JP2003105396A - Method for producing granular detergent composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method for producing a granular detergent composition having excellent poroductivity, that is, having a low viscosity of a concentrate and free from separation when an α-sulfofatty cid ester salt-containing mixed slurry is concentrated. SOLUTION: The method for producing a granular composition comprises the following processes (A) to (C). (A) A process in which an α-sulfofatty acid ester salt (a)-containing aqueous slurry and a nonionic surfactant (b) are mixed. (B) A process in which the mixed solution obtained in the process (A) is introduced into a thin film evaporator and concentrated so that the concentrate satisfies following conditions by mass ratio. 0.05<=water (c)/[the component (a)+the component (b)+the component (c)]<=0.2; and the component (b)/[the component (a)+the component (b)+the component (c)]=0.15-0.28. (C) A process in which the concentrate obtained in the process (B) is granulated.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a granular detergent composition. More specifically, the present invention relates to a method for producing a granular detergent composition, and a mixed slurry containing an α-sulfo fatty acid ester salt and a specific amount of a nonionic surfactant is mixed into a thin film evaporator. In the process of granulating after being concentrated by the method described above, when the mixed slurry containing the α-sulfofatty acid ester salt is concentrated, the viscosity of the concentrate is low, and the production of a granular detergent composition excellent in operability without separation occurs. Regarding the method.

[0002]

2. Description of the Related Art Conventionally, in the method for producing a granular detergent composition, when the .alpha.-sulfofatty acid ester salt is concentrated and then granulated, there has been a problem that the concentrate has high viscosity and poor handling property.

In order to solve such a problem, Japanese Patent Laid-Open No. 9-
Japanese Patent No. 20900 proposes a method of concentrating a mixed slurry of an α-sulfofatty acid ester salt and soap and granulating the obtained concentrate after cooling.

However, even in this proposal, the viscosity of the obtained concentrate is high and handling is difficult,
Further, when the amount of the nonionic surfactant is increased in order to reduce the viscosity, the α-sulfofatty acid ester salt and the nonionic surfactant are separated, and there is a problem that the operability after concentration is unstable. At present, a method for producing a granular detergent composition having stability is not yet provided.

[0005]

SUMMARY OF THE INVENTION Under the circumstances, the present invention aims to solve various problems in the related art and achieve the following objects. That is, the present invention provides a mixture containing an α-sulfofatty acid ester salt in a process of granulating a mixed slurry containing an α-sulfofatty acid ester salt and a specific amount of a nonionic surfactant after concentrating with a thin film evaporator. It is an object of the present invention to provide a method for producing a granular detergent composition which has a low viscosity of the concentrate when concentrating the slurry, has excellent operability without separation, and is highly efficient.

[0006]

In order to solve the above problems, the present invention provides the following method for producing a granular detergent composition.

The invention of claim 1 is a method for producing a granular detergent composition, which comprises the following steps (A) to (C): (A) Step of mixing (a) an aqueous slurry containing an α-sulfofatty acid ester salt with (b) a nonionic surfactant (B) The mixed slurry obtained in the step (A) is introduced into a thin film evaporator. , The concentrate is in a mass ratio of 0.05 ≦ (c) water /
[(A) component + (b) component + (c) component] ≤ 0.2, and (b) component / [(a) component + (b) component + (c) component] = 0.15 to 0. The step of concentrating so as to satisfy the condition of 28 (C) the step of granulating the concentrate in the step (B). The invention of claim 2 includes the step (d1) in the step (A).
Fatty acid soap and / or (d2) polyoxyalkylene glycol in a mass ratio [(d1) component + (d2) component]
/ [(A) component + (b) component + (d1) component + (d2)
Ingredient] = 0.001-0.25 It is a manufacturing method of the granular detergent composition according to claim 1 which is added so that the conditions may be met.

According to the present invention, by including the above steps (A) to (C), when the mixed slurry containing the α-sulfofatty acid ester salt is concentrated, the viscosity of the concentrate is low and the separation is performed. It is possible to achieve a highly efficient method for producing a granular detergent composition which is excellent in operability and which does not generate

[0009]

BEST MODE FOR CARRYING OUT THE INVENTION The present invention will be described in more detail below. The method for producing the granular detergent composition of the present invention includes the following steps (A) to (C). (A) Step of mixing (a) an aqueous slurry containing an α-sulfofatty acid ester salt with (b) a nonionic surfactant (B) The mixed slurry obtained in the step (A) is introduced into a thin film evaporator. , The concentrate is in a mass ratio of 0.05 ≦ (c) water /
[(A) component + (b) component + (c) component] ≦ 0.20,
And (b) component / [(a) component + (b) component + (c) component] = 0.15 to 0.28 concentration step so as to satisfy the condition (C) concentration in the (B) step The process of granulating things

<(A) Mixing Step> The mixing step (A) is a step of mixing (a) an aqueous slurry containing an α-sulfofatty acid ester salt with (b) a nonionic surfactant.

As the α-sulfo fatty acid ester salt (α-SF) as the component (a), those represented by the following general formula are generally used.

[0012]

[Chemical 1]

In the above formula, R ¹ has 10 to 2 carbon atoms.
2, preferably 12-18, particularly preferably 14-18
Is a linear or branched alkyl group or alkenyl group. R ² is a linear or branched alkyl group having 1 to 5 carbon atoms, preferably 1 to 4 carbon atoms, and examples thereof include a methyl group, an ethyl group, a propyl group and an isopropyl group. M is an alkali metal or ammonium,
Specific examples of the alkali metal include lithium, sodium, potassium and the like.

The α-SF is usually obtained by a known production method. For example, a fatty acid ester obtained by reacting fats and oils with a lower alcohol can be sulfonated with anhydrous sulfuric acid or the like, and finally neutralized with caustic alkali or the like. Examples of the raw material fats and oils include palm oil, palm kernel oil, pork oil, beef tallow, rice bran oil, palm oil,
Examples include fish oil.

As the nonionic surfactant as the component (b), an aliphatic alcohol having 6 to 22 carbon atoms, preferably 8 to 18 carbon atoms and an alkylene oxide having 2 to 4 carbon atoms on average 3 are used.
To 30 mol, preferably 5 to 20 mol added polyoxyalkylene alkyl (or alkenyl) ether and the like. Among these, polyoxyethylene alkyl (or alkenyl) ether, polyoxyethylene polyoxypropylene alkyl (or alkenyl) ) Ether is preferred. A primary alcohol or a secondary alcohol is used as the aliphatic alcohol. The alkyl group may have a branched chain. A primary alcohol is used as a preferable aliphatic alcohol.

Further, an alkylene oxide is added between ester bonds of a long-chain fatty acid alkyl ester, for example,
A fatty acid alkyl ester alkoxylate represented by the following general formula (1) can also be used. _{^{R 3 CO (OA) n OR}} 4 ... (1) ( In the ^{formula, R} 3 CO is 6 to 22 carbon atoms, .OA preferably represent from 8 to 18 of the fatty acid residues are ethylene oxide, propylene oxide, etc. Represents an addition unit of alkylene oxide having 2 to 4 carbon atoms, preferably 2 to 3 carbon atoms.
n represents the average number of moles of alkylene oxide added, and is generally 3 to 30, preferably 5 to 20. R ⁴ represents a lower alkyl group having 1 to 3 carbon atoms which may have a substituent. )

Examples of the fatty acid alkyl ester alkoxylate include polyoxyethylene sorbitan fatty acid ester, polyoxyethylene sorbitol fatty acid ester, polyoxyethylene fatty acid ester, polyoxyethylene hydrogenated castor oil, glycerin fatty acid ester, fatty acid alkanolamide and the like. .

Among the above nonionic surfactants, polyoxyethylene alkyl (or alkenyl) ethers, polyoxyethylene polyoxypropylene alkyl (or alkenyl) ethers and fatty acid methyl esters having a melting point of 40 ° C. or less and an HLB of 9 to 16 are used. Particularly preferred are fatty acid methyl ester ethoxylates to which ethylene oxide is added, fatty acid methyl ester ethoxypropoxylates to which ethylene oxide and propylene oxide are added to fatty acid methyl esters, and the like. Further, these nonionic surfactants may be used as a mixture.

In the step (A), (d1)
Fatty acid soap and / or (d2) polyoxyalkylene glycol in a mass ratio [(d1) component + (d2) component]
/ [(A) component + (b) component + (d1) component + (d2)
Ingredients] = 0.001-0.25, preferably 0.005
-0.2, more preferably 0.01-0. From the viewpoint of suppressing the separation of the concentrate, it is preferable to add it so as to satisfy the condition of 15.

The fatty acid soap as the component (d1) includes
The carbon number of the alkyl group is 10 to 18, preferably 12 to
Preference is given to the alkali metal or alkaline earth metal salts of the 18 saturated or unsaturated fatty acids. Examples of such fatty acids include oleic acid, palmitic acid, lauric acid, and mixtures thereof. As the alkali metal, sodium, potassium and the like are preferable. Further, as the alkaline earth metal, magnesium, calcium, strontium and the like are preferable.

As the polyoxyalkylene glycol as the component (d2), for example, polyoxyalkylene glycol having a molecular weight of 150,000 or less is suitable. Molecular weight is 15
If it exceeds 10,000, the viscosity of the concentrate may increase. Examples thereof include polyethylene glycol and polypropylene glycol.

<Concentration step of (B)> In the concentration step of (B), the mixed slurry obtained in the step (A) is introduced into a thin film evaporator, and the concentrate has a mass ratio of 0.05 ≦ (c )water/
[(A) component + (b) component + (c) component] ≤ 0.2, and (b) component / [(a) component + (b) component + (c) component] = 0.15 to 0. This is a step of concentrating so as to satisfy the condition of 28.

0.05 ≦ (c) water / [(a) component +
(Component (b) + Component (c)] ≦ 0.2, preferably 0.
06 ≦ (c) water / [(a) component + (b) component + (c) component] ≦ 0.19, more preferably 0.07 ≦ (c) water /
[(A) component + (b) component + (c) component] ≦ 0.18. If it is less than 0.05, the viscosity becomes high, which is not preferable from the viewpoint of handleability. On the other hand, if it exceeds 0.2,
In the granulating step (C), adhesion to the granulator increases, which is not preferable.

Component (b) / [component (a) + component (b) + component (c)] is 0.15 to 0.28, preferably 0.15 to 0.24, more preferably 0.15. ~ 0.2
Is. If it is less than 0.15, the viscosity becomes high, which is not preferable from the viewpoint of handleability. On the other hand, when it exceeds 0.28, the separation stability of the concentrate is not good.

The concentrator used in the concentrating step (B) is not particularly limited, but a thin film type concentrator is preferably used. The thin-film evaporator is not particularly limited, but as a vacuum thin-film evaporator for efficiently evaporating water while suppressing thermal deterioration of the surfactant, for example, Exeva (Shinko Pantec Co., Ltd.), evaporator ( Sakura Mfg. Co., Ltd., control dryer (manufactured by Hitachi Ltd.) and the like are used.

The concentration conditions are as follows. Moisture evaporation rate slurry is 8 to 58 kg / m ² · hr, preferably 9 to
Evaporate at a moisture evaporation rate of 28 kg / m ² · hr. 8
If it is less than kg / m ² · hr, the evaporation capacity is insufficient, the concentration operation is inefficient, and it is not suitable for concentration of decomposable substances. On the other hand, when it exceeds 58 kg / m ² · hr, uneven concentration (partial overconcentration) occurs, which is not preferable. Temperature 40-140 ° C, preferably 60-130 ° C. If the temperature is below 40 ° C, the evaporation rate is low
The degree of vacuum, which may cause deterioration of quality due to deterioration of sulfates, is 0.004 to 0.067 MPa, and preferably 0.006 to 0.060 MPa. <(C) Granulating Step> The (C) granulating step is a step of granulating the concentrate in the (B) step. As the granulating step (C), there are generally a method of pulverizing the obtained concentrated product after cooling, a method of pulverizing after kneading, a method of stirring granulation and the like.

The apparatus and method for cooling after the concentration include an air cooling method, a belt-type vacuum cooler (Belmax; manufactured by Okawara Seisakusho, a steel belt-type cooler; manufactured by Sandvik Company, etc.), a drum-type cooler ( Drum flaker; manufactured by Kusunoki Machinery Co., Ltd., double drum dryer; manufactured by Kansone Co., Ltd.) and the like can be used. At this time, when the cooled product is obtained in the form of flakes, it is also possible to make the target anionic surfactant-containing powder in the state of flakes. After cooling, it can be directly pulverized, pelletized by a pelletizer and pulverized, or flakes can be pulverized into a powder.
By adding 1 to 30 parts by mass of the inorganic particles to 100 parts by mass of the surfactant when pelletizing, pellet molding is facilitated and the fluidity of the powdered product is improved.

As the inorganic particles, sodium sulfate,
A material selected from the group consisting of sodium carbonate, sodium hydrogen carbonate, zeolite, fine particle silica and calcium silicate is preferable.

Examples of the type of crusher used include Fitzmill (manufactured by Hosokawa Micron Corporation) and speed mill (manufactured by Okada Seiko Co., Ltd.). At this time, it is possible to more efficiently grind by using a grinding aid.

As the kind of the grinding aid, the average particle size is 2
Inorganic particles of 0 μm or less are preferable, zeolite, sodium carbonate, white carbon, etc. are used, and the addition amount of the auxiliary is preferably 1 to 20 parts by mass, and 2 to 10 parts by mass or less with respect to 100 parts by mass of the concentrate. More preferable.

It is also possible to mix inorganic particles having an average particle size of 20 μm or less for coating after flake or pulverization, and to coat them. Zeolite, sodium carbonate, white carbon, etc. are used, and the coating amount is 1 to 20 parts by mass is preferable with respect to 100 parts by mass of the concentrated product, and 1 to 5 parts by mass is more preferable. The surfactant powder obtained by the present invention is mixed / granulated or powder-mixed with a detergent composition prepared by another method such as conventional method using spray drying or stirring granulation, or a granular detergent composition. Can be

The method of crushing after kneading is a step of kneading (kneading) a detergent raw material and spray-dried particles to prepare a solid detergent. Concentrated products, spray-dried particles, and other detergent raw materials are introduced into a kneading (kneading) device, and are gradually mixed with transportation, consolidation, and kneading (kneading) while applying shearing force to form a solid detergent. To do.

As the kneading (kneading) device, various devices can be used. Specifically, a closed type consolidation apparatus, and more preferably a horizontal continuous kneader can be preferably mentioned. In addition to the kneader, a single or twin screw extruder can be used. These devices may be either batch type or continuous type.

When using the above-mentioned continuous kneading (kneading) apparatus, the arrangement of the paddles involved in kneading (kneading) is particularly important in terms of the quality of the resulting detergent. JP 2000-1
As described in Japanese Patent No. 44194, when a kneading (kneading) machine having a stirring blade is continuously fed with a detergent component, a kneading (kneading) is carried out when a kneaded (kneaded) product of the detergent component is produced. It has the respective functions of (i) a function of transporting a detergent component from a supply port of a kneading machine to a discharge port in the machine, (ii) a function of consolidating the detergent component, and (iii) a function of kneading the detergent component. Stirring blades are sequentially arranged from the supply port of the kneading (kneading) machine toward the discharge port side to continuously knead (knead). In addition, in order to prevent abrasion after long-time operation, it is desirable to subject the screw, paddle, and body (casing) to treatment such as stellite or tungsten carbide.

The following is used as a continuous kneading device. Example 1: KRC Kneader [Kurimoto Steel Co., Ltd.] Example 2: Extruded Omics [Hosokawa Micron Co., Ltd.] Example 3: Fine Luther [Fuji Paudal Co., Ltd.] Example 4: Continuous Kneader [manufactured by Dalton Co., Ltd.] Example 5: JP-A-63-242334 and JP-A-6-2
No. 3251, No. 6-23252, No. 7-26
Device Example 6 described in Japanese Patent No. 5679: Twin Dome Gran [manufactured by Fuji Paudal Co., Ltd.] Example 7: Dome Gran [manufactured by Fuji Paudal Co., Ltd.]

The following are used as a batch type kneading (kneading) device. Example 1: Kneader [Dalton Co., Ltd.] Example 2: Universal mixing stirrer [Dalton Co., Ltd.]

The kneading (kneading) conditions are as shown below. It is suitable to operate at a temperature of generally 30 to 80 ° C, preferably 35 to 75 ° C, more preferably 40 to 70 ° C. If the temperature is lower than 30 ° C., the load on the kneading (kneading) device tends to be excessive, which is not preferable. On the other hand, the temperature is 8
If the temperature is higher than 0 ° C., on the contrary, the kneaded (kneaded) product tends to adhere to a device used in a subsequent step such as a crusher, which is not preferable.

Treatment time In the case of the batch type, the treatment time is usually 1 to 20 minutes, preferably 2 to 15 minutes, more preferably 3 to 10 minutes. The treatment time in the case of the continuous system is usually 10 to 120 seconds, preferably 20 to 90 seconds, more preferably 30 to 60 seconds.

Pressure As disclosed in Japanese Patent Application Laid-Open No. 61-118500, the kneader is controlled to an internal pressure of 0.01 to 5 kg / cm ² · G to continuously knead (knead).

As the binder at the time of kneading (kneading), generally, water,
Anionic surfactant aqueous solutions, nonionic surfactants, nonionic surfactant aqueous solutions, and mixtures thereof are used. Among these, nonionic surfactants, nonionic surfactant aqueous solutions, anionic surfactants and nonionic surfactants are used. A mixed aqueous solution of is preferable.

In order to suppress the temperature rise of the detergent solids due to cooling kneading (kneading), it is desirable to carry out kneading (kneading) while passing the refrigerant through the jacket of the kneading (kneading) device. As the refrigerant, an aqueous solution of ethylene glycol is suitable and its concentration is 1
5 to 30%, preferably 20 to 25% is used.

The physical properties of the kneading (kneading) are as shown below. Bulk density Generally 0.5-1.2 g / mL, preferably 0.6-
It is 1.0 g / mL. The size is generally 10 to 500 mm, but is not particularly limited as long as it is smaller than the pitch of the screw of the extruder for introducing the kneaded (kneaded) product.

The crushing step (C) is a step of crushing a mixture, kneaded material, pellets or granulated product of a detergent with a crushing granulator to prepare a desired particle size. In this case, as a particularly preferable crushing method, a detergent solid consisting of a surfactant and a builder (mixture, kneaded material, pellet or granulated material) is crushed and granulated, and a crusher of a cutter mill type having a classification screen is used. It is particularly preferable that a crusher having a large screen hole diameter is sequentially supplied to a crusher having a small screen diameter to perform multistage crushing.

As the crushing granulator, the following can be used. Granulator Generally, a crushing granulator equipped with a rotating body and a screen inside, preferably an impact crusher such as a hammer mill, atomizer or palpelizer, a cutting / shear crusher such as a cutter mill or a feather mill. Used. Example 1: Fitzmill [manufactured by Hosokawa Micron Co., Ltd.] Example 2: Speed mill [manufactured by Okada Seiko Co., Ltd.] Example 3: Crushing granulator Power Mill [Fuji Paudal Co., Ltd.]
Example 4: Atomizer [Fuji Paudal Co., Ltd.] Example 5: Pulverizer [Hosokawa Micron Co., Ltd.] Example 6: Comminator [Fuji Paudal Co., Ltd.] Although it does not matter, there is a rotary crushing blade in the crushing chamber, crushed by the rotary crushing blade,
The thing which discharges the crushed detergent granules from the screen of a predetermined hole diameter etc. is used suitably.

Screen The screen is not particularly limited to a wire mesh type, a herringbone type, a punching metal type, etc. However, considering the screen strength and the shape of the crushed material, punching metal is preferable.

A rotary hammer or a cutter is used, but a cutter type is preferable in order to avoid generation of fine powder due to impact crushing. However,
Treatment with stellite, tungsten carbide, etc. is desirable to prevent the blade of the cutter from becoming worn during long-term operation.

The crushing conditions are shown below. Peripheral speed of the rotating body Generally, it is set according to the pulverizability of the object to be pulverized (crushed material) and the desired particle size. Usually, in the case of detergent, it can be used in the range of 10 to 70 m / s. When the crushed material is brittle or has strong adhesion, crushing at 50 m / s or less is preferable, and 40 m
/ S or less is more preferable. On the contrary, when viscoelasticity is strong and adhesion is weak, pulverization at 50 m / s or more is preferable from the viewpoint of productivity and particle size control.

Introduction of Cold Air In general, it is desirable to introduce cold air into the crusher in order to prevent the crushed material from being softened by the crushing heat and attached to the crusher. The cold air temperature is suitably 5 to 30 ° C, preferably 10 to 25 ° C. In addition, the amount of cold air is 0.1
5 m ³ / kg (crushed material) is suitable. If the amount of cold air is too large, the temperature of the crushed product is remarkably lowered, and the crushed product becomes hard and brittle, resulting in over-pulverization and increase in fine powder and deterioration in shape. As a method of introducing the cold air, either a batch introduction of a necessary amount into the first stage or a divided introduction into each stage may be adopted. In addition, it is economically advantageous to recycle the cold air discharged from the crusher after separating it from the powder.

Upon crushing the crushing aid, it is preferable to add a crushing aid.
Grinding aids are generally grinding aids.
It is known as d), and when added in a small amount to the crusher, it has the effects of reducing the crushing power, improving the crushing particle size, and improving the properties of the crushed product. Particle size of crushing aid is 50
The thickness is preferably not more than μm, more preferably not more than 20 μm. Further, the amount of the crushing aid added is 0.5 to the crushing amount.
10% by mass is preferred. Examples of the crushing aid include stearates, aluminosilicates such as A-type zeolite, calcium carbonate, magnesium carbonate, alkaline earth metal carbonates, amorphous silica, calcium silicate, magnesium silicate, and other silica. Clay minerals such as acid salts, talc and bentonite, silicon dioxide, titanium dioxide, finely powdered sodium carbonate and sodium sulfate are preferable. By adhering these crushing aids to the surface of the crushed material and lowering the surface activity of the crushed material, it is possible to prevent adhesion to the crusher, reduce the crushing power associated therewith, and improve the fluidity of the crushed material. As a method of adding an auxiliary, a method of mixing before crushing in advance,
There are a method of adding all the necessary amount in a batch to the first stage of multistage crushing, and a method of dividing and adding each stage. Any of them may be selected, but it is preferable to add them all at once from the viewpoint of the effect of the auxiliary agent and the economical efficiency. Further, by forming a system in which the crushers are directly connected to each other and each stage is hermetically closed (closed direct connection type), the loss of the auxiliary agent is reduced, and a small amount of the auxiliary agent added can effectively act.

Milling Material Temperature The milling material temperature is generally 5 to 50 ° C., preferably 10 to 40.
It is suitable to carry out at 0 ° C, more preferably 10 to 30 ° C. The temperature and flow rate of the cold air are set so as to fall within this temperature range. When the temperature is lower than 5 ° C, dew condensation is likely to occur, which is not preferable. On the other hand, when the temperature is higher than 50 ° C., on the contrary, the adhesion to the crusher easily occurs, which is not preferable.

Processing time Usually, it is 1 to 30 seconds, preferably 3 to 30 seconds.

Screen Pore Diameter Generally, it is set according to the pulverizability of the material to be crushed (crushed material) and the desired particle diameter. Generally, in the case of detergent, a screen having a pore size of 3.0 to 30.0 times, preferably 4.0 to 25.0 times the desired average particle size can be used. Average particle size 500μm
In order to obtain the detergent particles, the screen having a hole diameter of 1.5 to 15 mm may be selected and used according to the size of the crushed material.

Multi-stage crushing It is preferable that the crushing ability of the high-bulk density detergent in multi-stage crushing is large and common to all stages because the crushers are connected in series. In order to realize this, it was found that there is an optimum value for the ratio of the average particle size of the crusher inlet and outlet obtained by selecting the screen hole diameter. When the average particle size at the start of the crushing process and the desired average particle size of the crushed granulated product are set, the number of crushing stages is naturally determined accordingly. At that time, it is more effective if the relationship between the screen hole diameter and the average particle diameter of the obtained crushed material can be predicted in advance. Further, when the particle size is large, the surface area of the powder is small and the load applied to the crusher is small, so that the ratio of the average particle size at the inlet-outlet can be widened. Therefore, in multistage crushing, it is desirable to reduce the crushed particle size as much as possible with the upper crusher. For multi-stage crushing, it is possible to install a sieve at the outlet of the crusher for each stage and supply only the desired level of crushed material to the crusher of the next stage, but clogging of the sieve, complication of the system, installation It is disadvantageous in terms of area increase. So 1
A direct connection type in which the discharged material (crushed material) from the crusher in the second stage is directly supplied to the crusher in the second stage (further, the third and subsequent stages) is preferable.

Regarding the property of the crushed product, the average particle size of the crushed granulated product is preferably 300 to 1500 μm, more preferably 500 to 1000 μm. If the average particle size is large, the solubility in laundry will be delayed, and problems such as cloth adhesion and detergency may occur.On the other hand, if the average particle size is small, the amount of dust generated due to an increase in fines and the crushing yield will increase. May lead to deterioration of liquidity and deterioration of liquidity.

The agitation granulating device in the agitation granulation is as follows:
It is important that the structure has a stirring shaft equipped with a stirring blade in the center thereof and forms a clearance between the stirring blade and the vessel wall when the stirring blade rotates. The average clearance is preferably 1 to 30 mm. Examples of the stirring type mixer having such a structure include Henschel mixer [manufactured by Mitsui Miike Kakoki Co., Ltd.], high speed mixer [manufactured by Fukae Industry Co., Ltd.], vertical granulator [Co., Ltd.].
Manufactured by Paulec, etc., and particularly preferably a horizontal mixing tank having a stirring shaft at the center of the cylinder, and a stirring blade is attached to this shaft to mix powders. A mixer [manufactured by Matsubo Co., Ltd.] and a broche mixer [manufactured by Taiheiyo Kiko Co., Ltd.].

The average clearance is preferably 1
-30 mm, more preferably 3-10 mm. 1m
If it is less than m, the mixer tends to be overpowered due to the adhesion layer.
On the other hand, if it exceeds 30 mm, the compaction efficiency decreases, and the particle size distribution becomes broad, and the granulation time becomes long and the productivity may decrease.

The granulation conditions are as shown below. Froude number (Fr number) The Froude number (Fr) defined by the following formula (1) is 1 to
It is preferably 4 and more preferably 1.2 to 3. If the Froude number is less than 1, consolidation is not promoted, which is not preferable. On the other hand, when it exceeds 4, the particle size distribution becomes wide, which is not preferable.

<Formula 1> Fr = V / (R × g) ^0.5 V: peripheral speed [m / s] of tip of stirring blade R: radius of rotation of stirring blade [m] g: acceleration of gravity [m / s ² ]

Granulation time The granulation time in batch granulation and the average residence time in continuous granulation to obtain a suitable granulation product is 0.5.
It is preferably -20 minutes, more preferably 3-10 minutes. If it is less than 0.5 minutes, the granulation time is too short and it is difficult to control the granulation to obtain a suitable average particle size and bulk density.
The particle size distribution may be broad. On the other hand, if it exceeds 20 minutes, the granulation time may be too long and the productivity may be reduced.

Filling Rate of Detergent Raw Material The filling rate (feeding amount) of the detergent raw material into the granulator is preferably 70% by volume or less, more preferably 15 to 40% by volume of the total internal volume of the mixer. If it exceeds 70% by volume, the mixing efficiency of the detergent raw material in the mixer is lowered, so that suitable granulation may not be performed in some cases.

The temperature granulator preferably has a structure having a jacket, and the temperature of the medium passed through the jacket is preferably 5 to 40 ° C.
More preferably, it is 10 to 20 ° C. Within this temperature range, the granulation time for obtaining a suitable granulated product is shortened, the productivity is improved, and the particle size distribution is sharpened. Further, among the detergent raw materials, the powder raw material may be supplied at room temperature and the nonionic activator may be supplied at a melting temperature, and it is not necessary to control the temperature in the mixer. The temperature of the granulated product is usually 30 to 60 ° C depending on the temperature of the feed material, the heat of stirring, and the like.

Additives In order to accelerate the granulation during granulation, a binder may be added. Examples of the binder, carboxymethyl cellulose, polyethylene glycol, water-soluble polymer solution such as polycarboxylic acid salts such as sodium polyacrylate,
Examples thereof include nonionic substances such as polyoxyethylene alkyl ether, fatty acid monoethanolamide and fatty acid diethanolamide, fatty acid, aqueous sodium silicate solution and water. The binder content is preferably 0.1 to 10 parts by mass with respect to 100 parts by mass of the mixture or granulated product,
It is particularly preferably 0.5 to 5 parts by mass.

[0063]

EXAMPLES The present invention will be specifically described below by showing Examples and Comparative Examples, but the present invention is not limited to the following Examples.

The raw materials used in this example are shown below together with their abbreviations. “Α-SF”: C obtained by the following production method
Sodium alphasulfofatty acid having a _14-16 alkyl chain (Purity 65.6% and others, 3.28% methyl sulfate, 1.31% sodium sulfate, 3.08% sodium salt of alphasulfofatty acid, methanol 1.
51%, unreacted methyl ester 1.21%, water 24.0
1%), provided that 7% of this sodium alphasulfofatty acid is converted into a di-salt of sodium alphasulfofatty acid in the manufacturing process of the detergent composition, and further 25% is equivalent to it in the long-term storage of the detergent composition. There is. (Manufacturing method) Thin film reactor (single tube, inner diameter = 10 m
m, reactor length = 2.5 m) as a raw material compound methyl myristate (manufactured by Lion Corporation, Pastel M-
14) and methyl palmitate (Lion Co., Ltd., Pastel M-16) were mixed at a mass ratio of 2: 8, and a fatty acid methyl ester (iodine value 0.40, molecular weight 264) was used.
Liquid SO ₃ was used as the SO ₃ gas system equipment, nitrogen gas was used as the dilution gas, and an inert gas containing 8% SO ₃ was used, and the gas absorption reaction was performed at a reaction molar ratio (SO ₃ / methyl ester) = 1.2. Perform in a thin film reactor, and after gas-liquid separation,
An aging reaction was performed at 0 ° C. for 60 minutes to obtain a sulfonic acid having a reaction rate of 97%. Then 20% by weight of methanol to sulfonic acid,
35% hydrogen peroxide water (2% as hydrogen peroxide pure content against sulfonic acid) was added, and after uniform mixing, a bleaching reaction was carried out at 80 ° C. for 180 minutes. Then, a neutralization reaction is performed with an aqueous sodium hydroxide solution to obtain a neutralized product having a concentration of 47% (surfactant concentration), and methanol (recycled by rectification in the subsequent step) by recycle flash concentration and water evaporated to 65.6. A concentrated neutralized product having a concentration of 10% (surfactant concentration) was obtained. Color tone (5% by mass ethanol solution 40 mm optical path length, measured with a Klett photoelectric photometer using No. 42 blue filter) is 30.
Met.

[0065] "soap": 1 sodium palmitate and sodium oleate and TMD _(ester compounds of _C 10 _{~ 20):} 3: 1 mixture of (mass ratio). 40-60
C. fatty acid methyl ester (pastel MC * O, manufactured by Lion Oreo Chemical Co., Ltd.) 1576 kg / h, 40
48% NaOH aqueous solution at -60 ° C 445 kg / h and water (Lion Chiba factory middle water) 336 kg / h were continuously introduced into the mixing pump, and a shell & tube type heat exchanger,
And while maintaining at 110-130 ℃ with a preheater, 9-10
The saponification reaction was allowed to proceed for a minute (reaction rate 99.5 to 99.8).
%). Then, the mixture was introduced into a flash evaporator having a column top pressure of 0.2 to 0.6 kPa and a column top temperature of 98 to 100 ° C., and methanol as a reaction product was evaporated at a residence time of 40 minutes. Finally, the soap from which the methanol has been removed is introduced into a stirring tank having a paddle type stirring blade, and 80 ° C warm water is added while maintaining the temperature at 98 ° C while stirring with a residence time of 140 minutes, so that the soap concentration becomes 66 to 67%. The density was adjusted as follows. The soap thus obtained has an AI of 66-67%, and as impurities, about 0.01% fatty acid, about 0.2% unreacted fatty acid ester, about 0.2% NaOH, about 0.4%. %
Including methanol.

"AAO": CH ₃ (CH ₂ ) _11-12 O
(CH ₂ CH ₂ O) ₁₅ H (manufactured by Lion Chemical Co., Ltd.) 40 diadol 13 (manufactured by Mitsubishi Chemical Co., Ltd.) in a 4-liter autoclave (manufactured by Pressure Resistant Glass Industry Co., Ltd.)
0 g and 2.3 g of a 30% NaOH aqueous solution were charged, the inside of the autoclave was replaced with nitrogen, and the temperature was raised with stirring (in the middle, dehydration was performed at a temperature of 100 ° C. for 30 minutes). Then, while maintaining the temperature at 180 ° C. and the pressure at 300 kPa, ethylene oxide (EO: manufactured by Mitsubishi Chemical Corporation) 1320
g (average number of added moles: 15) was introduced, and Diadol 1
The reaction between 3 and EO was performed. Finally, it was aged for 30 minutes to obtain a nonionic surfactant. Impurities in the nonionic surfactant were about 2.0% PEG and about 0.7% unreacted alcohol.

"MEE (C ₁₂ EO ₉ )": CH ₃ (C
_{H 2) 10 CO (OCH 2} CH 2) 9 OCH 3 ( Lion Chemical Co., Ltd.) _"MEE (C 12 _{EO 12)": CH 3 (CH 2) 10} C
_{O (OCH 2 CH 2) 1} 2 OCH 3 ( manufactured by Lion Chemical Co.) _"MEE (C 12 _{EO 15)": CH 3 (CH 2) 10} C
_{O (OCH 2 CH 2) 1} 5 OCH 3 ( manufactured by Lion Chemical Co.) "MEE _(C 16 EO _{9)": CH 3 (CH 2) 14} CO
(OCH ₂ CH ₂ ) ₉ OCH ₃ (Lion Chemical Co., Ltd.
"MEE (C ₁₆ EO ₁₂ )": CH ₃ (CH ₂ ) ₁₄ C
_{O (OCH 2 CH 2) 1} 2 OCH 3 ( manufactured by Lion Chemical Co.) _"MEE (C 16 _{EO 15)": CH 3 (CH 2) 14} C
_{O (OCH 2 CH 2) 1} 5 OCH 3 ( manufactured by Lion Chemical Co.) _{"MEE (C 180/181 = 10} /90 EO 9) ":
(CH ₃ (CH ₂ ) ₁₆ CO / C ₁₇ H ₃₃ CO = 10/9
0) (OCH ₂ CH ₂ ) ₉ OCH ₃ (manufactured by Lion Chemical Co., Ltd.) “MEE (C 180/181 _{= 10/90} E
O _{12) ":( CH 3 (CH 2) 16} CO / C 17 H 33 CO
= 10/90) (OCH ₂ CH ₂ ) ₁₂ OCH ₃ (manufactured by Lion Chemical Co., Ltd.) “MEE (C 180/181 _{= 10/90} E
O _{15) ":( CH 3 (CH 2) 16} CO / C 17 H 33 CO
= 10/90) (OCH ₂ CH ₂ ) ₁₅ OCH ₃ (manufactured by Lion Chemical Co., Ltd.)

The "MEE" was manufactured as follows. Description will be made by taking C ₁₂ EO ₉ as an example. (Production method) 400 g of Pastel M-12 (manufactured by Lion Oreo Chemical Co., Ltd.) and a catalyst (composite hydroxide of magnesium / aluminum / manganese in nitrogen) were placed in a 4-liter autoclave (manufactured by Pressure Resistant Glass Co., Ltd.). 1.2 g of 40% KOH aqueous solution, which was aged in the atmosphere at 800 ° C. for 3 hours to form a composite oxide of Mg / Al / Mn)
2 g was charged, the inside of the autoclave was replaced with nitrogen, and the temperature was raised with stirring (in the middle, dehydration was performed at a temperature of 100 ° C. for 30 minutes). Next, the temperature is 180 ° C and the pressure is 300 kPa.
While maintaining the above, 696 g (average added mole number: 15) of ethylene oxide (EO: manufactured by Mitsubishi Chemical Co., Ltd.) was introduced, and the reaction between Pastel M-12 and EO was performed. Finally, it was aged for 30 minutes to obtain a nonionic surfactant. Impurities in the nonionic surfactant were about 2.0% PEG and about 1.0% unreacted methyl ester. Other MEEs are produced in the same manner by changing the raw material (pastel) used and the ethylene oxide introduced. It is summarized in Table 1 below.

[0069]

[Table 1] (* 1) Pastel M-12, Pastel M-16, Pastel M-181 are all manufactured by Lion Oreo Chemical Co., Ltd.
All were reacted at 400 g.

"AAEP15030": CH ₃ (CH ₂ )
_11-12 O (CH ₂ CH ₂ O) ₁₅ (CH ₂ CH ₂ CH
₂ O) ₃ H (manufactured by Lion Chemical Co., Ltd.) 40 diadol 13 (manufactured by Mitsubishi Chemical Co., Ltd.) in a 4-liter autoclave (manufactured by Pressure Resistant Glass Industry Co., Ltd.)
0 g and 2.3 g of 30% NaOH aqueous solution were charged, the inside of the autoclave was replaced with nitrogen, and the temperature was raised with stirring (in the middle, dehydration was performed at 100 ° C. for 30 minutes). Next, ethylene oxide (EO: manufactured by Mitsubishi Chemical Corporation) 132 while maintaining the temperature at 180 ° C. and the pressure at 3 atm.
0 g (average number of moles added: 15) was introduced, the reaction between Diadol 13 and EO was performed, and the mixture was aged for 30 minutes. After that, the reaction liquid is cooled to a temperature of 120 ° C. and the temperature is 120 ° C.
While maintaining 0 kPa, propylene oxide (PO:
Asahi Glass Co., Ltd. product (350 g) (average added mole number: 3) was introduced and the reaction was carried out. Finally, it was aged for 30 minutes to obtain a nonionic surfactant. Impurity in the nonionic surfactant is P
EG was about 2.0% and unreacted alcohol was about 0.7%.

"PEG # 400": average molecular weight is 400
Polyethylene glycol (Lion Chemical Co., Ltd.)
"PEG # 1500": polyethylene glycol having an average molecular weight of 1500 (manufactured by Lion Chemicals Co., Ltd.) "Sannix diol PP-400": polypropylene glycol having an average molecular weight of 400 (manufactured by Sanyo Kasei Co., Ltd.) "EPAN 485": average molecular weight of 400, the content of ethylene oxide is 85% polyoxyethylene polyoxypropylene block polymer (manufactured by Dai-ichi Kogyo Seiyaku Co.) _"LAS": a C 10 _{-C 14} Linear sodium alkylbenzene sulfonate, Ripon LH-200 (manufactured by Lion Corporation)

"AOS-K": C14: 16: 18 = 15: 50: 35 obtained by the following production method.
A mixture of potassium α-olefin sulfonate and potassium hydroxyalkyl sulfonate (purity 70%, the ratio of potassium α-olefin sulfonate: potassium hydroxyalkyl sulfonate is 7: 3, the balance is unreacted α-olefin, sodium sulfate) , Sultone, sodium hydroxide, water, etc.) (Production method) α-olefin (dialen 14
8. Mitsubishi Chemical Co., Ltd., TO reactor (TO-500, Lion Co., Ltd.) with a capacity of 970 kg / hr continuously.
Manufactured, film-type reactor) and subjected to sulfonation reaction by contacting with SO ₃ gas inside to obtain a sulfonated product containing α-olefinsulfonic acid and impurities (mainly sultone) at about 35 ° C. It was This sulfonate 1370k
Caustic potash 630 kg / hr against g / hr (water content 52%
Aqueous solution) is added to carry out a neutralization reaction, and α-
Obtained potassium olefin sulfonate. In order to hydrolyze the sultone in the impurities, the temperature was heated to 140 ° C. through a shell-and-tube heat exchanger, and steam of 1.4 MPa was passed through the reaction coil to keep the temperature at 170 ° C. to accelerate the hydrolysis. After that, flash concentration and dehydration were performed at a pressure of 1 MPa to make the water content about 27%. The net content of AOS-K thus obtained is usually 66 to 74%.
The main component is potassium α-olefin sulfonate (about 7
0%) and potassium hydroxyalkyl sulfonate (about 3%)
0%), the color is (10% solution LK value) 70,
It is 1.8% of free alkali content (KOH) (vs. AOS-K pure content).

"Fine powder zeolite": 4A type zeolite,
Average particle size 3 μm (manufactured by Mizusawa Chemical Co., Ltd.) “Granular zeolite”: 4A type zeolite, average particle size 20
0 μm (manufactured by Cosmo, Korea) “Zeolite slurry”: 4A type zeolite aqueous solution, water content 47% (manufactured by Nippon Kagaku Co., Ltd.) “Potassium carbonate”: Food additive grade (manufactured by Asahi Glass Co., Ltd.) “Sodium sulfite”: Anhydrous sulfite Soda (manufactured by Shinshu Chemical Co., Ltd.) "Sodium carbonate": Granulated ash (manufactured by Asahi Glass Co., Ltd.) "MA agent": Aqualic TL-400 (manufactured by Nippon Shokubai Co., Ltd.) "CBS": Chinopearl CBS-X ( Ciba Specialty Chemicals) "AMS": AMS-GX (Ciba Specialty Chemicals)

Examples 1 to 52 and Comparative Examples 1 to 3 <Concentration Step> (a) Aqueous Slurries Containing (a) α-Sulfo Fatty Acid Ester Salts of Compositions shown in Tables 2 to 10 and (b) Nonionic Surfactant Agent, (d1) soap and / or (d2) polyoxyalkylene glycol at 70 ° C. static mixer (manufactured by Takumina Co., Ltd. N30 type (housing diameter:
1S, housing scale 5S, outer shape 25.4mm, total length 220mm, thickness 1.2mm)), and then this mixture with a capacity: 100kg / hr in a vacuum thin film evaporator (Exeba: Shinko Pantech, heat transfer area) 0.5m ² )
The inner wall heating temperature is 120 ° C and the degree of vacuum is 0.008-
The concentration operation was performed under the conditions of 0.067 MPa and a rotating blade peripheral speed of 11 m / s, and the viscosity and the separation were evaluated by the following methods. The results are shown in Tables 2-10.

The concentration operation can be performed at a capacity of 70 to 130 k.
g / hr, inner wall heating temperature: 60 to 130 ° C., rotary blade peripheral speed: 5 to 12 m / s are also possible.

<Viscosity Evaluation Method> A Brookfield type (B type) viscometer (manufactured by Tokyo Keiki Co., Ltd.) was used to measure the viscosity (Pa · s) at 10 ° C. 10 minutes after discharge from Exeva, The following criteria evaluated.

<Evaluation Criteria> A: Viscosity is 20 Pa · s or less (rotor No. 5, 20
(measured in rpm) and free flowing. ◯: Viscosity is 20 to 50 Pa · s (rotor No. 5, 2
It is measured at 0 rpm) and has fluidity, but depending on the conditions, problems may occur in pipe transfer and discharge from the tank. X: Viscosity exceeds 50 Pa · s (rotor No.
(Measurement is not possible at 5 or 20 rpm), there is no free flowing property, and problems occur in pipe transfer and discharge from the tank.

<Separation Evaluation Method> Measuring cylinder (100 m
Put 100mL sample in L volume, and put in a constant temperature bath (70 ℃, 6
The state of separation was measured from the movement of the interface position between α-SF and nonion in 0 RH%), and evaluated according to the following criteria.

<Evaluation Criteria> x: After 1 hour, when the interface position was pointing to any scale of 0 to 100 mL (that is, when there was separation) ◯: When there was no separation

[0080]

[Table 2]

[0081]

[Table 3]

[0082]

[Table 4]

[0083]

[Table 5]

[0084]

[Table 6]

[0085]

[Table 7]

[0086]

[Table 8]

[0087]

[Table 9]

[0088]

[Table 10]

From the results of Tables 2 to 10, Examples 1 to 52
And in Comparative Examples 1 to 3, PEG # 400 is PEG #
It was confirmed that even 1500, Sannix diol PP-400 and Epan 485 did not affect the transfer and separation. In Examples 1 to 52, "AA
“O” is C ₁₂ EO ₉ , C ₁₂ EO ₁₂ , C ₁₂ E
O ₁₅ , C ₁₆ EO ₉ , C ₁₆ EO ₁₂ , C ₁₆ EO
_{15, C 180/181 = 10} /90 EO 9, C
_{180/181 = 10/90} EO _12, C ₁₈
It was confirmed that even MEE of 0/181 _{= 10/90} EO ₁₅ did not affect the transfer and separation.

Next, the concentrated product obtained in Examples 1 and 18 was granulated with α-SF, 1 part of soap (the amount put in the concentrator), nonionic surfactant, 1 part of zeolite, enzyme,
A detergent slurry having a solid content of 60% and a temperature of 70 ° C. is prepared by using each component excluding colorant and fragrance, and a countercurrent spray drying tower (tower diameter: 2 m, effective length: 5 m) is used, and a pressure nozzle method is used. At a spray pressure of 0.3 MPa and a hot air temperature of 260 ° C. (hot air outlet temperature of 90 ° C.), the dried product was dried to a water content of 5%.

The spray-dried product obtained had an average particle size of 400.
μm, bulk density 0.35 g / mL, angle of repose 45 °, and good flowability. (In addition, ・ Solid content: 50-65%, dry product can be manufactured ・ Slurry temperature: 50-80 ℃, dry product can be manufactured ・ Hot air temperature: 200-300 ℃, dry product can be manufactured ・ Atomization method: 2 fluid nozzle Method, high-speed rotating disk method can be used for dry product production. ・ Spray pressure: 0.2-0.4 MPa can be used for dry product production. ・ Dry product water content: 2-10% for granulation. ・ Dry product average particle diameter: 150-500 μm. However, granulation is possible.-Bulk density: 0.10 to 0.50 g / mL is also possible.- Angle of repose: 30 to 60 is also possible.)

[Examples 53 to 56] A concentrated product, a spray-dried product, 1 part of a nonionic surfactant and water were introduced into a continuous kneader (KRC Kneader Model 4 manufactured by Kurimoto Iron Works Co., Ltd.) to give a dense and uniform kneaded product. Got Homogenization was performed under the conditions of a kneading capacity of 177 kg / hr and a kneading temperature of 60 ° C (rotation speed: 134 r
pm). The homogenized kneaded product is continuously supplied to a pelletizer double (EXD-100 type (manufactured by Fuji Paudal Co., Ltd.)) and extruded from a 10 mmφ die (die thickness 10 mm) and cut simultaneously (pelletter). (Cutter) Peripheral speed:
5m / s) Solid pellets (Pellet size: Diameter 10
mmφ, length 20 mm). At this time, the pressure applied to the pelletizing die was 0.93 MPa.

Then, the obtained pellet solid and a granulation aid of 8 kg / hr of zeolite granules (average particle size:
Fitzmill (DKA)
SO-6 type (manufactured by Hosokawa Micron Co., Ltd.)
Make the average particle diameter 500μm (rotary crushing blade peripheral speed:
30m / s, ratio of wind (ki) and pellet (solid) (ki / solid) =
2.5 m ³ / kg) was continuously pulverized in 3 stages (1st stage screen diameter 6 mmφ, rotational speed 1880 rpm, 2nd stage screen diameter 4 mmφ, rotational speed 2350 rpm, 3rd stage screen diameter 2 mmφ, rotational speed 3760 mmφ) . At this time, the temperature of the gas phase was 16 ° C and the temperature of the powder was 25 to 35 ° C. Then, the obtained granules were mixed with 1% zeolite and 1% nonionic surfactant having the final composition in a rolling drum (a horizontal cylindrical rolling granulator (diameter: 60 cm, height: 48 cm), mixing and stirring time: 2 min (Froude number:
0.14) The operation was performed. The pulverizer adhesion rate and solubility were evaluated by the following methods. The results are shown in Table 11.

<Measurement of pulverizer attachment rate> After kneading and pulverization for 5 minutes, the amount attached to the pulverizer was measured, and the pulverizer attachment rate (%) calculated by substituting into the following mathematical formula = 100 × attachment amount / feed Amount <Evaluation Criteria> A: 0% ≤ adhesion rate ≤ 0.03% ◯: 0.03% ≤ adhesion rate <0.05% △: 0.05% ≤ adhesion rate <0.1% x: 0.1 % <Adhesion rate

<Measurement of Solubility> Prepare 30 liters of tap water at 10 ° C. in a tub-type washing machine (Mitsubishi Electric; CW-225), and use 2 navy blue cotton shirts, 2 black acrylic sweaters, and black nylon strip. A total of 1.5 kg (a bath ratio of 20 times) of 2 sheets and 5 skin shirts as a charge cloth was put in to form a hollow in the center of the cloth to be washed, and 30 g of detergent was intensively put therein. After allowing the detergent to soak in water for 2 minutes, it was washed with a weak water flow for 5 minutes. It was naturally drained and dehydrated for 1 minute, and the amount of detergent adhering to the cloth was visually evaluated according to the following criteria.

<Evaluation Criteria> 0 point: No adhesion at all 1 point: Very slight adhesion, but good results by rinsing Level 2 points: Partial slight adhesion is observed 3 points: Whole cloth Slight amount of adhesion and unsatisfactory level after rinsing 4 points: Adhesion to the entire cloth 5 points: Adhesion to the entire cloth violently

[0097]

[Table 11] Even if the concentrates used in Examples 53 and 54 are Examples 2 to 17 and 49, there is no influence on the pulverizer adhesion and solubility. In addition, even if the concentrates used in Examples 55 and 56 are Examples 18 to 48 and 50 to 52, they are attached to the crusher,
Solubility is not affected.

(In addition, kneading ability: 100 to 300 kg
/ Hr can be manufactured ・ Kneading temperature: Can be manufactured at 40 to 80 ° C ・ Rotation speed: Can be manufactured at 100 to 150 rpm ・ Die diameter: Can be manufactured at 0.3 to 50 mmφ ・ Die thickness: Can be manufactured at 5 to 50 mm・ Pellet size: Diameter 0.3-50mmφ, Length 0.5-
100mm ・ Pellettor-Peripheral speed: 1-10m / s can also be manufactured. ・ Pelletter die pressure: 0.5-1.5MPa.
Can be manufactured. ・ Pulverization aid: Can be manufactured with 20 to 200 μm. ・ Pulverization aid: Can be manufactured with 2 to 18 kg / hr. ・ Average particle size can be 300 to 1000 μm. ・ Pulverizing speed of rotary crushing blade is 20 to Manufacture is possible even at 60 m / s. Gas / solid = 1.0-5 m ³ / kg can be manufactured. Blower temperature: 10-40 ° C can be manufactured. Mixing and stirring time: 0.5-5 min. )

[Examples 57 to 58] The concentrates obtained in Examples 1 and 18 were used to granulate the compositions shown in Table 12. Sodium carbonate and zeolite are used by Ledige Mixer (Co., Ltd.)
It is put into Matsubo's M-20 type, and the spindle (200 rp)
m), and the mixture was uniformly mixed for 30 seconds under stirring with a chopper (6000 rpm) (prepared amount: 7 kg, 10 L). Next, the concentrated product was added in 1 minute and granulated for 2 minutes, and coating zeolite was added to obtain a granulated product having an average particle size of 500 μm. The temperature of the contents was 30 to 50 ° C.

[0100]

[Table 12]

(Granulating apparatus: Horizontal type Loedige mixer, vertical type high speed mixer, Henschel mixer, etc. can be used for granulation. Main shaft speed: 120 ~ 360 rpm for granulation (M
-20 type) ・ Chopper rotation speed: Granulation is possible even at 1000 to 6000 rpm (M-20 type) ・ Concentration product addition time: Granulation is possible at 0.5 to 4 minutes ・ Granulation time: 0 to 5 minutes ) Can be used for granulation. ・ Coating time: 0.5 to 5 minutes can be used. )

[0102]

According to the present invention, in the process of granulating a mixed slurry containing an α-sulfo fatty acid ester salt and a specific amount of a nonionic surfactant after concentrating with a thin film evaporator, the α-sulfo fatty acid is used. In concentrating the mixed slurry containing the ester salt, the viscosity of the concentrate is low, and a highly efficient method for producing a granular detergent composition having excellent operability without separation can be achieved.

─────────────────────────────────────────────────── ─── Continuation of front page (51) Int.Cl. ⁷ Identification code FI theme code (reference) C11D 1/72 C11D 1/72 3/37 3/37 10/02 10/02 17/06 17/06 ( 72) Inventor Hiromichi Horie 1-3-7 Main Office, Sumida-ku, Tokyo Within Lion Co., Ltd. (72) Inventor Akito Morita 1-3-3 Main Office, Sumida-ku, Tokyo F-term inside Lion Co., Ltd. (Reference) 4D076 AA02 AA24 BA17 CD22 FA02 FA04 FA23 FA24 HA15 4H003 AB03 AB15 AB19 AB21 AC08 BA09 CA14 CA20 DA01 EA12 EA16 EA28 EB30 EB36 EC02 ED02 FA09 FA16 FA30 FA32

Claims (2)

[Claims] 1. A method for producing a granular detergent composition, which comprises the following steps (A) to (C): (A) Step of mixing (a) an aqueous slurry containing an α-sulfofatty acid ester salt with (b) a nonionic surfactant (B) The mixed slurry obtained in the step (A) is introduced into a thin film evaporator. , The concentrate is in a mass ratio of 0.05 ≦ (c) water /
[(A) component + (b) component + (c) component] ≤ 0.2, and (b) component / [(a) component + (b) component + (c) component] = 0.15 to 0. 28) Concentrating so as to satisfy the condition of 28. (C) Granulating the concentrate in the (B) step. 2. In the step (A), (d1) fatty acid soap and / or (d2) polyoxyalkylene glycol are [(d1) component + (d2) component] / in mass ratio.
The method for producing a granular detergent composition according to claim 1, wherein the component (a) + (b) component + (d1) component + (d2) component is added so as to satisfy the condition of 0.001 to 0.25.