JP4421460B2 - Method for producing bleach activator composition - Google Patents

Description

  The present invention relates to a method for producing a bleach activator composition having good solubility, a bleach activator composition obtained by the method, and a bleach activator obtained by further granulating the bleach activator composition. It relates to agent granules.

  Conventionally, various bleaching activators have been proposed in order to increase the bleaching power of oxygen bleaches such as sodium percarbonate and sodium perborate. Its function can be severely impaired during storage by interaction with oxygen bleaches or other ingredients incorporated in detergents. Accordingly, bleach activators are required to have high storage stability. In addition, it is required to have excellent solubility even under washing conditions with weak stirring power in cold water or under soaking bleaching conditions.

Patent Document 1 discloses at least one nonionic surfactant selected from a bleaching activator, a nonionic surfactant having a melting point of less than 20 ° C., and an alkylene oxide addition nonionic surfactant having a melting point of less than 20 ° C. A bleaching activator granule having good solubility and containing a surfactant in a specific ratio is disclosed. However, in recent years, the washing condition has a weak stirring force, the washing time is shortened, and in terms of solubility, a bleach activator composition having a higher dissolution rate has been demanded.
JP 2001-59099 A

  An object of the present invention is to provide a bleach activator composition having good solubility and a method for producing the same.

  The present invention relates to a method for producing a bleach activator composition in which a solvent and / or water is removed from a mixture of a bleach activator and a surfactant dispersed in a non-aqueous solvent, and the bleaching activity obtained by this production method. An activator composition and a bleach activator granulated product obtained by further granulating the bleach activator composition are provided.

  By the method of the present invention, it is possible to produce a bleach activator composition and a bleach activator granulated product having good solubility (hereinafter sometimes simply referred to as a bleach activator composition). The bleach activator composition of the invention can be suitably used even under washing conditions for clothing having a weak stirring force and a reduced washing time.

[Bleaching activator]
The bleach activator used in the present invention is not particularly limited as long as it can increase the bleaching power of the bleach. For example, tetraacetylethylenediamine, glucose pentaacetate, tetraacetylglycoluril, alkanoyl or alkenoyl (these) The number of carbons in the group is 8 to 14) oxybenzene carboxylic acid or a salt thereof, alkanoyl or alkenoyl (the number of carbons in these groups is 8 to 14) oxybenzene sulfonate, etc. Or alkenoyl (the number of carbon in these groups is 8 to 14, preferably 10 to 14 from the viewpoint of bleaching effect) oxybenzenecarboxylic acid or a salt thereof and alkanoyl or alkenoyl (the number of carbon in these groups is 8 to 14, bleaching effect) In view of the above, preferably 10-14) oxyben One or more selected from Nsuruhon acid salts are preferred. In particular, decanoyloxybenzenecarboxylic acid or a sodium salt thereof, and dodecanoyloxybenzenesulfonic acid sodium salt are preferable.

[Surfactant]
Examples of the surfactant used in the present invention include anionic surfactants, nonionic surfactants, amphoteric surfactants, and cationic surfactants. A combination of a nonionic surfactant and an anionic surfactant is used. Is preferred.

  Examples of the anionic surfactant used in the present invention include alkyl sulfates, polyoxyalkylene alkyl ether sulfates, alkylbenzene sulfonates, olefin sulfonates, alkane sulfonates, saturated or unsaturated fatty acid salts, alkyl or alkenyl ethers. Examples thereof include carboxylates, α-sulfo fatty acid salts, and α-sulfo fatty acid esters, and alkyl sulfates, polyoxyalkylene alkyl ether sulfates, and alkyl benzene sulfonates are more preferable.

  Examples of the alkyl sulfate include compounds represented by the general formula (I).

[R ¹ —SO ₃ ] _p M ¹ (I)
[Wherein, R ¹ represents a linear alkyl group having 8 to 20 carbon atoms, M ¹ represents a cation, and p represents a valence of M ¹ . ]
In general formula (I), from the viewpoint of solubility, R ¹ is preferably an alkyl group having 10 to 18 carbon atoms. M ¹ is preferably an alkali metal such as Na or K, an alkaline earth metal such as Ca or Mg, or an alkanol-substituted or unsubstituted ammonium group, and more preferably an alkali metal, particularly Na. p is the valence of M ¹ , preferably 1 or 2, and more preferably 1.

  As a polyoxyalkylene alkyl ether sulfate, the compound represented by general formula (II) is mentioned, for example.

[R ² —O (AO) _n —SO ₃ ] _q M ² (II)
[Wherein R ² is a linear alkyl group having 8 to 20 carbon atoms, AO is an oxyalkylene group having 2 to 4 carbon atoms, and n AOs may be the same or different. n represents an average number of added moles of alkylene oxide, a number of 0.05 to 5, M ² represents a cation, q represents a valence of M ² , preferably 1 or 2, and more preferably 1. ]
In general formula (II), R ² is preferably an alkyl group having 10 to 18 carbon atoms from the viewpoint of solubility. AO is preferably an oxyalkylene group having 2 to 3, particularly 2 carbon atoms. n is preferably a number from 0.1 to 3, particularly from 0.2 to 2. M ² is preferably an alkali metal such as Na or K, an alkaline earth metal such as Ca or Mg, or an alkanol-substituted or unsubstituted ammonium group, and more preferably an alkali metal, particularly Na. p is preferably 1 or 2, and more preferably 1.

  The polyoxyalkylene alkyl ether sulfate is not particularly limited in the addition distribution of alkylene oxide, and may be any of broad and narrow distributions generally called.

  As the alkylbenzene sulfonate, those having 8 to 20 carbon atoms in the alkyl group are preferable from the viewpoint of solubility, and sodium salt or potassium salt is particularly preferable.

  The anionic surfactants listed above may be used alone or in combination of two or more. For example, two types of combined use of alkyl sulfates and polyoxyalkylene alkyl ether sulfates, three types of combined use of alkyl sulfates, polyoxyalkylene alkyl ether sulfates, and alkylbenzene sulfonates can be used.

  Examples of the nonionic surfactant used in the present invention include alkylene oxide addition type nonionic surfactants, higher fatty acid alkanolamides or their alkylene oxide adducts, sucrose fatty acid esters, alkylglycosides and the like. From the viewpoint of solubility, at least one nonionic surfactant selected from alkylene oxides having a melting point of less than 20 ° C., preferably ethylene oxide and / or propylene oxide addition type nonionic surfactants, is preferable. Those selected from nonionic surfactants represented by the formula (III) are preferred.

_{^{R 3 O- (PO) r -}} (EO) s -H (III)
[Wherein, R ³ is an alkyl group or alkenyl group having 10 to 18 carbon atoms, preferably 10 to 14 carbon atoms, and r and s are each independently 0 to 20, preferably 1 to 10, more preferably 2 to 10 (Where r + s is 1 or more). PO is a propyleneoxy group, EO is an ethyleneoxy group, and PO and EO may be added in blocks or randomly. ]

  Among these nonionic surfactants, those represented by general formula (III-1) are particularly preferred from the viewpoint of the bleaching effect.

_{^{R 3 O- (EO) t -}} (PO) u - (EO) v -H (III-1)
[Wherein R ³ , EO and PO have the same meanings as described above, t is 0 to 10, preferably 1 to 7, u is 1 to 10, preferably 1 to 5, and v is 0 to 10, preferably Is 1-7. However, t and v are not 0 at the same time. ]
Specific examples of the nonionic surfactant represented by the general formula (III-1) include Emalgen KS-108 (C12 alcohol EO5 mol PO2 mol EO3 mol adduct), Emulgen LS-, manufactured by Kao Corporation. 106 (C12 alcohol EO 2.5 mol PO 1.5 mol EO 3 mol adduct) and the like.

  In addition, from the viewpoint of powder properties obtained by removing the solvent from the mixture of the bleach activator and the surfactant, when using a liquid surfactant, it is preferable to use it mixed with a surfactant paste such as an anionic surfactant. .

  Examples of the amphoteric surfactant used in the present invention include amine oxide, sulfobetaine, carbobetaine and the like.

  Examples of the cationic surfactant used in the present invention include quaternary ammonium salts and amine salts.

  In the present invention, the surfactant is preferably used in the form of a liquid or a paste because a mixture uniformly dispersed with the bleach activator can be easily formed when preparing the mixture with the bleach activator. Further, when the bleach activator composition is obtained as a granulated product, it is more preferably used in a paste form.

[Non-aqueous solvent]
The non-aqueous solvent used in the present invention may be any solvent that does not substantially dissolve the bleach activator, and the type thereof is not particularly limited. For example, hydrocarbons, ketones, alcohols and ethers are preferably used. Among these, specifically, toluene, xylene, benzene, hexane, octane, acetone, ethyl alcohol, isopropyl alcohol, diethyl ether and the like are preferable from the viewpoint of dispersion of the bleach activator and solvent removal.

  Further, when water in which the bleach activator is dissolved is used, an aqueous solvent is not preferable because the bleach activator is hydrolyzed and the effective component is reduced.

[Method for producing bleach activator composition]
In the production method of the present invention, a bleaching activator dispersed in a non-aqueous solvent and a surfactant are mixed to obtain a mixture (hereinafter referred to as step 1), and the solvent and / or water is removed from the mixture obtained in step 1. It comprises a step of removing to obtain a bleach activator composition (hereinafter referred to as step 2).

  In Step 1, the order of addition of the bleach activator and the surfactant to the non-aqueous solvent may be any if the bleach activator can be prevented from aggregating, but in order to prevent the bleach activator from aggregating, It is preferable to uniformly disperse / mix with the surfactant in a state where the bleach activator is dispersed in a non-aqueous solvent in which the bleach activator is substantially insoluble.

  The dispersion method of the bleach activator is not particularly limited, but after adding a non-aqueous solvent in which the bleach activator is not dissolved to the stirring and mixing tank, the bleach activator is supplied to the stirring and mixing tank while stirring to perform bleaching activity. There is a method of preparing an agent dispersion. Further, the thinner the bleaching activator dispersion is, the lower the viscosity is, and the easier it is to handle. However, if the solid content is too low, the load of the subsequent step 2 is increased, and if the solid content is too high, the viscosity is too high. The solid content is preferably 20 to 80% by weight, and more preferably 40 to 60% by weight, because of the increase in the thickness and the handling.

  Moreover, when there exists the state disperse | distributed to the non-aqueous solvent in the middle of processes, such as the refinement | purification process after a bleaching activator synthesis reaction, you may use the bleaching activator dispersion liquid.

  As a means for mixing the bleach activator and the surfactant dispersed in the non-aqueous solvent, as long as the bleach activator and the surfactant can be uniformly dispersed / mixed while preventing aggregation of the bleach activator. A general batch-type stirring and mixing tank, continuous mixer, or the like can be used. Examples of the batch-type stirring and mixing tank include a stirring and mixing tank, a batch kneader manufactured by Satake Chemical Machinery Co., Ltd., a Nauter mixer manufactured by Hosokawa Micron Co., Ltd., and examples of the continuous mixer include Noritake Company ( Examples thereof include a static mixer manufactured by Kurimoto Corporation, and a KRC kneader manufactured by Kurimoto Iron Works.

  In addition, the temperature condition at the time of mixing is a temperature at which the solvent does not boil at room temperature, and the temperature should be low in order to suppress the decomposition of the bleach activator, but if it is too low, the fluidity of the mixture will deteriorate and uniform dispersion will occur / Because mixing becomes difficult, 10 to 80 ° C. is preferable, and 30 to 60 ° C. is more preferable.

  The mixing ratio of the bleach activator and the surfactant is preferably bleach activator / surfactant = 100/30 to 100/5, and more preferably 100/15 to 100/10 in weight ratio.

  Further, the solid content concentration of the mixture of the bleach activator and the surfactant is preferably 80% by weight or less which is in a fluid state at room temperature, and the solvent and water removal load in Step 2 is reduced to 50 to 80% by weight. Is more preferable. By controlling it to 80% by weight or less, it is preferable because appropriate fluidity can be secured.

  Step 2 is a step of removing the solvent and / or water from the non-aqueous solvent mixture of the bleach activator and surfactant prepared in Step 1 under various conditions. It can happen at the same time. The residual ratio of the solvent and / or water in the bleach activator composition after removal of the solvent and / or water is preferably 10% by weight or less, and more preferably 5% by weight or less.

  As the removing means, drying is preferable, and in order to suppress degradation of the bleach activator due to heating and degradation such as hydrolysis, drying under vacuum is preferable. The drying conditions at this time include non-aqueous solvents and water. It is preferable to dry at a degree of vacuum at which the removal temperature is 80 ° C. or less from the viewpoint of reducing thermal history and suppressing degradation of quality such as decomposition. Furthermore, in consideration of the pulverization at the end of drying, a continuous or batch type vacuum dryer having a stirring blade and a pulverizer or a drying process capable of obtaining an effect equivalent thereto is preferable.

  Examples of the continuous dryer include rotating thin film evaporators such as Contro, Cebucon [manufactured by Hitachi, Ltd.], Smith thin film evaporator [manufactured by Shinko Pantech Co., Ltd.], and the like. In the case of these continuous dryers, a non-aqueous solvent mixture of a bleach activator and a surfactant can be continuously charged into a rotary thin film evaporator under reduced pressure to obtain a dried product. Examples of the batch type dryer having a vacuum function include SV mixer manufactured by Shinko Pantech Co., Ltd., batch kneader manufactured by Satake Chemical Machinery Industry Co., Ltd., Nauta mixer manufactured by Hosokawa Micron Co., Ltd., Fukae Powtech Co., Ltd. High speed mixer manufactured by Mitsui Mining Co., Ltd., Henschel mixer manufactured by Mitsui Mining Co., Ltd., Super mixer manufactured by Kawada Seisakusho Co., Ltd., Mixer dryer manufactured by Tanabe Wiltech Co., Ltd., Vertical granulator manufactured by POWREC CO., LTD. . Among these, particularly when the batch type is used, by adding a non-aqueous solvent mixture of a bleach activator and a surfactant to a powder raw material that is in a fluid state with the removal of the non-aqueous solvent and water, High speed mixers, vertical granulators, Henschel mixers, and super mixers are preferred because the load on the equipment is small because a uniform granulated product can be obtained.

  As a more preferable drying method, the powder of the bleach activator and / or the powder other than the bleach activator is previously stirred and disintegrated as a powder raw material in a batch type vacuum dryer having a stirring blade and / or a crusher. After charging to such an extent that a crushing effect can be obtained, a non-aqueous solvent mixture of a bleach activator and a surfactant is supplied at a supply rate such that the powder raw material in the machine maintains a powder state under reduced pressure. By drying, a more preferable dried product having a uniform particle size can be obtained. The powder raw material prepared in advance at this time is shown below.

  As the powder raw material charged in advance, a powder containing a bleach activator is preferable. The reason for this is that the bleach activator content in the resulting bleach activator composition is high and the performance per weight (bleachability, peracid production rate, etc.) of the bleach activator composition is also high. Is mentioned. From the viewpoint of solubility, the bleach activator powder preferably has an average particle size of 0.1 to 50 μm, more preferably 0.5 to 20 μm, and more preferably 1 to 10 μm. The addition amount of the powder raw material is preferably 10 to 30% by weight based on the total amount of the composition.

  For the purpose of uniforming the particle size, a powder other than the bleach activator may be used as a powder raw material. Examples of powders other than the bleach activator include sodium sulfate, sodium carbonate, and baking soda. The addition amount of these powders is preferably 10 to 30% by weight based on the total amount of the composition. From the viewpoint of granulation properties, the average particle size is preferably 10 to 200 μm, and more preferably 50 to 100 μm.

  In order to further align the particle size, the granulation method is not particularly limited, but i) Stirring rolling granulation method, ii) Fluidized bed granulation method, iii) Extrusion granulation method, iv) Tableting (tablet) and briquette A desired granulated product can be obtained by a compression granulation method such as casting and compacting.

  Moreover, it does not specifically limit as a binder used at the time of granulation, However, Water or a water-soluble binder can be used individually or in mixture of 2 or more types. Examples of the water-soluble binder include polyethylene glycol, polypropylene glycol, polyoxyethylene-polyoxypropylene glycol, carboxymethyl cellulose, polyvinyl alcohol, polyvinyl pyrrolidone, and water-soluble cellulose derivatives (these derivatives include ether compounds). , Carboxylic acid polymers, polyoxyethylene (ethylene oxide addition moles = 3 to 300) alkyl (C8-22) ether, polyoxyethylene (ethylene oxide addition moles = 10 to 300) alkyl (C8-14) phenol ether , Sucrose ester, alkylglycoside, carboxylic acid, sulfonic acid, sulfate ester, phosphate ester anionic surfactant, amphoteric surfactant, polyoxyethylene alkylamine, fatty acid monoethanolamide, fat Acid diethanolamide, and the number 8 to 20 fatty acid glyceride carbon, starch, starch hydrolyzate, and saccharides and derivatives thereof.

Next, each granulation method will be described in detail.
i) Stirring tumbling granulation method The stirring tumbling granulation method adds a liquid or solid binder to the bleach activator composition charged in the tank, and sometimes superheats or cools, optionally with stirring blades. Is a method of granulating by rotating. According to this method, it is possible to control the solubility of the resulting granulated material by appropriately adjusting the binder type and amount to be added or the granulation time, and granulation is carried out either batchwise or continuously. be able to.
The addition of the binder may be performed all at once, but the addition time can be adjusted or added intermittently in order to obtain a desired granulated product or depending on the physical properties of the binder. Among these water-soluble binders, polyethylene glycol and polypropylene glycol having a molecular weight in the range of 400 to 20,000, preferably 600 to 10,000 are preferable from the viewpoint of easy granulation control and storage stability of the granulated product. When the binder is added in liquid form, it is preferably added by a spray method. The amount of the binder to be added is not particularly limited, but is preferably 5 to 40% by weight, particularly 10 to 20% by weight based on the bleach activator composition from the viewpoint of productivity and the like.

The granulator which can be used is not particularly limited. (1) A mixer having a mixing shaft in the mixing tank and mixing the powder by attaching a stirring blade to this shaft: for example, Henschel mixer (Mitsui Miike Chemical) Machine Co., Ltd.), High Speed Mixer (Fukae Kogyo Co., Ltd.), Vertical Granulator (Powrec Co., Ltd.), Redige Mixer (Matsuzaka Giken Co., Ltd.), Proshare Mixer (Pacific Kiko Co., Ltd.) (2) A mixer of a type that performs mixing by rotating a ribbon-like blade forming a spiral in a cylindrical or semi-cylindrical fixed container: For example, a ribbon mixer (Nichiwa Machinery Industries ( Co., Ltd.), batch kneader (Satake Chemical Machinery Co., Ltd.), etc. (3) Along the conical container, the screw rotates around an axis parallel to the container wall. Type mixers for mixing by: for example, Nauta Mixer (manufactured by Hosokawa Micron Corporation), and the like.
After granulation, drying, coating, and classification can be appropriately performed.

ii) Fluidized bed granulation method The fluidized bed granulation method is a method in which the bleach activator composition is kept in a fluid state by a fluid introduced from the lower part of the apparatus, and a liquid binder is added to the fluidized bed to perform aggregation granulation. . The binder may be added all at once, but the addition time can be adjusted or added intermittently in order to obtain a desired granulated product or depending on the physical properties of the binder.
In order to obtain a uniform granulated product, it is preferable to add a binder by a spray method. The amount of the binder to be added is not particularly limited, but is preferably 5 to 40% by weight, particularly 10 to 20% by weight, based on the bleach activator composition from the viewpoint of productivity and the like. Preferred examples of the fluidized bed granulator include a flow coater (manufactured by Freund Sangyo Co., Ltd.), a spiraflow (manufactured by the company), an agromaster (manufactured by Hosokawa Micron Corporation), and a GROMAX (manufactured by Fuji Powdal Corporation). After granulation, coating and classification can be appropriately performed.

iii) Extrusion granulation method In the extrusion granulation method, the above-mentioned binder is added to the bleach activator composition to knead it to give plasticity, and then it is pressed against the die or screen surface having a large number of holes by the extrusion mechanism. Extruded from the hole and molded, and a granulated product having a uniform average particle size of 0.3 to 30 mm is obtained.
When a thermoplastic substance is used for the binder, it is heated and extruded and granulated under the condition that it exhibits thermoplasticity. The binder is preferably premixed in advance with a Nauta mixer or the like. Moreover, the granulated product obtained by the fluidized bed granulation method described above can be further extruded and granulated. The amount of the binder to be added is not particularly limited, but is preferably 5 to 40% by weight, particularly 10 to 20% by weight, based on the bleach activator composition from the viewpoint of productivity and the like. The binder is preferably polyethylene glycol or polypropylene glycol having a molecular weight in the range of 400 to 20,000, preferably 600 to 10,000, from the viewpoint of easy control of granulation and storage stability of the granulated product.
Preferable extruding granulators include pelleter double (manufactured by Fuji Powder Co., Ltd.), twin dome gran (manufactured by the same company), and the like. After granulation, it is possible to further adjust the particle size by appropriately performing pulverization, granulation (rounding) and classification as post-treatment.

iv) Tableting / Briqueting / Compacting Tableting / Briqueting / Compacting are all compression granulation methods, low dustiness and uniform grain size. It is suitable for preparing a granulated product of a bleach activator composition. Tableting is a granulation method in which a bleach activator composition is filled in a mold and then pressed with a punch. Also, among the roll press methods in which the bleach activator composition is compressed and molded between two rotating rolls, briquetting is performed on the surface of the roll, and compacting is performed on the surface where the mold is not engraved. That's it. In these compression granulation methods, it is possible to granulate without adding a binder by applying a high compression force of 0.2 to 5 ton / cm ² to the bleach activator composition. It is possible to obtain a high granulated product.
Further, even when a binder is added, the amount may be extremely small, and may be about 2 to 10% by weight based on the bleach activator composition. Tableting is suitable for making a granulated product having an average particle size of about 0.5 to 1.0 mm, and briquetting is suitable for making it about 2 to 3 mm, but flakes formed by compacting are suitable. By crushing, it is possible to obtain a compacted granulated product of 1 to 2 mm or less. As the mold shape of the roll surface of the briquetting apparatus, there are a pillow type, a lens type, an almond type, a prism type, a wave type, etc., which can be appropriately selected and used.

[Bleaching activator composition]
The bleach activator composition of the present invention contains a bleach activator and a surfactant obtained by the method as described above. The content of the bleach activator in the composition of the present invention is preferably 50 to 95% by weight, more preferably 70 to 90% by weight. Moreover, 1-30 weight% is preferable and, as for content of surfactant, 5-15 weight% is still more preferable.

  The following additives may be added to the composition of the present invention as other components. These components may be blended at the time of producing the bleach activator composition or may be blended after the production.

  From the viewpoint of the stability of the bleach activator, a solid or powdered acid can be added. For example, formic acid, succinic acid, maleic acid, fumaric acid, citric acid, glycolic acid, p-hydroxybenzoic acid, phosphoric acid, fatty acid, zeolite showing solid acidity and the like can be mentioned, and succinic acid and citric acid are preferable. In this case, the acid may form a salt, and the counter ion is an alkali metal ion, an ammonium ion, or the like. The acid content is preferably 0.01 to 20% by weight, more preferably 1 to 15% by weight, particularly preferably 1 to 10% by weight, based on the total amount of the composition. Within this range, excellent ability as a stabilizer for the bleach activator can be exhibited.

From the aesthetic point of view, pigments or dyes may be blended and colored. As such a colorant, phthalocyanine green (for example, CIPigment 7, 36, 37) is used from the viewpoint of storage stability.
, 38, etc.), or ultramarine blue (for example, CIPigment Bule 29) is preferable, and the blending amount is preferably 0.01 to 1% by weight, particularly preferably 0.05 to 0.5% by weight in the bleach activator composition. .

  Further, as a modifier of the obtained bleach activator composition, a crystalline aluminosilicate such as zeolite having a particle size of 0.5 μm to 15 μm, which can provide a modification effect, amorphous silica, pulverized sodium sulfate, etc. May be blended. The blending amount is preferably 0.5 to 20% by weight, particularly 1 to 10% by weight in the bleach activator composition.

  Moreover, you may add a fragrance | flavor to the obtained bleach activator composition. Although it does not specifically limit as a fragrance | flavor, A musk fragrance | flavor, a citrus fragrance | flavor, an herb fragrance | flavor, a plant-type essential oil, etc. are mentioned. The blending amount is preferably 0.001 to 5% by weight, particularly 0.05 to 1% by weight in the bleach activator composition.

  A water-soluble polymer may be added as a granulation improver. Here, the water-soluble polymer preferably has a water solubility at 20 ° C. of 60% or more, more preferably 80% or more. The molecular weight is preferably 600 or more. Further, those having a melting point of 20 ° C. or higher are preferred. Specific examples of the water-soluble polymer include polyethylene glycol and polypropylene glycol. The molecular weight of polyethylene glycol and polypropylene glycol is preferably 600-20000, more preferably 1000-10000. The content of the water-soluble polymer in the composition of the present invention is not particularly limited, but is preferably 0.5 to 20% by weight, more preferably 1 to 15% by weight. A granulated product with properties can be obtained.

  Further, a re-contamination inhibitor such as polyvinylpyrrolidone, or a dissolution accelerator such as urea, urea derivative, thiourea, paratoluenesulfonate, and water-soluble inorganic salts may be added. Further, known magnesium salts such as magnesium sulfate and magnesium silicate may be used as stabilizers for peroxides or peroxide adducts.

  The size and shape of the bleach activator composition of the present invention are not particularly limited, but from the viewpoint of solubility and prevention of dusting during handling, the particle size is preferably 125 to 2000 μm, more preferably 125 to 1410 μm. Further, the granulated product having a large particle size may be pulverized to the above particle size range and recovered.

  The bleach activator composition of the present invention is useful for garment detergents, and can be suitably used particularly in garment washing conditions where the stirring power is weak and the washing time is shortened.

  Unless otherwise specified,% in the examples is based on weight.

Comparative Example 3
Formula (A)

28 liters of a toluene dispersion slurry (effective content 37%) of a bleach activator represented by the following formula (abbreviated as bleach activator (A)) 1 L batch kneader (Irie Shokai Co., Ltd .: batch kneader PNV-1 type) ) And 75% of the surfactant [alcohol having 12 to 16 carbon atoms (distribution is C12 / C14 / C16 = 67% / 28% / 5%), and average 1.0% of ethylene oxide in the alcohol. Surfactant paste (active ingredient is 75%) adjusted to 25% (average molecular weight 209) of mole-added ethoxylate, hereinafter abbreviated as surfactant (B)] 11.5 g was added, and the rotational speed was 60 r / m. After uniformly mixing for 15 minutes, the inside of the mixer was evacuated to 20 kPa (feeding amount: 300 g / Batch) while stirring at a jacket warm water flow of 70 ° C. and a rotational speed of 60 r / m for 120 minutes under these conditions. While 拌, to remove toluene and water to obtain a dried product. The obtained dried product was sieved to obtain a bleach activator composition having a particle size of 125 to 1410 μm.

Example 2
183 g of bleach activator (A) and 170 g of toluene were charged into a 2 L beaker, and stirred and dispersed for 10 minutes with a laboratory stirrer (6 paddle blades φ5 cm) at 450 r / m. After addition of 37 g of surfactant (B) The mixture was again stirred and dispersed for 10 minutes under the above conditions using a laboratory stirrer. A 2 L Henschel mixer (Mitsui Mining Co., Ltd .: Henschel mixer UM2E type) was charged with 90 g of bleach activator (A), and the inside of the mixer was vacuumed while stirring at a temperature of 750 r / m. The mixture was granulated while removing toluene and water while dropping a mixture of the above-described bleach activator (A) and surfactant (B) at a rate of 5.0 g / min. The obtained granulated product was classified to obtain a bleaching activator composition having a particle size of 125 to 1410 μm.

Example 3
162 g of bleach activator (A) and 156 g of toluene were charged into a 2 L beaker, and stirred and dispersed for 10 minutes with a laboratory stirrer (6 paddle blades φ5 cm) at 450 r / m, and a surfactant [with 12 to 16 carbon atoms] After neutralizing the sulfate of alcohol (distribution C12 / C14 / C16 = 67% / 28% / 5%) with aqueous sodium hydroxide solution and adding 75% phosphoric acid (buffer), 30.1% water Surfactant paste finely adjusted to pH = 10 with aqueous sodium oxide solution (active ingredient is 75%, hereinafter abbreviated as surfactant (C)) After adding 64 g, again using a laboratory stirrer for 10 minutes under the above conditions Dispersed with stirring. A 2 L Henschel mixer (Mitsui Mining Co., Ltd .: Henschel mixer UM2E type) was charged with 90 g of bleach activator (A), and the inside of the mixer was vacuumed while stirring at a temperature of 750 r / m. A dried product was obtained while removing toluene and water while dropping the mixture of the bleach activator (A) and the surfactant (B) described above at a rate of 10.0 g / min. The obtained dried product was classified to obtain a bleaching activator composition having a particle size of 125 to 1410 μm.

Example 4
249.0 g of the dried product obtained in Example 3, 9.0 g of succinic acid (succinic acid manufactured by Kawasaki Kasei Kogyo Co., Ltd., hereinafter abbreviated as succinic acid), nonionic surfactant (Emulgen KS110S95 manufactured by Kao Corporation), (Hereinafter abbreviated as E-KS-110) 9.0 g, polyethylene glycol (KPEG6000LA manufactured by Kao Co., Ltd., hereinafter abbreviated as PEG6000) 33.0 g blender (Fukae Pautech Co., Ltd. high speed mixer LFS-GS-2J type) ), The jacket temperature was 75 ° C., the agitator was 350 r / m, the chopper was stirred at 1850 r / m and mixed until the powder temperature reached 70 ° C., and then extracted. Next, the obtained mixture was extruded through a screen having a pore diameter of 0.7 mm by an extrusion granulator (Fuji Paudal Co., Ltd. Dome Gran DG-L1 type) to be consolidated.
The obtained extrudate was cooled to room temperature and then crushed with a granulator (Power Mill PS-02S manufactured by Dalton Co., Ltd.). The obtained pulverized product was sieved to obtain a bleaching activator granulated product having a particle size of 350 to 1410 μm.

Comparative Example 1
273 g of powdery bleach activator (A) and 27 g of dry powder of surfactant (B) were charged into a 2 L Henschel mixer (Mitsui Mining Co., Ltd .: Henschel mixer UM2E type), jacket warm water flowing at 70 ° C., rotating Granulation was performed while stirring at several 750 r / m. The obtained granulated product was classified to obtain a bleaching activator composition having a particle size of 125 to 1410 μm.

Comparative Example 2
Blender (Fukae Powtech) 210.0 g of powdered bleach activator (A), 39 g of dry powder of surfactant (C), 9.0 g of succinic acid, 9.0 g of E-KS-110, 33.0 g of PEG6000 (High-speed mixer LFS-GS-2J type manufactured by Co., Ltd.) (feed amount 300g / Batch), jacket temperature is 75 ° C, agitator 350r / m, chopper 1850r / m, and the powder temperature becomes 70 ° C Until mixed. Next, the obtained mixture was extruded through a screen having a pore diameter of 0.7 mm by an extrusion granulator (Fuji Paudal Co., Ltd. Dome Gran DG-L1 type) to be consolidated.
The obtained extrudate was cooled to room temperature and then crushed with a granulator (Power Mill PS-02S manufactured by Dalton Co., Ltd.). The obtained pulverized product was sieved to obtain a bleaching activator granulated product having a particle size of 350 to 1410 μm.

Table 1 shows the production conditions of Examples 2 to 4 and Comparative Examples 1 to 3 , and the physical properties of the resulting bleach activator compositions. Further, the solubility (peracid production rate) of these bleach activator compositions was evaluated by the following method. The results are also shown in Table 1.

<Peracid production rate measurement method>
A bleach activator composition was prepared by dissolving 0.3 g of sodium percarbonate and 0.3 g of an anionic detergent having the following composition in 75 mL of tap water, and the bleach activator was used for hydrogen peroxide in sodium percarbonate. After dissolving at 1/16 equivalent and reacting at 20 ° C. for 2 minutes and 10 minutes, adding 2.5 mL of 0.3% catalase solution and stirring for 1 minute, 10 mL of 20% sulfuric acid, 10% iodine Potassium fluoride solution is added, titrated with 0.1N sodium thiosulfate solution, and the peracid production rate after 2 minutes and 10 minutes is determined by the following formula.
・ Anionic detergent linear alkyl (C12-13) sodium benzenesulfonate 25%
Alkyl (carbon number 14-15) sodium sulfate 8%
Sodium carbonate 20%
Amount of mirabilite totaling 100%

Claims (5)

Production of a bleach activator composition that removes solvent and / or water while adding a mixture of a bleach activator and a surfactant dispersed in a non-aqueous solvent to a powder raw material that is in a fluid state in a mixer Method. The manufacturing method of Claim 1 whose powder raw material is the powder containing a bleaching activator. The production method according to claim 1 or 2, wherein the means for removing the solvent and / or water is drying. The bleach activator composition obtained by the manufacturing method in any one of Claims 1-3. A bleaching activator granulated product obtained by further granulating the bleach activator composition according to claim 4 .