispersion of the fine powder, the number of the Froude is preferably 2 or more, and more preferably 3 or more. Further, from the viewpoint of the efficiency of mixing with the fine powder and the dispersion of the fine powder, the number of the dough of the crushed blade is preferably 8,000 or less, more preferably 5,000 or less. When the number of the Froude is within this range, a detergent particle group excellent in fluidity can be obtained.

As a preferred mixer in this step, a mixer having both a stirring blade and a grinding blade in the mixer used in the step (C) can be mentioned. Further, by performing the step (C) and the surface modification using different mixers, the temperature adjustment of the mixed substance is facilitated. For example, when a non-heat-resistant component such as a fragrance or an enzyme is added in the middle or after the surface modification, it is preferred to adjust the temperature of the mixture at the time of surface modification. This temperature adjustment can be made by setting or venting the casing temperature. In order to efficiently transfer the detergent particle group obtained in the step (C) to the apparatus for surface modification, it is also preferable to add a part of the fine powder to the detergent particle group at the end of the step (C). kind.

<cleaner 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, and is a detergent particle group produced by using a base particle group as a core, and preferably has one base particle as a core in one detergent particle. A group of detergent particles characterized by features.

As an index indicating such a characteristic of the detergent particle group, the length of the particles defined by the following formula (1) can be used:

The particle formation length = [average particle diameter of the detergent particle group] / [average particle diameter of the base particle group] (1).

Specifically, it is preferable that the particles have a detergent particle group having a length of 1.25 or less, more preferably 1.20 or less, still more preferably 1.15 or less. The lower limit of the particle formation length is not particularly limited, but is preferably 1.0 or more. Therefore, from the viewpoint of suppressing aggregation of the detergent particle group, the particle formation length is preferably from 1.0 to 1.25, more preferably from 1.0 to 1.20, still more preferably from 1.0 to 1.15.

Since the detergent particle group of the present invention can suppress aggregation between the detergent particles, there is an advantage that the amount of particles (agglomerated particles) outside the desired particle size range is smaller, and the solubility of the detergent particle group is excellent. Moreover, the particle size distribution of the detergent particle group is steep.

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

The coarse particle ratio in the present specification is defined by the weight % of particles having a size of 500 μm or more in the proportion of the base particle group or the detergent particle group. Specifically, the coarse particle ratio of the detergent particle group or the base particle 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 still more preferably 10% by weight or less, and more preferably 5% by weight or less.

One of the features of the present invention is that even when a base particle group having a relatively high coarse particle ratio is used, the coarse particle ratio of the detergent particle group to be produced does not increase significantly. This feature can be clearly indicated by the "difference in the coarse particle ratio increase of the detergent particle group" defined below. In the present specification, the difference in the coarse particle ratio increase of the detergent particle group is defined as the result of subtracting the coarse particle ratio of the base particle group from the coarse particle ratio of the detergent particle group. Specifically, the difference in the coarse particle ratio of the detergent particle group of the present invention is preferably smaller, and is, for example, preferably 15% by weight or less, more preferably 10% by weight or less.

The bulk density of the detergent particle group is preferably from 300 to 2,000 g/L, more preferably from 500 to 1,500 g/L, and still more preferably from 600 to 1000 g/L. The method for measuring the bulk density of the detergent particle group is the same as the method for measuring the bulk density of the spray-dried base particle group (a).

In the detergent particle group obtained by the production method of the present invention having the above-described configuration, as described above, the growth of the particles is suppressed, and the particle size distribution is steep, and the detergent particles are excellent in appearance and solubility. group.

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

The 60 second dissolution rate of the detergent particle group was calculated by the following method.

Fill 1 liter of hard water (Ca/Mg molar ratio 7/3) equivalent to 71.2 mg CaCO ₃ / liter to 5 ° C. Fill a 1 liter beaker (cylinder with an inner diameter of 105 mm and a height of 150 mm, such as Yancheng) In a fixed state of a water temperature of 5 °C, a stirrer (35 mm in length and 8 mm in diameter, for example, model: ADVANTEC), trade name: Teflon (in the 1 liter beaker made by the company) Teflon) (registered trademark) SA (circular fine type) is stirred at a rotational speed (800 r/m) in which the depth of the vortex is approximately 1/3 with respect to the water depth. The detergent particle group was weighed to 1.0000 ± 0.0010 g, and the detergent particle group was weighed and stirred, and dispersed in water, and stirring was continued. 60 seconds after the input, the detergent particle group dispersion in the beaker was filtered using a standard sieve (diameter: 100 mm) of a mesh size of 7 μm as defined in JIS Z8801, which is known to have a hydration state remaining on the sieve. The particles of the agent are recovered together with the sieve into an open container of known weight. Further, the operation time from the start of filtration to the recovery of the sieve was set to 10 ± 2 seconds. The residue of the recovered detergent particles was dried by an electric dryer heated to 105 ° C for 1 hour, and then held in a desiccator (25 ° C) placed in a cerium oxide gel for 30 minutes and cooled. After cooling, the total weight of the dry detergent residue and the sieve and the recovery container is measured, and the dissolution rate (%) of the detergent particle group is calculated by the formula (4):

Dissolution rate (%) = {1 - (T / S)} × 100 (4)

S: input weight of detergent particle group (g)

T: dry weight (g) of the residue of the detergent particle group remaining on the sieve when the aqueous solution obtained by the above stirring conditions is supplied to the sieve.

Further, the detergent particle group of the present invention is excellent in cleanability. As an indicator of the cleanability in the present specification, the following method is used unless otherwise specified.

(Preparation of artificially contaminated cloth)

An artificially contaminated cloth was prepared by attaching an artificially contaminated liquid having the following composition to a cloth. The adhesion of the artificial contamination liquid to the cloth can be carried out by printing the artificial contamination liquid on the cloth using a gravure roll coater. The step of attaching the artificial contaminated liquid to the cloth to prepare the artificially contaminated cloth is based on the cell capacity of the gravure roll of 58 cm ³ /cm ² , the coating speed of 1.0 m/min, the drying temperature of 100 ° C, and the drying time of 1 minute. Under the conditions. The cloth was made of muslin 2003 cloth (made by Gutou Store).

Composition of artificial pollution liquid:

Lauric acid: 0.44% by weight

Myristic acid: 3.09 wt%

Fifteen carbonic acid: 2.31% by weight

Palmitic acid: 6.18% by weight

Heptadecanoic acid: 0.44% by weight

Stearic acid: 1.57 wt%

Oleic acid: 7.75 wt%

Triolein: 13.06% by weight

Cetyl palmitate: 2.18 wt%

Squalene: 6.53 wt%

Protein lecithin liquid crystal: 1.94% by weight

Luuma red clay: 8.11% by weight

Carbon black: 0.01% by weight

Tap water: balance

(cleaning conditions)

The washing was carried out using a Tergotometer under the conditions of a rotation speed of 85 r/m, a washing time of 10 minutes, a temperature of 20 ° C, a use of water of 4 ° DH (Ca/Mg = 3/1), and a concentration of detergent particles of 0.0667% by weight. Generally, the hardness component of the washing water is represented by Ca ²⁺ and Mg ²⁺ , and the weight ratio thereof is Ca/Mg=(60-85)/(40-15), and Ca/Mg=3/1 is used here. Model water. The term "4°DH" refers to the hardness when the molar amount of Mg ions is replaced by Ca.

(calculation of cleaning rate)

The reflectance at 550 mμ before and after the cleaning of the original cloth and before and after washing was measured by a self-recording color meter (manufactured by Shimadzu Corporation), and the cleaning rate D (%) was calculated by the following formula. The higher the cleaning rate, the cleaner the cleaning agent particle group:

D=(L2-L1)/(L0-L1)×100(%)

L0: reflectivity of the original cloth

L1: Reflectivity of contaminated cloth before cleaning

L2: Reflectivity of the contaminated cloth after cleaning.

[Examples]

The invention is further illustrated based on the following examples and the like. This embodiment is merely illustrative of the invention and does not represent any limitation. In addition, in the following examples and the like, the following components were used unless otherwise specified.

Sodium polyacrylate: weight average molecular weight 10,000 (made by Kao Corporation)

Zeolite: Zeobuilder (4A, manufactured by Zeobuilder; median particle size: 3.0 μm)

Clay mineral powder: Roundrojiru DGA powder; oil absorption capacity is 0.44 mL/g (manufactured by Sud-Chemi Co., Ltd.)

Light soda ash: average particle size 100 μm; oil absorption capacity is 0.45 mL/g (manufactured by Central Glass Co., Ltd.)

Sodium alkyl sulfate: the carbon number of the alkyl group is C12: C14: C16 = 67: 28: 5 (weight ratio)

Crystalline citrate: pre-feed granules (manufactured by Tokuyama Siltech Co., Ltd.)

Polyoxyethylene alkyl ether: Emulgen 106KH (manufactured by Kao Corporation).

Production Example 1: Production of spray-dried base particle group (a)

The spray-dried base particle group (a) was produced by the following procedure.

<Step (A-1)>

405 kg of water was added to a mixing tank of 1 m ³ with agitating blades, 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 the mixing tank. After stirring for 10 minutes, 137 kg of a 40% by weight aqueous sodium polyacrylate solution was added to the mixing tank. After further stirring for 10 minutes, 37 kg of sodium chloride and 120 kg of zeolite were added to the mixing tank, and the mixture was further stirred for 30 minutes to obtain a homogeneous slurry. The final temperature of the slurry was 58 °C.

The slurry was sprayed at a spray pressure of 2.5 MPa from a pressure spray nozzle provided near the top of the spray drying tower to produce a spray-dried base particle group (a). The high-temperature gas supplied to the spray drying tower was supplied from the lower portion of the column at a temperature of 235 ° C and discharged at 119 ° C from the top of the column. The moisture of the spray-dried base particle group (a) obtained was 0.15% by weight.

The obtained spray-dried base particle group (a) had physical properties of an average particle diameter 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 particle group (b-1)

The non-spray dried base particle group (b-1) was produced by the following procedure.

<Step (A-2)>

As powder raw material (a), 2.1 kg of clay mineral powder and 4.2 kg of light soda ash in a 75 L drum granulator with separator ( Φ 40 cm × L60 cm, rotation speed 30 r/m, Froude number 0.2 ) mixed. After mixing for 2 minutes, 2 fluid nozzles (manufactured by Spraying Systems Japan Co., Ltd.; spray spray pressure of 0.15 MPa / atomization air spray pressure of 0.3 MPa; all of which are gauge pressure) were used, and it took 5 minutes to make 25% by weight of polyacrylic acid. A 3.8 kg aqueous sodium solution was added to the granulator. After the addition, the mixture was further mixed and granulated for 3 minutes, and the obtained granules were discharged from a drum type granulator. The pellets were then dried using an electric dryer at 200 ° C for 3 hours. The moisture in the dried particle group (non-spray dried base particle group (b-1)) was 1.3% by weight.

The physical properties of the obtained non-spray-dried base particle group (b-1) were: an average particle diameter of 289 μm, a bulk density of 511 g/L, a coarse particle ratio of 12.2% by weight, and an oil absorption capacity of 0.51 mL/g.

Production Example 3: Production of non-spray dried base particle group (b-2)

The non-spray dried base particle group (b-2) was produced by the following procedure.

<Step (A-2)>

As the powder raw material (a), 4.55 kg of light soda ash was mixed in a 75 L drum type granulator ( Φ 40 cm × L60 cm, rotation speed 30 r/m, and Froude number 0.2) having a separator. After mixing for 2 minutes, a 2-fluid nozzle (manufactured by Atomax Co., Ltd.; a binder spray pressure of 0.15 MPa/micronized air spray pressure of 0.3 MPa; all of which is gauge pressure) was used, and it took 3.7 minutes to apply 40% by weight of sodium polyacrylate aqueous solution. 2.45 kg was added to the granulator. After the addition, the mixture was further mixed and granulated for 3 minutes, and the obtained granules were discharged from a drum type granulator. The pellets were then dried using an electric dryer at 200 ° C for 3 hours. The moisture in the dried particle group (non-spray dried base particle group (b-2)) was 1.8% by weight.

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

Examples 1 to 6 <Step (B)>

To an anionic surfactant paste containing 75 wt% of sodium alkyl sulfate and 25% by weight of water, 20 parts by weight (Example 1) and 30 parts by weight (Example 2) were added to 100 parts by weight of sodium alkyl sulfate (Example 2) Or 40 parts by weight of a mixture of 90% by weight of isodecyl glyceryl ether of Example 3 and 10% by weight of water; or 20 parts by weight (Example 4), 30 parts by weight (Example 5) or 40 parts by weight A mixture of 90% by weight of 2-ethylhexyl glyceryl ether (Example 6) and 10% by weight of water was mixed at a temperature of 60 ° C for 1 minute to obtain an anionic surfactant composition.

The viscosity of the anionic surfactant compositions of Example 1 and Example 4 was measured using MCR300 (manufactured by PHYSICA Messtechnik GmbH) at a temperature of 50 ° C and a shear rate of 10 [1/s], and found to be 12.2 Pa ‧ (Example) 1), 10.1 Pa‧s (Example 4).

<Step (C)>

33.9 parts by weight (Examples 1, 4) and 36.1 of the anionic surfactant composition prepared in the step (B) were added to 100 parts by weight (50 g) of the spray-dried base particle group (a) produced in Production Example 1. Parts by weight (Examples 2, 5) and 38.3 parts by weight (Examples 3 and 6) were mixed using a spatula for 10 minutes to obtain each mixture. The obtained mixture was observed, and as a result, no liquid was found in all the mixture, and the mixture formed a granulated substance without agglomerates.

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

Comparative example 1 <Step (C)>

29.5 parts by weight of an anionic surfactant paste containing 75% by weight of sodium alkyl sulfate and 25% by weight of water was added to 100 parts by weight (50 g) of the spray-dried base particle group (a) produced in Production Example 1, using a scraping The spoon took 10 minutes to mix and obtain a mixture. The obtained mixture was observed, and as a result, no liquid was observed, but a large amount of aggregate was observed.

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

Comparative example 2 <Step (B)>

To a mixture containing 75 wt% of sodium alkyl sulfate and 25% by weight of water, 25 parts by weight of polyoxyethylene alkyl ether based on 100 parts by weight of sodium alkyl sulfate was added, and the mixture was mixed at a temperature of 60 ° C for 1 minute to obtain Anionic surfactant composition. The viscosity of the obtained anionic surfactant composition was measured using a MCR300 (manufactured by PHYSICA Messtechnik GmbH) at a temperature of 50 ° C and a shear rate of 10 [1/s], and it was 11.2 Pa ‧ s.

<Step (C)>

To 100 parts by weight (50 g) of the spray-dried base particle group (a) produced in Production Example 1, 35.0 parts by weight of the anionic surfactant composition prepared in the step (B) was added, and it took 10 minutes to mix using a spatula. , to obtain a mixture. The obtained mixture was observed, and as a result, no liquid was observed, but a large amount of aggregate was observed.

The mixture obtained by the above operation was added to a polyethylene plastic bag containing 4.2 parts by weight of crystalline phthalate and 23.1 parts by weight of zeolite with respect to 100 parts by weight of the spray-dried base particle group (a). The polyethylene plastic bag was shaken up and down 30 times, and the surface of the granulated product (mixture) was modified to obtain a detergent particle group.

The physical properties and the like of the detergent particle groups obtained in Examples 1 to 6 and Comparative Examples 1 and 2 are shown in Table 1.

Example 7~10 <Step (B)>

To an anionic surfactant paste containing 75 wt% of sodium alkyl sulfate and 25% by weight of water, 20 parts by weight (Example 8) or 30 parts by weight based on 100 parts by weight of sodium alkyl sulfate was added (Example 7) a mixture of 90% by weight of isodecyl glyceryl ether and 10% by weight of water; or a mixture comprising 20 parts by weight (Examples 9, 10) of 2-ethylhexyl glyceryl ether 90% by weight and 10% by weight of water, The mixture was mixed at a temperature of 60 ° C for 1 minute to obtain an anionic surfactant composition.

<Step (C)>

The anionic surfactant composition prepared in the step (B) was added to the non-spray-dried base particle group (b-1) or (b-2) 100 parts by weight (50 g) manufactured in Production Example 2 or 3. Parts by weight (Example 7), 36.2 parts by weight (Examples 8 and 9), and 50.7 parts by weight (Example 10) were mixed using a spatula for 10 minutes to obtain each mixture. The obtained mixture was observed, and as a result, no liquid was found in all the mixture, and the mixture formed a granulated substance without agglomerates.

Adding each granule obtained by the above operation to 4.2 parts by weight of crystalline phthalate with respect to 100 parts by weight of the non-spray-dried base particle group (b-1) or (b-2) Zeolite 23.1 parts by weight in a polyethylene plastic bag. The polyethylene plastic bag was shaken up and down 30 times, and the surface of the granulated product (mixture) was modified to obtain each detergent particle group.

Comparative example 3~5 <Step (C)>

With respect to 100 parts by weight (50 g) of the non-spray-dried base particle group (b-1) or (b-2) produced in Production Example 2 or 3, 75 wt% of sodium alkyl sulfate and 25 wt% of water were added. 29.5 parts by weight of anionic surfactant paste (Comparative Example 3), 31.5 parts by weight (Comparative Example 4), and 44.1 parts by weight (Comparative Example 5) were mixed using a spatula for 10 minutes to obtain each mixture. The obtained mixture was observed, and as a result, no liquid was observed in all the mixture, but a large amount of aggregate was observed.

Adding each granule obtained by the above operation to 4.2 parts by weight of crystalline phthalate with respect to 100 parts by weight of the non-spray-dried base particle group (b-1) or (b-2) Zeolite 23.1 parts by weight in a polyethylene plastic bag. The polyethylene plastic bag was shaken up and down 30 times, and the surface of the granulated product (mixture) was modified to obtain each detergent particle group.

The physical properties and the like of the detergent particle groups obtained in Examples 7 to 10 and Comparative Examples 3 to 5 are shown in Table 2.

In Table 1, the results of using the spray-dried base particle group (a) are summarized. As is clear from Table 1, the coarse particle ratio of the detergent particle group obtained in Examples 1 to 6 and the difference in the coarse particle ratio of the detergent particle group, the particle formation length, and the solubility were compared with those of Comparative Examples 1 and 2. The cleaning property was good, and it was found from the observation results of the obtained detergent particle group that the cleaning agent particle group having less aggregates can be produced by the production method of the present invention. From the comparison of Examples 1 to 6 and Comparative Example 2, it was found that when only a nonionic surfactant (polyoxyethylene alkyl ether in Comparative Example 2) and an anionic surfactant paste were mixed, a specific effect could not be exhibited. The specific effect is exerted by using an alkyl glyceryl ether as defined in the present case.

Further, in Table 2, the results of using the non-spray dried base particle group (b-1) or (b-2) were summarized. As is clear from Table 2, the coarse particle ratio of the detergent particle group obtained in Examples 7 to 10, the difference in the coarse particle ratio of the detergent particle group, the particle formation length, and the solubility were compared with those of Comparative Examples 3 to 5. The cleaning property was good, and it was found from the observation results of the obtained detergent particle group that the cleaning agent particle group having less aggregates can be produced by the production method of the present invention. Further, it is understood that although the non-spray-dried base particle group (b-1) or (b-2) tends to have a higher coarse particle ratio than the spray-dried base particle group (a), even if such (b- In the case of 1) or (b-2), the difference in the coarse particle ratio of the detergent particle group is also small. This shows that, according to the production method of the present invention, it is possible to produce a detergent particle group in which the increase in the coarse particle ratio is suppressed regardless of the difference in the coarse particle ratio of the base particle group to be used.

Industrial availability

Since the detergent particle group of the present invention has a steep particle size distribution, a small amount of aggregates, and excellent solubility, it can be suitably used for, for example, a detergent for clothing, a detergent for dishwashing, and the like.

Claims (12)

A method for producing a detergent particle group, comprising the steps of: step (B): mixing an anionic surfactant paste with an alkyl glyceryl ether to prepare an anionic surfactant composition; and step (C): step ( The anionic surfactant composition prepared in B) is mixed with a base particle group having an oil absorption capacity of 0.2 mL/g or more to prepare a detergent particle group, wherein the anionic surfactant is selected from the group consisting of alkyl sulfates and alkyl groups. One or more groups consisting of a sulfate salt, an α-sulfo fatty acid ester salt, an α-olefin sulfonate, and a polyoxyethylene alkyl sulfate salt, and the above alkyl glyceryl ether is the following general formula (3) And 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). The manufacturing method of claim 1, wherein the particle size of the detergent particle group produced by the following formula (1) is 1.25 or less: particle length = [average particle diameter of the detergent particle group] / [basis Average particle size of the particle group] (1). The production method of claim 1, wherein 10 to 40 parts by weight of the alkyl glyceryl ether is mixed with respect to 100 parts by weight of the anionic surfactant in the anionic surfactant paste. The production method of claim 1, wherein 5 to 100 parts by weight of the anionic surfactant composition is mixed with respect to 100 parts by weight of the base particle group. The method of claim 1, wherein the base particle group is prepared by a method comprising any of the following steps: Step (A-1): spray drying a slurry containing a water-soluble inorganic salt to obtain a base particle group; or Step (A-2): in a container rotary granulator, using a multi-fluid nozzle to absorb oil A detergent agent is added to the powder raw material of 0.4 mL/g or more and granulated to obtain a base particle group. The method of claim 1, wherein the anionic surfactant is represented by the following formula (2): RO-SO ₃ M (2) (wherein R represents an alkyl group or an alkenyl group having 10 to 18 carbon atoms; M represents an alkali metal atom or ammonium). The process of claim 1, wherein the alkyl glyceryl ether is isodecyl glyceryl ether and/or 2-ethylhexyl glyceryl ether. The method of claim 1, wherein the content of water in the anionic surfactant paste is 15 to 50% by weight. The method of claim 1, wherein the anionic surfactant composition has a viscosity (50 ° C) of 0.01 to 20 Pa ‧ . The manufacturing method of claim 1, wherein the base particle group has an oil absorption capacity of 0.7 mL/g or less. The manufacturing method of claim 1, wherein the basic particle group has an average particle diameter of 140 to 600 μm. The manufacturing method of claim 5, wherein the oil-absorbing ability of the powder raw material for detergent is 1.0 mL/g or less.