JP5465872B2 - Anionic surfactant composition - Google Patents

Description

  The present invention relates to an anionic surfactant composition having a viscosity that is low enough to handle even if the concentration of the anionic surfactant is high, and a method for producing a detergent particle group using the composition.

Examples of conventionally known high concentration anionic surfactant compositions in paste form include, for example, an anionic surfactant which is stable at a high concentration and has a low viscosity, and a polyethylene glycol having an average molecular weight of 1,000 to 20,000. A paste containing higher alcohol and / or its ethoxylate, sodium sulfate and an alkaline substance in a specific ratio (Patent Document 1), and a liquid aqueous concentrated alkyl sulfate composition comprising alcohol ethoxylate and alcohol ethoxy sulfate And a paste made of a composition containing a polyethylene glycol or polypropylene glycol, a polyethylene glycol or a sulfate of polypropylene glycol (Patent Document 2).
Japanese Patent Laid-Open No. 5-93199 Japanese Patent Laid-Open No. 5-140586

  However, the viscosities of the compositions disclosed in Patent Document 1 and Patent Document 2 are not yet satisfactory. In addition, when a detergent particle group is produced using such a composition, a large amount of agglomerates of detergent particles are formed in the resulting detergent particle group, so the solubility is poor, and this point is still unsatisfactory. It was not a level to go.

  Accordingly, an object of the present invention is to provide an anionic surfactant composition that is easy to handle at a shear rate applied during pumping or granulation, even if the composition is an aqueous paste and has a high concentration of anionic surfactant. Is to provide. Furthermore, an object of the present invention is a method for producing a detergent particle group using an anionic surfactant composition having a high concentration of such an anionic surfactant, wherein the resulting detergent particle group has few aggregates of detergent particles and dissolves. It is to provide a method for producing detergent particles having good properties.

That is, the present invention
[1] An anionic surfactant composition containing a hydroxycarboxylic acid ester and / or a monohydric alcohol having 3 to 8 carbon atoms and an anionic surfactant of 50 to 90% by weight;
[2] The following process:
Step (A): Step of preparing a surfactant-supporting granule group, Step (B): Hydroxycarboxylic acid ester and / or monovalent alcohol having 3 to 8 carbon atoms, and anionic surfactant 50 to 90% by weight A step of preparing an anionic surfactant composition, step (C): a granule group for supporting a surfactant prepared in step (A), and an anionic surfactant prepared in step (B) A step of mixing the composition to obtain a mixture, and step (D): a step of surface-modifying the mixture obtained in step (C) to obtain detergent particles,
And a detergent particle group obtained by the production method according to [2] above.

  The anionic surfactant composition of the present invention has a low viscosity by containing a hydroxycarboxylic acid ester and / or a monohydric alcohol having 3 to 8 carbon atoms in spite of a high concentration of the anionic surfactant. Therefore, it is excellent in handling properties when manufacturing detergent particles. Furthermore, the detergent particle group obtained by using such an anionic surfactant composition is one in which aggregation and consolidation of particles are suppressed, and as a result, an effect of increasing the bulk density (compacting) and improving solubility. Is played.

1. Anionic surfactant composition The anionic surfactant composition of the present invention contains a hydroxycarboxylic acid ester and / or a monovalent alcohol having 3 to 8 carbon atoms, and an anionic surfactant of 50 to 90% by weight. One feature of the anionic surfactant composition of the present invention is that it contains a hydroxycarboxylic acid ester and / or a monohydric alcohol having 3 to 8 carbon atoms (both components are collectively referred to as “viscosity modifier”). And By containing a predetermined amount of such a viscosity modifier, there is an effect that the viscosity can be reduced even if the concentration of the anionic surfactant composition is high. In addition, unless otherwise specified, the percentage display of the content of each component described below and the blending amount is weight%.

  As the anionic surfactant contained in the composition of the present invention, 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 Examples thereof include sulfate ester salts, fatty acid monoglyceride sulfate esters 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 are alkyl sulfates, alkyl sulfate esters, α-sulfo fatty acid ester salts, α-olefin sulfonates, polyoxyethylene alkyl sulfate esters, and the like. . Alkyl sulfates and / or alkyl sulfates are more preferable in that a remarkable effect can be obtained.

  The content of the anionic surfactant used in the present invention in the anionic surfactant composition is 50 to 90%, preferably 60 to 85%, more preferably 65 to 80%. Within this range, a low-viscosity aqueous paste-like composition that can be handled can be obtained on an industrial scale even when the anionic surfactant is in a high concentration.

  The hydroxycarboxylic acid ester used in the composition of the present invention is an ester compound having a hydroxy group, such as lactic acid ester, malic acid ester, tartaric acid ester, citric acid ester, glycol monoester, glycerin monoester, glycerin diester. And ricinoleic acid ester and castor oil. As such hydroxycarboxylic acid ester, one kind can be used alone, or a plurality of kinds can be used in combination. More preferable hydroxycarboxylic acid esters include lactic acid esters specified by the following general formula (1).

CH ₃ CH (OH) COOR (1)
(In the formula, R represents a hydrocarbon group having 1 to 16 carbon atoms, preferably an alkyl group, alkenyl group or cycloalkyl group having 1 to 16 carbon atoms.)

  Specific examples of the lactic acid ester include methyl lactate, ethyl lactate, propyl lactate, butyl lactate, pentyl lactate, hexyl lactate, and tetradecyl lactate. Among these, more preferred lactate esters are methyl lactate, ethyl lactate, propyl lactate and butyl lactate, and even more preferred is ethyl lactate.

  The monohydric alcohol having 3 to 8 carbon atoms used in the composition of the present invention may have a linear structure or a branched structure. For example, 1-propanol, 2-methyl-2-propanol, Isopropanol, 1-butanol, 2-butanol, 2-methyl-2-butanol, 1-pentanol, 2-methyl-2-pentanol, 1-hexanol, 2-ethyl-1-hexanol, 1-heptanol and 1- Examples include octanol. As such monohydric alcohol, one kind can be used alone, or a plurality of kinds can be used in combination. More preferable monohydric alcohols include 1-propanol, isopropanol, 1-butanol, and 1-hexanol.

  The content of the viscosity modifier in the composition of the present invention, that is, the content of the hydroxycarboxylic acid ester and / or the monohydric alcohol having 3 to 8 carbon atoms is 100 weights of the anionic surfactant in the composition of the present invention. 1 to 80 parts by weight is preferred, 10 to 60 parts by weight is more preferred, and 20 to 50 parts by weight is even more preferred. From the viewpoint of handling the anionic surfactant composition, the content is preferably 1 part by weight or more. From the viewpoint of the effective amount of the anionic surfactant that can be supported on the granules and the cost of the viscosity modifier, the content is 80 parts. Part by weight or less is preferred. A hydroxycarboxylic acid ester and a monohydric alcohol having 3 to 8 carbon atoms may be used in combination as a viscosity modifier, and there is no particular limitation on the use ratio of both in the case of using both in this way. The ratio can be used. Therefore, when using both together, content of hydroxycarboxylic acid ester and / or C3-C8 monohydric alcohol turns into total content of both.

  The viscosity of the anionic surfactant composition of the present invention is preferably lower from the viewpoint of handling. For example, when the temperature is 50 ° C., the following viscosity range is preferable. For example, when the shear rate is 0.1 [1 / s], it is preferably 1 mPa · s or more and 1500 Pa · s or less, and more preferably 1000 Pa · s or less. When the shear rate is 1.0 [1 / s], 100 Pa · s or less is preferable, and 50 Pa · s or less is more preferable. When the shear rate is 10.0 [1 / s], it is preferably 8.0 Pa · s or less, and more preferably 6.0 Pa · s or less. In the present specification, the viscosity of the anionic surfactant composition is determined using MCR300 (manufactured by PHYSICA Messtechnik GmbH, rotor: cone plate (cp50-1)) at a temperature of 50 ° C. and a shear rate of 0.1 to 10 [1 / s] to determine.

  The anionic surfactant composition of the present invention can be prepared by mixing a predetermined amount of an anionic surfactant, a predetermined amount of a viscosity modifier and water. You may add components other than these components as needed.

2. Manufacturing method of detergent particle group The manufacturing method of the detergent particle group of the present invention includes the following steps:
Step (A): Step of preparing a granule group for supporting a surfactant,
Step (B): a step of preparing an anionic surfactant composition containing a hydroxycarboxylic acid ester and / or a monovalent alcohol having 3 to 8 carbon atoms and an anionic surfactant of 50 to 90% by weight,
Step (C): Step of obtaining a mixture by mixing the surfactant-supporting granule group prepared in Step (A) with the anionic surfactant composition prepared in Step (B), and Step (D) ): A step of surface-modifying the mixture obtained in step (C) to obtain detergent particles.

<Process (A)>
Examples of the granule group for supporting a surfactant used in the step (A) of the present invention include a granule group capable of supporting a surfactant. More specifically, the following spray-dried base granules (a) and non-jet-dried base granules (b) can be mentioned.

(Preparation of spray-dried base granules (a))
The spray-dried base granule (a) is a granule obtained by spray-drying a slurry containing a water-soluble inorganic salt. For example, by spray-drying a slurry containing the following components, the spray-dried base granule (a) Can be prepared.

  Although it does not specifically limit as water-soluble inorganic salt, For example, sodium carbonate, potassium carbonate, sodium sulfate, sodium sulfite, sodium chloride, etc. 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.

  Among them, it is preferable to use zeolite together with a water-soluble inorganic salt. When the zeolite is blended, the water content in the spray-dried base granule (a) after spray drying is preferably 5% or less of the spray-dried base granule (a) from the viewpoint of increasing the action of the zeolite to adsorb water. 3% or less is more 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.

[Physical properties of spray-dried base granules (a)]
The carrying capacity of the spray-dried base granule (a) is preferably 20 mL / 100 g or more, more preferably 30 mL / 100 g or more. Moreover, as a preferable upper limit of carrying ability, it is 70 mL / 100g or less. In this range, aggregation of the spray-dried base granules (a) is suppressed, which is suitable for suppressing particle growth of the particles in the detergent particle group.

  The measuring method of the carrying ability of the spray-dried base granule (a) is as follows. 100 g of a sample (spray-dried base granule (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. 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 input amount of linseed oil when the stirring power becomes the highest is defined as the carrying capacity (mL / 100 g).

  The bulk density of the spray-dried base granule (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 (a) is measured by the method defined in JIS K3362 unless otherwise specified.

  The average particle size of the spray-dried base granule (a) is preferably 150 to 500 μm, more preferably 180 to 300 μm. In this specification, the average particle sizes of the detergent particles, the surfactant-supporting granules, the powder raw material (a), the spray-dried base granules (a) and the non-jet-dried base granules (b) are unless otherwise specified. Using a sieve specified in JIS Z 8801, it is obtained as follows.

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 (a) is measured by the following infrared moisture meter method. That is, 3 g of a sample (jet drying base granule (a)) is weighed on a sample pan having a known weight, and the sample is heated and dried for 3 minutes by an infrared moisture meter (Infrared lamp 185 W manufactured by Kett Science Laboratory Co., Ltd.). 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.

(Preparation of non-sprayed base granule (b))
Non-sprayed base granule (b) means, for example, adding water or an aqueous binder solution to “a powder raw material having an oil absorption capacity of 0.4 mL / g or more excluding clay mineral powder” (referred to as “powder raw material (a)”). Thus, it is a granule obtained by a method including a step of obtaining a granule. Non-jet drying base granule (b) also includes a granule obtained by a method including a step of obtaining granules by adding water or an aqueous binder solution to a mixture of powder raw material (a) and clay mineral powder. The structure is considered to be a structure in which the powder raw material (a) is gently aggregated or a structure in which the powder raw material (a) and the clay mineral powder are gradually aggregated.

  Examples of the clay mineral powder that can be used in the present invention include talc, pyrophyllite, smectite (saponite, hectorite, saconite, stevensite, montmorillonite, beidellite, nontronite, etc.), vermiculite, mica (phlogopite, biotite, biotite). ), Chinwald mica, muscovite, paragonite, ceradonite, sea chlorite, etc.), Chlorite (clinochlore, chamosite, nimite, penantite, Sudowite, Dongbasite, etc.), brittle mica (Clintnite, margarite, etc.), sulite, serpentine Stone minerals (antigolite, lizardite, chrysotile, amesite, cronstedite, burcherin, greenerite, garnierite, etc.), kaolin minerals (kaolinite, dickite, nacrite, halloysite, etc.) It is below. These can be used alone or in combination of a plurality of types. 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. The average particle size of the clay mineral powder is the average particle size obtained by dispersing the particles in a solvent that does not dissolve the particles using a laser diffraction / scattering particle size distribution analyzer LA-920 (manufactured by Horiba, Ltd.). Asking.

  In the powder raw material (a) that can be used in the present invention, the oil absorption capacity is a value determined by the following evaluation method.

  That is, 30 to 35 g of a sample (powder raw material (a)) was put into an absorption measuring device (S410 manufactured by Asahi Research Institute), and the driving blade was 200 r. p. m. Rotate with 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.

  The powder raw material (a) is an essentially porous substance having fine pores of 10 μm or less inside, and a substance capable of supporting a surfactant in the pores. In addition, although the upper limit of oil absorption ability is not specifically limited, For example, it is desirable that it is 1.0 mL / g or less.

  From the viewpoint of granulation, the average particle diameter of the powder raw material (a) is preferably 50 to 250 μm, more preferably 50 to 200 μm, and further preferably 80 to 200 μm. From the viewpoint of solubility, the powder raw material (a) is preferably a water-soluble substance.

  Examples of the powder raw material (a) include light ash or soda ash prepared by baking sodium bicarbonate, sodium silicate, porous powder prepared by drying trihydrate of sodium triphosphate. From the viewpoint of ease of handling and availability, light ash is more preferable.

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

  When the clay mineral powder and the powder raw material (a) are used in combination, the weight ratio of the clay mineral powder and the powder raw material (a) (clay mineral powder / powder raw material) is preferably 1/1 to 1/30, More preferably, it is 1/1 to 1/20, and more preferably 1/2 to 1/20.

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

  As the mixing method used in the step of obtaining the mixture by mixing the powder raw material (a), or the clay mineral powder and the powder raw material (a), and further mixing other components as necessary, both are preferably substantially uniform. If it is a method which can be mixed, it will not specifically limit. For example, it may be mixed using a low shear granulator, or may be mixed in advance using another mixer and then transferred to a low shear granulator. Other mixers used for this operation include, for example, a drum type mixer (manufactured by Nikko Corporation), a bread type mixer (manufactured by Fuji Machine Co., Ltd.), and a ribbon mixer (manufactured by Hiwa Machine Industry Co., Ltd.) , Nauter mixer (manufactured by Hosokawa Micron Corporation), Shugi mixer (Pauleck Co., Ltd.), Redige mixer (manufactured by Matsubo Co., Ltd.), high speed mixer (manufactured by Fukae Kogyo Co., Ltd.) and the like.

  Next, water or an aqueous binder solution is added to the resulting mixture to obtain granules. The concentration of the aqueous binder solution is not particularly limited, but the particle size at the time of granulation of the non-spray-dried base granule (b) is greatly affected by the volume of the aqueous binder solution. What is necessary is just to determine a density | concentration. Specific examples of the binder herein include polyethylene glycol, polypropylene glycol, polyoxyethylene alkyl ether and derivatives thereof, polyvinyl alcohol and derivatives thereof, and water-soluble cellulose derivatives (these derivatives include ether compounds and the like. ), Organic polymers such as carboxylic acid polymers, starches and saccharides, and inorganic polymers such as amorphous silicates. From the viewpoint of caking property and detergency, water-soluble cellulose derivatives, saccharides and carboxylic acid polymers are preferable, and salts of acrylic acid-maleic acid copolymers and polyacrylates are more preferable. The salt is preferably a sodium salt, potassium salt or ammonium salt. In addition, as a weight average molecular weight of a carboxylic acid-type polymer, 1000-100000 are preferable and 2000-80000 are more preferable.

  The content of the binder in the non-sprayed base granule (b) is preferably 0 to 35% by weight, and preferably 5 to 30% by weight in the non-sprayed base granule (b) from the viewpoints of caking property and oil absorption. More preferably, 8 to 20% by weight is further preferable, and 10 to 20% by weight is more preferable.

  Examples of the method for obtaining the granule include a method of granulating each component with a low shear granulator. In this way, a granule having a structure in which the powder raw material (a) is gently aggregated, or a granule having a structure in which the clay mineral powder and the powder raw material (a) are gently aggregated is prepared as a non-spray-dried base granule (b). .

[Physical properties of non-sprayed base granule (b)]
The non-jet drying base granule (b) is a granule having a structure in which the powder raw material (a) is gently aggregated, or a granule having a structure in which the clay mineral powder and the powder raw material (a) are gently aggregated. Therefore, it has three supporting sites: (1) large gaps between granules, (2) small gaps of 10 μm or less in the powder raw material (a), and (3) clay mineral powder layers. By adjusting the three loading sites, a non-sprayed base granule (b) having a desired loading ability can be obtained.

  30 mL / 100g or more is preferable and, as for the carrying ability of a non-jet drying base granule (b), 40 mL / 100g or more is more preferable. On the other hand, the carrying ability is preferably 70 mL / 100 g or less. In such a range, aggregation of the non-sprayed base granules (b) is suppressed, which is preferable because the degree of particle growth of the particles in the detergent particle group can be suppressed. The measuring method of the supporting ability of the non-sprayed base granule (b) is the same as the measuring method of the supporting ability of the spray-dried base granule (a).

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

  The average particle size of the non-jet dried base granule (b) is preferably 140 to 600 μm, more preferably 200 to 500 μm. In the present specification, the method for measuring the average particle size of the non-jet dried base granule (b) is the same as the method for measuring the average particle size of the spray dried base granule (a).

  The method for measuring the water content in the non-sprayed base granule (b) is the same as the method for measuring the water content in the spray-dried base granule (a).

<Process (B)>
Step (B) is a step of preparing an anionic surfactant composition containing a hydroxycarboxylic acid ester and / or a monovalent alcohol having 3 to 8 carbon atoms and an anionic surfactant of 50 to 90% by weight. is there. The anionic surfactant composition prepared by this step is the above-described anionic surfactant composition of the present invention. Therefore, in the method of the present invention, the anionic surfactant composition prepared in step (B) is used. As described above, the anionic surfactant composition of the present invention can be used as it is.

  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. Examples thereof include those enumerated in the description of the anionic surfactant composition of the present invention. 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 are alkyl sulfates, alkyl sulfate esters, α-sulfo fatty acid ester salts, α-olefin sulfonates, polyoxyethylene alkyl sulfate esters, and the like. . Alkyl sulfates and / or alkyl sulfates are more preferable in that a remarkable effect can be obtained.

  The content of the anionic surfactant used in this step in the composition is 50 to 90%, preferably 60 to 85%, more preferably 65 to 85%. Within this range, a low-viscosity aqueous paste-like composition that can be handled can be obtained on an industrial scale even when the anionic surfactant is in a high concentration.

  The hydroxycarboxylic acid ester used in this step is an ester compound having a hydroxy group, and examples thereof include those listed in the description of the anionic surfactant composition of the present invention. As such hydroxycarboxylic acid ester, one kind can be used alone, or a plurality of kinds can be used in combination. More preferable hydroxycarboxylic acid esters include lactic acid esters specified by the following general formula (1).

CH ₃ CH (OH) COOR (1)
(In the formula, R represents a hydrocarbon group having 1 to 16 carbon atoms, preferably an alkyl group, alkenyl group or cycloalkyl group having 1 to 16 carbon atoms.)

  Specific examples of the lactic acid ester include those listed in the description of the anionic surfactant composition of the present invention. Among these, more preferred lactate esters are methyl lactate, ethyl lactate, propyl lactate and butyl lactate, and even more preferred is ethyl lactate.

  The monovalent alcohol having 3 to 8 carbon atoms used in this step may be a linear structure or a branched structure, and examples thereof include those listed in the description of the anionic surfactant composition of the present invention. Can be mentioned. As such monohydric alcohol, one kind can be used alone, or a plurality of kinds can be used in combination. More preferable monohydric alcohols include 1-propanol, isopropanol, 1-butanol, and 1-hexanol.

  The content of the viscosity modifier in this step, that is, the total content of both the hydroxycarboxylic acid ester and / or the monovalent alcohol having 3 to 8 carbon atoms is the anionic surface activity in the composition prepared in this step. The amount is preferably 1 to 30 parts by weight, more preferably 5 to 25 parts by weight, and still more preferably 6 to 20 parts by weight with respect to 100 parts by weight of the agent. In addition, you may use combining a hydroxycarboxylic acid ester and C3-C8 monohydric alcohol as a viscosity modifier, and there is no restriction | limiting in particular in the usage ratio of both in this case, It is used by arbitrary ratios. it can.

  The viscosity of the anionic surfactant composition prepared in this step is preferably lower from the viewpoint of handling. The specific viscosity is the same as the viscosity of the anionic surfactant composition of the present invention.

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

<Process (C)>
Step (C) is a step of obtaining a mixture by mixing the surfactant-carrying granule group prepared in step (A) and the anionic surfactant composition prepared in step (B). The mixture obtained by this step may form a granulated product.

  As a mixer for mixing the anionic surfactant composition and the surfactant-supporting granule group used in the step (C), for example, a nozzle for adding the surfactant composition or a temperature in the mixer is used. Those with a jacket for control are preferred.

  The ratio of the two components when mixing the surfactant-carrying granule group and the anionic surfactant composition is not particularly limited as long as a uniform mixture is obtained. For example, the surfactant-carrying granule group 100 It is preferable that an anionic surfactant composition is 5-100 weight part with respect to a weight part, It is more preferable that it is 10-90 weight part, It is further more preferable that it is 20-70 weight part, 30-60 More preferred are parts by weight. From the viewpoint of detergency, the anionic surfactant composition is preferably 5 parts by weight or more with respect to 100 parts by weight of the granules, and from the viewpoint of the degree of freedom in composition and solubility, On the other hand, the anionic surfactant composition is preferably 100 parts by weight or less.

  As the mixing condition in the step (C), a mixing condition that substantially maintains the morphology of the surfactant-supporting 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 a mixer equipped with a stirring blade is used, the viewpoint of suppressing the disintegration of the particles for supporting the surfactant and the mixing efficiency From the viewpoint, when the shape of the mixing blade of the stirring blade provided in the machine 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, More preferably, it is 0.5-2.0. Moreover, when the shape of the said mixing blade is a screw type, the fluid number of the said stirring blade becomes like this. Preferably it is 0.1-4.0, More preferably, it is 0.15-2.0. Moreover, when the shape of the said mixing blade is a ribbon type, the fluid number of the said stirring blade becomes like this. Preferably it is 0.05-4.0, More preferably, it is 0.1-2.0.

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 or crushing blade, R represents the rotational radius [m] of the stirring blade or crushing blade, and g represents the acceleration of gravity [m / s ² ].)

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

  The powder raw material other than the surfactant-supporting granule group referred to in the present specification means a powder cleaning strength enhancer or an oil absorbing agent 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 together with a surfactant-supporting granule group as desired, an anionic surfactant composition can be highly compounded and the adhesion of the mixture to the mixer can be reduced, and the cleaning power can be improved. Can also be planned. As such a powder raw material, one type can be used alone, or a plurality of types can be used in combination.

  Preferably, after mixing the anionic surfactant composition and the surfactant-supporting granules, polyethylene glycol (PEG) and / or fatty acid and / or soapy water is preferably added to 100 parts by weight of the surfactant-supporting granules. The surface of the granule group for supporting a surfactant may be coated by adding 1 to 10 parts by weight and further mixing. This coating is preferred because the caking resistance of the detergent particles is improved. Furthermore, the addition of PEG and / or fatty acid and / or soapy water makes it possible to suppress aggregation and enhance dispersibility when dissolving the detergent particles, resulting in improved solubility of the detergent particles. This is preferable.

  In addition, as the temperature in the mixer during mixing, the anionic surfactant composition and the surfactant-carrying granule group can be efficiently mixed while substantially suppressing the collapse of the surfactant-carrying granule group. Temperature is preferred. 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. Moreover, as mixing time at the time of mixing, about 2 to 20 minutes are preferable, and about 2 to 10 minutes are further more preferable. 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 surfactant-supporting granule group may be a batch type or a continuous type. When mixing batchwise, it is preferable to add the anionic surfactant composition after the surfactant-supporting granule group is previously charged in 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 Application Laid-Open No. 10-296065, etc. (2) As a mixer with a mixing blade shape of a ribbon type, a cylindrical, semi-cylindrical or conical type is fixed. Mixer that mixes by rotating ribbon-shaped blades that form spirals in a container that has been rotated: Ribbon mixer (manufactured by Hiwa Machinery 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. .

  Further, in the case of continuous mixing, there is no particular limitation as long as it is a continuous mixer that is generally used for continuous mixing. For example, a surfactant is supported using a continuous apparatus among the above mixers. You may mix the granule group for use and an anionic surfactant composition.

<Process (D)>
Step (D) is a step of obtaining detergent particles by surface-modifying the mixture obtained by mixing in step (C). By performing this step (D), 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 or the like. When fine powder or the like is used, surface modification can be performed by mixing the mixture obtained in step (C) with the fine powder or the like 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 average particle diameter of the fine powder is determined by a method using light scattering.

  The amount of the fine powder used is preferably 0.5 to 40.0 parts by weight with respect to 100 parts by weight of the surfactant-carrying granules prepared in the step (A) from the viewpoint of fluidity and usability. More preferably, it is 1-30 weight part.

  What is necessary is just to select the mixing conditions which can maintain substantially the form of the granule group for surfactant holding containing an anionic surfactant composition as mixing conditions in a process (D). 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. When such a mixer is used, the fluid number of the stirring blade provided in the apparatus is preferably 10 or less, more preferably 7 or less, from the viewpoint of suppressing the collapse of the surfactant-supporting granules. 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 (A), one equipped with both a stirring blade and a crushing blade can be mentioned. Moreover, the temperature adjustment of the substance mixed becomes easy by implementing a process (A) and a process (D) using a respectively different mixer. For example, when non-heat resistant components such as fragrances and enzymes are added during or after the step (D), it is preferable to adjust the temperature of the mixture in the step (D). The temperature can be adjusted by setting the jacket temperature and venting. In order to efficiently transfer the mixture obtained in the step (C) to the apparatus in the step (D), it is also a preferable aspect that a part of the fine powder is added to the mixture at the end of the step (C).

3. 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 surfactant-supporting granule group as a core, and substantially 1 in one detergent particle. A detergent particle group having a feature of having a group of granules for supporting a surfactant as a core is preferable.

As an index representing such characteristics of the detergent particles, the following formula (2):
Degree of particle growth = [average particle diameter of detergent particles obtained in step (D)] / [average particle diameter of granules for supporting surfactant] (2)
Can be used. Specifically, a detergent particle group having a particle growth degree of 1.5 or less is preferable, 1.4 or less is more preferable, and 1.3 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.

  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.

  As an average particle diameter of the detergent particle group of this invention, 150 micrometers or more are preferable, the range of 150-500 micrometers is more preferable, and the range of 180-350 micrometers is further more preferable. In this specification, the average particle diameter of the detergent particles is the same as the method for measuring the average particle diameter of the spray-dried base granules (a).

  The coarse particle ratio of the detergent particles of the present invention is very small. In the present specification, the coarse particle ratio of the detergent particle group is defined as the weight percentage of the proportion of particles having a size of 500 μm or more in the detergent particle group. Specifically, the coarse particle ratio of the detergent particle group of the present invention is preferably 15% or less, and more preferably 10% or less.

  The yield of the detergent particle group of the present invention is calculated by dividing the weight of the sample (detergent particle group) that has passed through a sieve having an opening of 1180 μm by the weight of the entire sample. The yield of the detergent particle group of the present invention is preferably 90% or more, and more preferably 95% or more.

  The bulk density of the detergent particle group 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 granule (a).

  The anionic surfactant composition of the present invention and a detergent particle group obtained using the composition, particularly a detergent particle group obtained by further modifying the surface of such a composition are excellent in solubility. As the solubility index in this specification, the following method is used unless otherwise specified.

Tap water, ion-exchanged water or 25 ° C. corresponding to a hardness of 71.2 mg CaCO ₃ / liter, 1 liter of hard water (Ca / Mg molar ratio 7/3), 1 liter beaker (inner diameter 105 mm, height 150 mm cylindrical type) For example, 1 liter glass beaker manufactured by Iwaki Glass Co., Ltd.). With a water temperature of 25 ° C. kept constant in a water bath, the number of revolutions (700 r.p.) with a stirrer (length: 30 mm, for example, model: ADVANTEC, Teflon (registered trademark) SA (round thin type)) M.) Stir the water. A sample (for example, an anionic surfactant composition or detergent particle group) that has been reduced and weighed to an appropriate amount is charged and dispersed in the water in the beaker while stirring, and stirring is continued. Using an electrical conductivity meter (D-54, manufactured by Horiba, Ltd.), the electrical conductivity over time is measured, and the dissolution rate at a specific time is calculated by the following equation (3). By measuring the time for the dissolution rate to reach 100%, the solubility of the sample can be evaluated.

Dissolution rate [%] = [(TZ) / (S−Z)] × 100 (3)
T: electrical conductivity at a specific time Z: electrical conductivity before sample introduction S: electrical conductivity at complete dissolution

The present invention will be further described based on the following examples. 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 (manufactured by Sud Kemi)
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 carbon number of C12: C14: C16 = 67: 28: 5 (molar ratio) Sodium alkyl sulfate ester (polyoxyethylene lauryl ether sodium sulfate): The average number of added moles of ethylene oxide is 2 PEG400: Polyethylene glycol (weight average molecular weight 10,000)
Crystalline silicate: Pre-feed granule (manufactured by Tokuyama Siltech)

Production Example 1: Production of spray-dried base granule (a) The spray-dried base granule (a) was produced by the following procedure.
<Process (A)>
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% 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 the mixture was further stirred for 30 minutes to obtain a homogeneous slurry. The final temperature of this slurry was 58 ° C.

This slurry was sprayed at a spray pressure of 25 kg / cm ³ from a pressure spray nozzle installed near the top of the spray drying tower to produce spray-dried base granules (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 (a) was 0.15%.

  The physical properties of the obtained spray-dried base granule (a) were an average particle diameter of 257 μm, a bulk density of 538 g / L, and a supporting capacity of 45 mL / 100 g.

Production Example 2: Production of non-sprayed base granule (b) A non-sprayed base granule (b) was produced by the following procedure.
<Process (A)>
Clay mineral powder 2.1 kg and light ash 4.2 kg (clay mineral powder / powder raw material = 1/2) as a powder raw material were mixed into a 70 L drum granulator (φ40 cm × L60 cm / rotation number 32 r. pm / Froude number 0.23). After mixing for 2 minutes, 3.8 kg of 25% 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). And added to the granulator over 5 minutes. After the addition, the mixture was further mixed and granulated for 3 minutes, and the obtained granule was discharged from the drum granulator. The granules were then dried for 3 hours at 200 ° C. using an electric dryer. The moisture in the dried granule (non-sprayed base granule (b)) was 1.3%.

  As for the physical properties of the obtained non-jet dried base granule (b), the average particle size was 320 μm, the bulk density was 495 g / L, and the supporting ability was 51 mL / 100 g.

Examples 1 to 4 and Comparative Examples 1 and 2 (Example 4 is a reference example)
<Process (B)>
In a mixture composed of 75% sodium alkyl sulfate and 25% water, 2.1 parts by weight (Example 1), 20 parts by weight (Example 2) or 50 parts by weight (Example 3) per 100 parts by weight of sodium alkyl sulfate. ) Ethyl lactate, or 20 parts by weight of 1-propanol (Example 4), or 2.1 parts by weight of PEG400 (Comparative Example 2) in place of the viscosity modifier, at a temperature of 60 ° C. After mixing for 1 minute, an anionic surfactant composition of the present invention (Examples 1 to 4) and a comparative anionic surfactant composition (Comparative Example 2) were obtained. Using MCR300 (manufactured by PHYSICA Messtechnik GmbH), the viscosity of the obtained composition and a composition not containing a viscosity modifier (mixture comprising sodium alkyl sulfate 75%, water 25%: Comparative Example 1) The measurement was performed at a temperature of 50 ° C. and a shear rate of 0.1 to 10 [1 / s]. Table 1 shows the results of each example and each comparative example.

Examples 5 to 6 and Comparative Example 3 (However, Example 6 is a reference example.)
<Process (B)>
20 parts by weight of ethyl lactate (Example 5) or 20 parts by weight with respect to 100 parts by weight of sodium alkyl sulfate ester in a mixture composed of 70% sodium alkyl sulfate ester (sodium polyoxyethylene lauryl ether sulfate) and 30% water 1-propanol (Example 6) was added and mixed at a temperature of 60 ° C. for 1 minute to obtain an anionic surfactant composition (Examples 5 to 6) of the present invention. Using MCR300 (manufactured by PHYSICA Messtechnik GmbH), the viscosity of the obtained composition and a composition not added with a viscosity modifier (a mixture of 70% sodium alkyl sulfate ester and 30% water: Comparative Example 3) was used. The measurement was performed at a temperature of 50 ° C. and a shear rate of 0.1 to 10 [1 / s]. Table 2 shows the results of each example and each comparative example.

Examples 7 and 8
<Process (C)>
Addition of 36.2 parts by weight (Example 7) or 50.7 parts by weight (Example 8) of the composition of Example 2 to 100 parts by weight of the spray-dried base granule (a) produced in Production Example 1 Then, mixing was performed using a spatula for 10 minutes 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.

<Process (D)>
Each granulated product obtained by the above operation is added to a plastic bag containing 4.2 parts by weight of crystalline silicate and 23.1 parts by weight of zeolite per 100 parts by weight of the spray-dried base granule (a). It was. 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.

Examples 9 and 10
<Process (C)>
62.8 parts by weight (Example 9) or 72.6 parts by weight (Example 10) of the composition of Example 2 is added to 100 parts by weight of the spray-dried base granule (a) produced in Production Example 1. Then, the mixture was mixed for 15 minutes using a spatula to obtain each mixture. When the obtained mixture was observed, no liquid was observed in any of the mixtures, and the mixture formed a granulated product without agglomerates.

<Process (D)>
Each granulated product obtained by the above operation is added to a plastic bag containing 4.2 parts by weight of crystalline silicate and 23.1 parts by weight of zeolite per 100 parts by weight of the spray-dried base granule (a). It was. 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.

Example 11
<Process (C)>
65.2 parts by weight of the composition of Example 2 is added to 100 parts by weight of the non-sprayed base granule (b) produced in Production Example 2, and the mixture is mixed for 20 minutes using a spatula. Obtained. When the obtained mixture was observed, the presence of liquid was not observed, and the mixture formed a granulated product without aggregates.

<Process (D)>
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 non- sprayed base granules ( b ). . The plastic bag was shaken up and down 30 times to carry out surface modification of the granulated product (mixture) to obtain detergent particles.

Example 12
<Process (C)>
77.1 parts by weight of the composition of Example 5 is added to 100 parts by weight of the spray-dried base granule (a) produced in Production Example 1, and mixed using a spatula for 15 minutes to obtain a mixture. It was. When the obtained mixture was observed, the presence of liquid was not observed, and the mixture formed a granulated product without aggregates.

<Process (D)>
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 (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 Examples 4-6
<Process (C)>
31.5 parts by weight (Comparative Example 4 ), 44 parts by weight of a mixture of 75% sodium alkyl sulfate and 25% water of Comparative Example 1 with respect to 100 parts by weight of the spray-dried base granules (a) produced in Production Example 1 1 part by weight (Comparative Example 5 ) or 54.6 parts by weight (Comparative Example 6 ) was 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, but many aggregates were observed.

<Process (D)>
Each 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 (a). . 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 7
<Process (C)>
56.7 parts by weight of a mixture of 75% sodium alkyl sulfate and 25% water of Comparative Example 1 were added to 100 parts by weight of the non-sprayed base granule (b) produced in Production Example 2, and a spatula was used. For 20 minutes to obtain a mixture. When the obtained mixture was observed, no liquid was observed in any of the mixtures, but many aggregates were observed.

<Process (D)>
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 non-spray-dried base granules (b). . 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 8
<Process (C)>
67.6 parts by weight of a mixture of 70% sodium alkyl sulfate ester and 30% water of Comparative Example 3 was added to 100 parts by weight of the spray-dried base granule (a) produced in Production Example 1, and a spatula was used. For 15 minutes to obtain a mixture. When the obtained mixture was observed, the presence of liquid was not observed, but many aggregates were observed.

<Process (D)>
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 (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.

  Tables 3 and 4 show the physical properties and the like of the detergent particle groups obtained in Examples 7 to 12 and Comparative Examples 4 to 8. In addition, about the bulk density of a detergent particle group in a table | surface, the bulk density (bulk density (whole grain)) of the obtained detergent particle group itself, and the bulk density (bulk density) of a detergent particle group with a particle size of 125-1000 micrometers are obtained. (125-1000 μm)) was measured and described. As for the coarse particle ratio, the ratio of particles having a size of 500 μm or more in the detergent particle group was expressed by weight%.

Examples 13-17, Comparative Examples 9-10 (however, Examples 13-17 are reference examples)
<Process (C)>
20 parts by weight of 1-propanol (Example 13), isopropanol (Example 14), and 1 part each of 100 parts by weight of sodium alkyl sulfate were added to a mixture of sodium alkyl sulfate 75% and water 25% of Comparative Example 1. Add butanol (Example 15), 1-hexanol (Example 16), 1-octanol (Example 17), 1-decanol (Comparative Example 9), or 1-dodecanol (Comparative Example 10), temperature 60 The mixture was mixed at 1 ° C. for 1 minute to obtain an anionic surfactant composition. 36.2 parts by weight of the obtained composition is added to 100 parts by weight of the spray-dried base granule (a) produced in Production Example 1 and mixed for 5 minutes using a spatula. Obtained. When the obtained mixture was observed, no liquid was observed in any of the mixtures, but the mixtures of Examples 13 to 17 formed a granulated product in which no agglomerates were found. Many aggregates were observed in the mixtures of Comparative Examples 9 to 10.

<Process (D)>
Each granulated product obtained by the above operation is added to a plastic bag containing 4.2 parts by weight of crystalline silicate and 23.1 parts by weight of zeolite per 100 parts by weight of the spray-dried base granule (a). It was. 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 5 shows the physical properties of the obtained detergent particles. In Table 5, the items of the physical property values have the same meaning as in Table 3.

Example 18
<Process (C)>
20 parts by weight of ethyl lactate per 100 parts by weight of sodium alkyl sulfate was added to a mixture of sodium alkyl sulfate 75% and water 25% of Comparative Example 1 and mixed for 1 minute at a temperature of 60 ° C. An agent composition was obtained. 36.2 parts by weight of the obtained composition was added to 100 parts by weight of the spray-dried base granule (a) produced in Production Example 1, and mixed using a spatula for 10 minutes to obtain a mixture. . When the obtained mixture was observed, the presence of liquid was not observed, and the mixture formed a granulated product without aggregates.

<Process (D)>
The granulated product obtained by the above operation was added to a plastic bag containing 6.3 parts by weight of zeolite with respect to 100 parts by weight of the spray-dried base granule (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. The solubility (25 ° C.) of 0.45 g of the detergent particle group obtained by the above operation was evaluated using ion-exchanged water.

Comparative Example 11
31.5 parts by weight of a mixture of 75% sodium alkyl sulfate and 25% water of Comparative Example 1 was added to 100 parts by weight of the spray-dried base granule (a) produced in Production Example 1, and a spatula was used. Mixing over 10 minutes gave a mixture. When the obtained mixture was observed, no liquid was observed in any of the mixtures, but many aggregates were observed.

  The granulated product obtained by the above operation was added to a plastic bag containing 6.3 parts by weight of zeolite with respect to 100 parts by weight of the spray-dried base granule (a). 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.

  The solubility (25 ° C.) of 0.43 g of the detergent particle group obtained by the above operation was evaluated using ion-exchanged water.

Example 19
<Process (B)>
20 parts by weight of ethyl lactate is added to 100 parts by weight of sodium alkyl sulfate to a mixture of 75% sodium alkyl sulfate and 25% water of Comparative Example 1, and the mixture is mixed at a temperature of 60 ° C. for 1 minute. An anionic surfactant composition was obtained.

  The resulting composition was stored for 1 day in a screw tube at room temperature and cooled. Next, the solubility (25 ° C.) of 0.23 g of the composition was evaluated using tap water.

Comparative Example 12
The solubility (25 ° C.) of 0.21 g of a mixture composed of 75% sodium alkyl sulfate of Comparative Example 1 and 25% water was evaluated using tap water.

  Regarding the solubility in Examples 18 and 19 and Comparative Examples 11 and 12, the time until the dissolution rate for each of them was 100% was measured. The results are shown in Tables 6 and 7.

  From Tables 1 and 2, compared with those of Comparative Examples 1 to 3, the anionic surfactant compositions shown in Examples 1 to 6 have a shear rate of 0.1 to 10 [1 / s]. It turns out that it is thinning. Furthermore, it turns out that the effect | action of the viscosity reduction in this invention can be exhibited not only in an alkyl sulfate but in various anionic surfactants.

  Furthermore, from Tables 3 to 5, the detergent particle groups obtained in Examples 7 to 17 all have a high coarse particle ratio and a high degree of particle growth as compared with those of Comparative Examples 4 to 10, and have a high bulk. From the observation of the density and the obtained detergent particle group, it can be seen that the detergent particle group with few aggregates can be produced by the production method of the present invention. Furthermore, from Comparative Examples 9 and 10, when the number of carbon atoms of the monohydric alcohol exceeds a specific range, even if the monohydric alcohol is used as a viscosity modifier, aggregates may be generated in the resulting detergent particles. I understand.

  Furthermore, it can be seen from Table 6 that the detergent particle group in Example 18 is more soluble than the detergent particle group in Comparative Example 11.

  Furthermore, it can be seen from Table 7 that the anionic surfactant composition in Example 19 is more soluble than the anionic surfactant composition in Comparative Example 12.

  Since the anionic surfactant composition of the present invention has a low viscosity, it can provide excellent handling properties in the production process of detergent particles. Furthermore, the anionic surfactant composition of the present invention can be used for the production of detergent particles having a sharp particle size distribution and excellent solubility.

Claims (5)

(a) hydroxycarboxylic acid ester le also there in (b) monohydric alcohol hydroxycarboxylic acid esters and 3 to 8 carbon atoms, and an anionic surfactant composition containing 50 to 90 wt% anionic surfactant The hydroxycarboxylic acid ester is represented by the following general formula (1):
CH ₃ CH (OH) COOR (1)
(In the formula, R represents a hydrocarbon group having 1 to 16 carbon atoms.)
An anionic surfactant composition, which is a compound represented by: The content of the hydroxycarboxylic acid ester or the content of the hydroxycarboxylic acid ester and the monovalent alcohol having 3 to 8 carbon atoms is 1 to 80 parts by weight with respect to 100 parts by weight of the anionic surfactant. 2. The composition according to 1.   The monohydric alcohol having 3 to 8 carbon atoms is 1-propanol, 2-methyl-2-propanol, isopropanol, 1-butanol, 2-butanol, 2-methyl-2-butanol, 1-pentanol, 2-methyl The composition according to claim 1 or 2, which is one or more alcohols selected from the group consisting of 2-pentanol, 1-hexanol, 2-ethyl-1-hexanol, 1-heptanol and 1-octanol.   The composition according to any one of claims 1 to 3, wherein the anionic surfactant is an alkyl sulfate and / or an alkyl sulfate salt.   A detergent particle group containing the anionic surfactant composition according to any one of claims 1 to 4.