JP2007177013A - Method for producing powder detergent composition - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method capable of producing a powder detergent composition in which the influence of an acid precursor of an anionic surfactant on the color of detergent particles is reduced. <P>SOLUTION: The method for producing a powder detergent composition comprises: a step (a) for dissolving a fluorescent dye in a solvent; a step (b) for mixing a solution obtained by the step (a) with an acid precursor of an anionic surfactant; and a step (c) for bringing the mixture obtained by the step (b) into contact with a water-soluble alkaline inorganic substance to thereby neutralize the precursor of an anionic surfactant in the mixture. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a method for producing a powder detergent composition.

  From the viewpoint of energy saving, in recent years, a method for producing a powder detergent for clothing, particularly a high bulk density powder detergent without using a drying tower has been proposed. A production method including neutralizing an acid precursor of an anionic surfactant with a solid alkali inorganic material is one of the most important ones. That is, a method for producing a high bulk density detergent in which an acid precursor of an anionic surfactant (water content of 1% or less) is used as a starting material and neutralized with a solid alkali inorganic material is a surfactant that is an example of a current detergent production method. Unlike the production method in which the aqueous slurry (water content of 30 to 70%) is spray-dried using a starting material, a large-scale spray-drying apparatus is not required, so that the equipment cost is low and the energy is saved. For example, Patent Document 1 discloses a method of producing detergent particles by neutralizing an acid precursor of an anionic surfactant with a granular neutralizer having a small particle size.

In addition, in a production method including neutralizing an acid precursor of such an anionic surfactant with a solid alkali inorganic material (so-called dry neutralization), as a technique for uniformly dispersing a fluorescent dye, Patent Literature A few are proposed.
JP-A-10-152700 JP-A-9-506122 JP 11-236599 A

  However, when a detergent is obtained by dry neutralization, there is a problem that the hue of the acid precursor of an anionic surfactant, particularly the alkylbenzenesulfonic acid, greatly affects the hue of the finally obtained detergent particles.

  The problem of the present invention is to solve such problems and reduce the influence of the acid precursor of the anionic surfactant on the hue of the detergent particles (for example, the detergent particles are colored yellow due to the influence of the hue of alkylbenzene sulfonic acid). To provide a production method capable of obtaining a powder detergent composition.

The present invention relates to a method for producing a powder cleaning composition comprising the following steps (a), (b) and (c).
Step (a): Step of dissolving fluorescent dye in solvent Step (b): Step of mixing solution obtained by step (a) and acid precursor of anionic surfactant Step (c): Step (b) The step of bringing the mixture obtained by the above into contact with a water-soluble alkaline inorganic substance and neutralizing the acid precursor of the anionic surfactant in the mixture

  The present invention also relates to a powder detergent composition having a bulk density of 500 g / L or more obtained by the production method of the present invention.

  According to the present invention, the influence of the acid precursor of the anionic surfactant on the hue of the detergent particles is reduced (for example, the detergent particles are reduced in yellow color due to the influence of the hue of the alkylbenzene sulfonic acid) and powder washing is performed. The manufacturing method which can obtain an agent composition is provided.

<Process (a)>
Step (a) is a step of preparing a fluorescent dye solution by dissolving the fluorescent dye in a solvent. The solvent may be any solvent that can dissolve the fluorescent dye, and may be a single solvent or a mixed solvent.

  In the step (a), a first combination in which the solvent is a mixed solvent containing water and a nonionic surfactant can be employed.

  Nonionic surfactants include polyoxyalkylene alkyl ether, sorbitan fatty acid ester, polyoxyalkylene sorbitan fatty acid ester, polyoxyalkylene sorbitol fatty acid ester, glycerin fatty acid ester, polyoxyalkylene fatty acid ester, polyoxyalkylene hydrogenated castor oil, polyoxyalkylene Examples thereof include oxyalkylene alkyl amines and alkyl alkanol amides. Among them, polyoxyalkylene alkyl ether is preferable, and polyoxyethylene alkyl ether having an average added mole number of ethylene oxide of 4 to 50 and an alkyl group having 8 to 18 carbon atoms is more preferable. Although the density | concentration of a nonionic surfactant is based also on the composition in a final detergent composition, 50-80 mass% in the sum total of water and a nonionic surfactant is 60 to 70 mass%.

    In the step (a), a second combination in which the solvent is a mixed solvent containing water, an alcohol having 1 to 3 carbon atoms (preferably methyl alcohol) and a nonionic surfactant can be employed. The nonionic surfactants described above can be used.

  In the second combination, the concentration of the nonionic surfactant depends on the composition in the final detergent composition, but 50 to 80 mass in the total of water, the nonionic surfactant and the alcohol having 1 to 3 carbon atoms. %, And more preferably 60 to 70% by mass. Moreover, although the density | concentration of C1-C3 alcohol is based also on the composition in a final detergent composition, it is 10-50 mass% in the sum total of water, a nonionic surfactant, and C1-C3 alcohol, 20-40 mass% is preferable.

  The fluorescent dye used in the step (a) is not particularly limited, but, for example, a dye having a solubility in ion exchange water at 30 ° C. of preferably 0.05% by mass or more, more preferably 1% by mass or more. Can be mentioned. Examples of fluorescent dyes having a solubility in ion-exchanged water at 30 ° C. of 0.05% by mass or more include Photin CBUS-3B (manufactured by Hixon), Photin CBUS-560B (manufactured by Hixon), and # 31 (manufactured by Shanghai Fine Chemicals). ), BRY-10 D2100 (manufactured by McTesim), Chino Pearl AMS-GX (manufactured by Ciba Specialty Chemicals), blank fore RKH 120% (manufactured by Bayer), blank fore HRS (manufactured by Bayer), Chino Pearl LMS-X (Ciba) Specialty Chemicals), Hotin CBUS-Ultra (made by Hixon), Shino White CBW-HI Conc (made by Kyungjin), Opti Blank BT-11 extra Conc (made by 3V Sigma), Chino Pearl TAS (Cibas) Charity Chemicals), Chinosorb FD (Ciba Specialty Chemicals), Chinosorb FR (Ciba Specialty Chemicals), Chino Pearl UNPA-GX (Ciba Specialty Chemicals), Chino Pearl 5BM-GX (Ciba Specialty) Chemicals), Chino Pearl CBS-X (Ciba Specialty Chemicals), Shining CF-351 (Shenyang Chemical), A-1497 (Ciba Specialty Chemicals), A-1455 (Ciba Specialty Chemicals) Product), W-3346 (manufactured by Ciba Specialty Chemicals), Chino Pearl PLC (manufactured by Ciba Specialty Chemicals), and the like.

  Among them, as fluorescent dyes having a solubility in ion-exchanged water at 30 ° C. of 1% by mass or more, for example, Tinopearl CBS-X (manufactured by Ciba Specialty Chemicals), Shining CF-351 (manufactured by Shenyang Chemical), A- 1497 (manufactured by Ciba Specialty Chemicals), A-1455 (manufactured by Ciba Specialty Chemicals), W-3346 (manufactured by Ciba Specialty Chemicals), Chino Pearl PLC (manufactured by Ciba Specialty Chemicals), and the like.

  In the step (a), the temperature of the solvent (mixed solution) is preferably 20 to 60 ° C. The concentration of the fluorescent dye in the fluorescent dye solution is not particularly limited as long as the fluorescent dye can be dissolved. Although depending on the composition in the final detergent composition, it is preferably 5 to 30% by mass, more preferably 10 to 25% by mass from the viewpoint of handling properties.

  The mixer used in this step is not particularly limited, and examples thereof include a liquid mixing tank equipped with a stirrer. Moreover, although it is sufficient that each component is uniformly mixed, it is preferable that the fluorescent dye is uniformly dissolved.

<Step (b)>
Step (b) is a step of obtaining a mixture by mixing the fluorescent dye solution obtained by step (a) and an acid precursor of an anionic surfactant.

  The acid precursor of an anionic surfactant (hereinafter referred to as an acid precursor) is an acid form of an anionic surfactant, which is in a liquid form, and forms a salt by a neutralization reaction. The acid precursor is an acid form of a known anionic surfactant and is not particularly limited as long as it is a liquid. Linear alkylbenzene sulfonic acid (LAS), α-olefin sulfonic acid (AOS), alkyl Examples include sulfuric acid (AS), internal olefin sulfonic acid, fatty acid ester sulfonic acid, alkyl ether sulfuric acid, dialkyl sulfosuccinic acid, and fatty acid. As the acid precursor, only one component may be used, or two or more components may be used in combination.

  The amount of the acid precursor can be appropriately set based on the composition of the cleaning composition, but is preferably 5 to 45% by mass as an anionic surfactant generated by a neutralization reaction in the final product composition. 10 to 40% by mass is more preferable, 20 to 40% by mass is particularly preferable, and 20 to 35% by mass is further preferable. The present invention is effective even when the main surfactant in the cleaning composition is provided in another form.

  The mixing ratio of the fluorescent dye solution and the acid precursor can be appropriately set depending on the composition of the cleaning composition, but from the viewpoint of production suitability, the fluorescent dye solution is preferably 1 to 10% by mass in the mixture. Preferably it is 1-7 mass%.

  The mixer used in this step is not particularly limited, and examples thereof include a liquid mixing tank equipped with a stirrer. Further, it is sufficient that each component is mixed uniformly.

<Step (c)>
Step (c) is a step of bringing the mixture obtained in step (b) into contact with a water-soluble alkaline inorganic substance and neutralizing the acid precursor of the anionic surfactant in the mixture.

In the step (c), the mixture of the fluorescent dye solution and the acid precursor obtained in the step (b) is brought into contact with a water-soluble alkaline inorganic substance, and dry neutralization of the acid precursor is performed. In this step, neutralization reaction and granulation occur simultaneously and in contact with the acid precursor to form neutralized particles. For example, this process can be performed including the following process (c1) and process (c2). That is,
Step (c1): a water-soluble alkaline inorganic material in an amount (neutralization equivalent) or more necessary to neutralize the acid precursor in the mixture of the fluorescent dye solution and the acid precursor obtained in the step (b), And / or mixing with known substances commonly used in detergent compositions;
Step (c2): The mixture obtained in step (c1) is granulated by bringing the mixture obtained in step (c1) into contact with the mixture of the fluorescent dye solution obtained in step (b) and the acid precursor. It is the process of neutralizing, maintaining. In order to keep the mixture granular, the acid precursor may be added gradually.

  Examples of water-soluble alkaline inorganic substances include those usually used as alkaline agents in detergent compositions, such as sodium carbonate, sodium bicarbonate, sodium silicate, potassium carbonate, phosphate, polyphosphate, crystalline silicate. , Etc. are exemplified.

  Among alkali inorganic substances, sodium carbonate is a preferred embodiment, and sodium carbonate can function as a detergent builder and an alkaline agent in the final composition. Therefore, the neutralization reaction can be satisfactorily performed by adding and mixing in the step (c) in an amount including sodium carbonate for the above functions. That is, the amount of the alkali inorganic material is preferably more than the amount necessary for neutralization, for example, 1 to 20 times the neutralization equivalent, more preferably 2 to 10 times, particularly preferably 3 to 8 times. .

  The water-soluble alkali inorganic substance is used as a particulate solid, and the average particle diameter is not particularly limited, but is preferably 30 μm or more, more preferably 40 to 200 μm from the viewpoint of yield improvement and storage stability. Especially preferably, it is 50-100 micrometers. In addition, the average particle diameter of the particulate solid water-soluble alkali inorganic substance referred to in the present specification is calculated on a volume basis, and a laser diffraction particle size distribution analyzer: LA-500 (manufactured by Horiba, Ltd.) is used. It is a value measured using.

  When obtaining a detergent composition having tripolyphosphate as a main builder, the average particle size of tripolyphosphate is not particularly limited, but is preferably 1 to 30 μm, more preferably 5 to 20 μm. More preferably, it is 6-15 micrometers. From the viewpoint of suppressing agglomeration of the neutralized granular mixture, the smaller the average particle size of the tripolyphosphate, the better the yield, but from the viewpoint of productivity for industrially obtaining a small particle size, the average The particle size is preferably 1 μm or more, and preferably 30 μm or less from the viewpoint of suppressing aggregation of the neutralized granular mixture. In addition, the average particle diameter of the tripolyphosphate referred to in the present specification is calculated on a volume basis, and is measured using a laser diffraction particle size distribution analyzer: LA-500 (manufactured by Horiba, Ltd.). Value. Moreover, although the addition time of a tripolyphosphate is not specifically limited, Preferably it is a process (c1) and the quantity is not specifically limited, either 2-50 in the detergent composition which is a final product. % By mass is preferable, 10 to 40% by mass is more preferable, and 15 to 35% by mass is particularly preferable. 2 mass% or more is preferable from a viewpoint of aggregation suppression of the neutralized granular mixture, and 50 mass% or less is preferable from a viewpoint of ensuring the composition freedom of a cleaning composition.

  In addition, when obtaining a detergent composition having an alkali metal aluminosilicate as a main builder, adding an alkali metal aluminosilicate in step (c) suppresses excessive aggregation and stirs and granulates the aggregate. This is suitable because it is an auxiliary agent for crushing with a chopper of a machine. The average particle diameter of the alkali metal aluminosilicate is preferably 1 to 30 μm.

  The average particle size of the aluminosilicate is calculated on a volume basis, and is a value measured using a laser diffraction particle size distribution analyzer: LA-500 (manufactured by Horiba, Ltd.).

  Furthermore, in this invention, you may add and mix the well-known substance generally used for a detergent composition. Such substances include pigments, anti-staining agents (polycarboxylate polymers, sodium carboxymethyl cellulose, etc.), particulate surfactants (fatty acids or salts thereof, linear alkylbenzene sulfonates, alkyl sulfates, etc.), spray-dried powders Diatomaceous earth, calcite, kaolin, bentonite, sodium sulfate, sodium sulfite and the like. Such a substance is arbitrarily used depending on its application. When such a substance is added, it is preferably used by mixing with a water-soluble alkaline inorganic substance. Further, the amount of pigment, anti-staining agent, particulate surfactant, spray dried powder, diatomaceous earth, calcite, kaolin, bentonite, sodium sulfate, sodium sulfite and the like are not particularly limited.

  Although it does not specifically limit as a mixer for mixing said each component used in a process (c), A stirring granulator is used suitably. The stirring granulator is not particularly limited, but a stirring granulator having a stirring blade and a crushing / dispersing chopper (or a functionally equivalent one) is preferable.

  Specific examples of the agitation granulator used in the present invention include a batch granulator, a vertical granulator (manufactured by POWREC Co., Ltd.), a high speed mixer (manufactured by Fukae Kogyo Co., Ltd.), and a redige mixer ((stock ) Matsubo), Proshare mixer (manufactured by Taiheiyo Kiko Co., Ltd.), Garycke mixer (manufactured by Meiji Kikai Co., Ltd.), and the like. Particularly preferred are Redige mixers and Proshare mixers. As a continuous type, continuous-type Redige mixer (medium speed mixer: relatively long residence time), CB recycler (manufactured by Loedige), turbulizer (Hosokawa Micron Corporation) )), Shugi mixer (manufactured by Powrec Co., Ltd.), flow jet mixer (manufactured by Powder Research Co., Ltd.), and the like. In the present invention, the mixers may be used in appropriate combination.

  Further, the stirring granulator is more preferably equipped with a jacket for adjusting the internal temperature or equipped with a nozzle for performing a gas blowing operation.

  The degree of mixing in step (c) is not particularly limited as long as each component is uniformly mixed. For example, when an agitation granulator is used, the operating condition of the agitation granulator is preferably, for example, a mixing time of within 5 minutes. The spindle stirring speed and crushing / dispersing chopper speed can be appropriately set depending on the model. For example, in the case of a batch type, the spindle stirring peripheral speed is preferably 2 to 15 m / s. Is preferably 20 to 60 m / s.

  In addition, you may add the water as a reaction initiator during the mixing in a process (c), or after completion | finish of mixing. The addition of a reaction initiator is preferable because the neutralization reaction can be promoted. The amount of water added is not particularly limited, but is preferably 0.2 to 3 parts by mass and more preferably 0.5 to 1.5 parts by mass with respect to 100 parts by mass of the powder mixture in the step (c). From the viewpoint of initiating the neutralization reaction, 0.2 part by mass or more is preferable, and from the viewpoint of suppressing aggregation of the detergent composition particles, 3 part by mass or less is preferable. In addition, when components such as acid precursors contain water, when using other aqueous solution raw materials, or when using powder raw materials containing water, considering the amount of water, the amount of water to be added Just decide.

  Moreover, alkaline aqueous solution can be added as a more preferable reaction initiator. By using an alkaline aqueous solution as a reaction initiator, not only can the neutralization reaction be promoted more than in the case of water, but also the particle size of the resulting particles can be reduced and the bulk density can be increased.

  The addition amount of the alkaline aqueous solution is preferably 0.05 to 0.5 times the neutralization equivalent of the acid precursor, more preferably 0.10 to 0.45 times, and particularly preferably 0.15 to 0.40 times. From the viewpoint of starting the neutralization reaction and obtaining a desired effect, the amount is preferably 0.05 times or more the neutralization equivalent, and from the viewpoint of suppressing particle aggregation, it is preferably 0.5 times or less. The concentration of the aqueous alkaline solution is not particularly limited. However, when the concentration is low, excessive water is supplied to the mixture as a predetermined amount of the aqueous alkaline solution is added, and thus aggregation of particles may occur. Therefore, the concentration of the alkaline aqueous solution is preferably 20 to 50% by mass, more preferably 30 to 50% by mass, and particularly preferably 40 to 50% by mass.

  Further, the type of the alkaline aqueous solution used is not particularly limited, and examples thereof include strong alkaline aqueous solutions that easily cause a neutralization reaction with an acid precursor, such as a sodium hydroxide aqueous solution and a potassium hydroxide aqueous solution. Among these, a sodium hydroxide aqueous solution is preferably used from the viewpoint of cost. Further, such an aqueous alkaline solution preferably has a pH of 12 or more.

  Further, the mixing is preferably performed to such an extent that the added aqueous alkali solution is uniformly dispersed.

  In order to dry neutralize the acid precursor, a mixture of the acid precursor and the fluorescent dye solution may be gradually added to the water-soluble alkaline inorganic substance. Although the time required for the addition of the mixture depends on the amount to be added, it cannot be generally stated. However, in the case of a batch type, it is generally 1 minute or more, more preferably 1 to 10 minutes, further preferably 2 to 7 minutes. It is. Here, if the above-mentioned mixture is added in a remarkably short time, unreacted liquid acid tends to accumulate, and excessive aggregation tends to occur.

  Moreover, as an addition method of the above-mentioned mixture, you may carry out continuously or divided | segmenting into multiple times, and you may provide multiple addition means.

  Further, after the addition of the above-mentioned mixture, the stirring granulator may be further operated for 30 seconds or longer, more preferably for 1 minute or longer. By performing such an operation, the neutralization reaction and the granulation operation can be completed, which is preferable.

In the step (c), neutralization is preferably performed while blowing gas. This is for the purpose of preventing the particulate matter from becoming a large lump by evaporating excess water generated by the neutralization reaction and cooling the particulate matter using gas. Examples of such gas include N ₂ gas and air. The amount of gas blown in (aeration amount) is not particularly limited, but is preferably 0.002 parts by mass or more per minute, and more preferably 0.02 parts by mass or more per 100 parts by mass of the granular material.

  As described above, the dry neutralization step is completed.

The powder cleaning composition which is a granular mixture with a bulk density of 500 g / L or more can be obtained by the production method including the above steps. As for the detergent composition obtained by the manufacturing method of this invention, what shows the following physical properties is more preferable.
Bulk density: 500 to 950 g / L is preferable, and 700 to 900 g / L is more preferable. In the present specification, the bulk density is a value obtained by a method defined in JIS K 3362.

Particle size: The average particle size is preferably 1000 μm or less, more preferably 850 μm or less, more preferably 300 to 800 μm, particularly preferably 350 to 650 μm from the viewpoint of dissolution rate. Further, the proportion of 1400 μm or less (1400 μm pass yield) (%) is preferably 55% or more, more preferably 60% or more, more preferably 65% or more, and more than 70%. Particularly preferred. In the present specification, the average particle diameter of the cleaning composition is a value obtained from a mass fraction according to the size of the sieve mesh after being vibrated for 5 minutes using a standard sieve of JIS K 8801. A rate is a value calculated | required from the ratio for which a particle | grain of 1400 micrometers or less occupies this mass fraction.
Fluidity: preferably 8 seconds or shorter, more preferably 7 seconds or shorter. In this specification, the fluidity of the cleaning composition is the time required for 100 mL of powder to flow out from the bulk density measurement hopper defined in JIS K 3362.

  In this invention, you may further provide the process (d) which is a process of surface-modifying the granular mixture obtained at a process (c). In order to further improve the fluidity and storage stability of the detergent composition obtained by this production method, it is effective to provide the step (d). Specifically, surface modification is achieved by adding a predetermined amount of the surface modifying agent shown below while mixing the granular mixture obtained in step (c) with a stirring granulator.

  As the surface modifier, a commonly used known one can be used, and crystalline or amorphous alkali metal aluminosilicate, calcite, diatomaceous earth, silica and the like are preferably used. Such an aluminosilicate preferably has an average particle size of 1 to 30 μm, more preferably 1 to 10 μm or less. Moreover, as the quantity, 2-15 mass% is preferable in the detergent composition which is a final product, and 4-12 mass% is more preferable. The average particle diameter of the surface modifier is calculated on a volume basis, and is a value measured using a laser diffraction particle size distribution analyzer: LA-500 (manufactured by Horiba, Ltd.). The operation time of the stirring granulator when the surface modifier is added is not particularly limited, but is preferably 1 to 5 minutes.

  In this production method, a desired liquid component can be added depending on the composition of the detergent composition to be obtained. The liquid component may be added in any of the steps (a), (b), (c), and (d), for example, preferably before the surface modifier is added. Examples of the liquid component include any liquid component in the detergent composition such as a liquid nonionic surfactant, an aqueous polymer solution (polyethylene glycol, maleic acrylate copolymer, etc.), and a fatty acid. As the liquid component, only one component may be used, or two or more components may be used in combination. The amount of the liquid component is preferably 15% by mass or less, and more preferably 10% by mass or less, of the cleaning composition as the final product, from the viewpoint of suppressing aggregation of the cleaning composition. Moreover, the operation time of the stirring granulator when the liquid component is performed before the addition of the surface modifier is not particularly limited, but is preferably 0.5 to 8 minutes.

  In the present invention, other optional components may be added. Examples of such optional components include enzymes, fragrances, bleaches, bleach activators, and colored particles. Such components are blended by mixing the cleaning composition obtained by the production method of the present invention and the above components using a mixer such as a rotating drum. Moreover, you may use the high bulk density cleaning composition obtained by the manufacturing method of this invention as another component for cleaning composition composition.

Example 1
A detergent composition was produced in units of 35 kg using a Redige mixer FKM-130D (manufactured by Matsubo Co., Ltd.). This mixer is equipped with a shearing machine corresponding to a stirring blade and a crushing / dispersing chopper. Here, the detergent composition was prepared by the following operation.

Step (a): The solution obtained in step (a) is 100% by mass, Tinopal CBS-X (manufactured by Ciba Specialty Chemicals) 15% by mass, carbon number 12/14 = 6/4 at 50 ° C., ethylene Tinopal CBS-X (manufactured by Ciba Specialty Chemicals Co., Ltd.), which is a fluorescent dye, is mixed and stirred at 50 ° C with 60% by mass of an average 7.7 mol addition type nonionic surfactant and 25% by mass of ion-exchanged water at 50 ° C. ) Was dissolved.

Step (b): 0.08% by mass (the ratio in the final composition, the same applies hereinafter) of the solution obtained by the step (a) as a blending amount of the fluorescent dye, and linear alkyl having 50 ° C. (10 to 10 carbon atoms) 13) 29.88% by mass of benzenesulfonic acid (manufactured by Nippon Petrochemical Co., Ltd.) was stirred at 50 ° C. for 15 minutes.

Step (c): Sodium carbonate as a solid component (light ash: manufactured by Central Glass Co., Ltd., average particle size 56.1 μm) 40.59% by mass, sodium tripolyphosphate (manufactured by Mitsui Chemicals, Inc .: average particle size 11.2 μm) ) Mix 20.0% by mass in advance with a Redige mixer under the conditions of stirring blade rotation speed 130 rpm (circumferential speed 3.4 m / s) and shearing machine rotation speed 2850 rpm (circumferential speed 27 m / s). The mixture obtained in the step (b) was added for 4 minutes while being operated under the same conditions as above, followed by dry neutralization and granulation. During this time, water at 25 ° C. was cooled through the mixer jacket. At this stage, the temperature reached a maximum of 68.8 ° C. Throughout this stage, the reaction mixture was granular. After adding the liquid mixture obtained by the step (b), the mixer was continuously operated for 1 minute under the same conditions. Further, while operating the mixer under the same conditions as described above, an aqueous solution of 40% by mass maleic acrylate copolymer (acrylic acid / maleic acid = 7/3 molar ratio, weight average molecular weight 70000) was added to the 1.2% by mass mixer. After mixing for 30 minutes, surface modification was performed by adding 7.51% by mass of zeolite having an average particle size of 4 μm as a surface modifier in step (d) and operating the mixer for 2 minutes. The zeolite contained 20% by mass of crystal water. Furthermore, the detergent composition obtained by mixing 0.3% by mass of Savinase 12T Type W Blue (manufactured by Novozymes) was passed through a 1400 μm sieve, and the passed particles were used as the final detergent composition. The b value of the composition was 1.0, which was particles with a whiter powder hue than Comparative Examples 1 and 3 described later. In addition, b value was measured by Color Meter SE 2000 (Nippon Denshoku).

Example 2
The amount of the fluorescent dye in step (b) is 0.16% by mass (ratio in the final composition, the same applies hereinafter), and sodium carbonate (light ash: manufactured by Central Glass Co., Ltd.), which is a solid component in step (c) The cleaning composition was obtained by the same composition and operation as in Example 1 except that the average particle size was 56.1 μm. The components used are the same as in Example 1. The b value of the composition was 0.7, which was particles with a whiter powder hue than Comparative Examples 1 and 3 described later.

Example 3
Using the same Redige mixer FKM-130D (manufactured by Matsubo Co., Ltd.) as in Example 1, a detergent composition was produced in units of 35 kg by the following operation.

Step (a): The solution obtained in step (a) is 100% by mass, 12.5% by mass of ion-exchange water and 12.5% by mass of methyl alcohol are mixed at 20 ° C., and there is Photin CBUS-3B (Hixon). 15% by mass), and mixed with stirring and stirred with 60% by mass of nonionic surfactant having carbon number of 12/14 = 6/4 at 50 ° C. and an average of 7.7 moles of ethylene oxide. Dissolution of Photin CBUS-3B (Hixon) was confirmed.

Step (b): 0.08% by mass (the ratio in the final composition, the same applies hereinafter) of the solution obtained by the step (a) as a blending amount of the fluorescent dye, and linear alkyl having 50 ° C. (10 to 10 carbon atoms) 13) 29.88% by mass of benzenesulfonic acid (manufactured by Nippon Petrochemical Co., Ltd.) was stirred at 50 ° C. for 15 minutes.

Step (c): Sodium carbonate as a solid component (light ash: manufactured by Central Glass Co., Ltd., average particle size 56.1 μm) 40.59% by mass, sodium tripolyphosphate (manufactured by Mitsui Chemicals, Inc .: average particle size 11.2 μm) ) Mix 20.0% by mass in advance with a Redige mixer under the conditions of stirring blade rotation speed 130 rpm (circumferential speed 3.4 m / s) and shearing machine rotation speed 2850 rpm (circumferential speed 27 m / s). The mixture obtained in the step (b) was added for 4 minutes while being operated under the same conditions as above, followed by dry neutralization and granulation. During this time, water at 25 ° C. was cooled through the mixer jacket. At this stage, the temperature reached a maximum of 68.8 ° C. Throughout this stage, the reaction mixture was granular. After adding the liquid mixture obtained by the step (b), the mixer was continuously operated for 1 minute under the same conditions. Further, while operating the mixer under the same conditions as described above, an aqueous solution of 40% by mass maleic acrylate copolymer (acrylic acid / maleic acid = 7/3 molar ratio, weight average molecular weight 70000) was added to the 1.2% by mass mixer. After mixing for 30 minutes, surface modification was performed by adding 7.51% by mass of zeolite having an average particle size of 4 μm as a surface modifier in step (d) and operating the mixer for 2 minutes. The zeolite contained 20% by mass of crystal water. Furthermore, the detergent composition obtained by mixing 0.3% by mass of Savinase 12T Type W Blue (manufactured by Novozymes) was passed through a 1400 μm sieve, and the passed particles were used as the final detergent composition. The components used are the same as in Example 1. The b value of the composition was 1.8, which was particles with a whiter powder hue than Comparative Example 2 described later.

Comparative Example 1
Using the same Redige mixer FKM-130D (manufactured by Matsubo Co., Ltd.) as in Example 1, a detergent composition was produced in units of 35 kg by the following operation.

  Sodium carbonate (light ash: manufactured by Central Glass Co., Ltd., average particle size 56.1 μm) 40.59% by mass (ratio in the final composition, the same applies hereinafter), sodium tripolyphosphate (manufactured by Mitsui Chemicals, Inc.) The average particle size of 11.2 μm) 20.44% by mass of Tinopal CBS-X (manufactured by Ciba Specialty Chemicals) 0.08% by mass in advance with a Readyge mixer was added to a stirring blade speed of 130 rpm (circumferential speed 3.4 m / s), and mixing was performed for 1 minute under conditions of a shearing machine rotational speed of 2850 rpm (circumferential speed 27 m / s).

  While operating the mixer under the same conditions as described above, 29.88% by mass of linear alkyl (10 to 13 carbon atoms) benzenesulfonic acid (manufactured by Shin Nippon Petrochemical Co., Ltd.) was added in 4 minutes to dry neutralize and granulate. During this time, water at 25 ° C. was cooled through the mixer jacket. At this stage, the temperature reached a maximum of 68.8 ° C. Throughout this stage, the reaction mixture was granular. After the addition of the linear alkylbenzene sulfonic acid, the mixer was continuously operated for 1 minute under the same conditions. Further, while the mixer was operated under the same conditions as described above, an aqueous solution of 40% by mass acrylic acid maleic acid copolymer (acrylic acid / maleic acid = 7/3 molar ratio, weight average molecular weight 70000) was added to the 1.2% by mass mixer. After mixing for 30 minutes, surface modification was performed by adding 7.51% by mass of zeolite having an average particle size of 4 μm as a surface modifier in step (d) and operating the mixer for 2 minutes. The zeolite contained 20% by mass of crystal water. Furthermore, the detergent composition obtained by mixing 0.3% by mass of Savinase 12T Type W Blue (manufactured by Novozymes) was passed through a 1400 μm sieve, and the passed particles were used as the final detergent composition. The components used are the same as in Example 1. The composition had a b value of 4.5 and was a particle having a poor powder hue.

Comparative Example 2
A detergent composition was obtained by the same composition and operation as in Comparative Example 1 except that Tinopal CBS-X (manufactured by Ciba Specialty Chemicals) of Comparative Example 1 was replaced with Photin CBUS-3B (manufactured by Hixon). The b value of the composition was 4.8, which was a particle having an inferior powder hue.

Comparative Example 3
Tinopal CBS-X (manufactured by Ciba Specialty Chemicals) with 29.88% by mass (ratio in the final composition, the same applies hereinafter) of linear alkyl (carbon number 10 to 13) benzenesulfonic acid (manufactured by Nippon Petrochemical Co., Ltd.) What prepared 0.08 mass% of dispersion | distribution for 24 hours at 25 degreeC was prepared.

  Solid component sodium carbonate (light ash: Central Glass Co., Ltd., average particle size 56.1 μm) 40.59% by mass, sodium tripolyphosphate (Mitsui Chemicals, Inc .: average particle size 11.2 μm) 20.44 masses Is mixed in advance with a Redige mixer for 1 minute under the conditions of a stirring blade rotation speed of 130 rpm (circumferential speed 3.4 m / s) and a shearing machine rotation speed of 2850 rpm (circumferential speed 27 m / s). The dispersion liquid of linear alkyl (carbon number 10 to 13) benzenesulfonic acid (manufactured by Nippon Petrochemical Co., Ltd.) and Tinopal CBS-X (manufactured by Ciba Specialty Chemicals Co., Ltd.) was obtained for 4 minutes. And dry neutralized and granulated. During this time, water at 25 ° C. was cooled through the mixer jacket. At this stage, the temperature reached a maximum of 68.8 ° C. Throughout this stage, the reaction mixture was granular. After adding the linear alkyl (C10-13) benzenesulfonic acid (manufactured by Shin Nippon Petrochemical Co., Ltd.) and Tinopal CBS-X (manufactured by Ciba Specialty Chemicals Co.) dispersion obtained above, Run for 1 minute. Further, while operating the mixer under the same conditions as described above, an aqueous solution of 40% by mass maleic acrylate copolymer (acrylic acid / maleic acid = 7/3 molar ratio, weight average molecular weight 70000) was added to the 1.2% by mass mixer. After mixing for 30 minutes, surface modification was performed by adding 7.51% by mass of zeolite having an average particle size of 4 μm as a surface modifier in step (d) and operating the mixer for 2 minutes. The zeolite contained 20% by mass of crystal water. Furthermore, the detergent composition obtained by mixing 0.3% by mass of Savinase 12T Type W Blue (manufactured by Novozymes) was passed through a 1400 μm sieve, and the passed particles were used as the final detergent composition. The components used are the same as those in Comparative Example 1. The composition had a b value of 4.2 and was a particle having a poor powder hue.

Claims (5)

The manufacturing method of a powder cleaning composition containing following process (a), (b) and (c).
Step (a): Step of dissolving fluorescent dye in solvent Step (b): Step of mixing solution obtained by step (a) and acid precursor of anionic surfactant Step (c): Step (b) The step of bringing the mixture obtained by the above into contact with a water-soluble alkaline inorganic substance and neutralizing the acid precursor of the anionic surfactant in the mixture The method for producing a powder detergent composition according to claim 1, wherein the solvent in step (a) is a mixed solvent containing water and a nonionic surfactant. The method for producing a powder cleaning composition according to claim 1, wherein the solvent in the step (a) is a mixed solvent containing water, an alcohol having 1 to 3 carbon atoms and a nonionic surfactant. The method for producing a powder detergent composition according to any one of claims 1 to 3, wherein the fluorescent dye in step (a) is a fluorescent dye having a solubility in ion-exchanged water at 30 ° C of 1% by mass or more. A powder cleaning composition having a bulk density of 500 g / L or more, obtained by the production method according to claim 1.