JPH09143500A - Production of granular detergent having high bulk density - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method for simply producing a gramular detergent excellent in solubility, appearance and resistance to hydrolysis and useful for cleaning clothes, capable of saving energy because spray-driving method is not used by directly kneading a specific surfactant-containing condensate with the other detergent component at a specific ratio and pulverizing the kneaded material. SOLUTION: (A) An α-sulfofatty acid alkylester salt-containing condensate having <=10wt.% water content [e.g. obtained by concentrating an aqueous solution containing α-sulfofatty acid alkylester salt such as a compound of the formula (R is an alkyl or an alkenyl; R<2> is a lower alkyl; Z is a group forming a salt such as sodium) to 10-19wt.% and concentrating the treated aqueous solution to <=10wt.% by a vacuum rotation thin film evaporator] in an amount of 10-40wt.% is directly kneaded with (B) 60-90wt.% other detergent component (e.g. nonionic surfactant) so that the total amount of the components A and B becomes 100wt.% and the kneaded material is pulverized.

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 high bulk density granular detergent which is excellent in solubility and appearance of powder and can suppress hydrolysis of α-sulfofatty acid alkyl ester salt.

[0002]

2. Description of the Related Art In recent years, laundry detergents have been shifted to the use of high bulk density detergent compositions which can be washed with a small amount of detergent and are excellent in transportability, storability and displayability. There is. Further, among the surfactants, α-sulfo fatty acid ester salt (hereinafter, sometimes abbreviated as α-SF) is known as a surfactant derived from a natural raw material and having excellent cleaning ability, particularly hard water resistance. A high bulk density detergent composition containing the same is disclosed in JP-A-62-199695, JP-A-64-60695, JP-A-64-60696, and JP-A-3-35098. JP-A-6-609
No. 7, etc.

Various methods are known as methods for producing a high bulk density detergent composition, for example, JP-A-61-69.
No. 900 and No. 61-69899 propose that the spray-dried particles of detergent are granulated or compacted in a horizontal mixer and then pulverized. However, this manufacturing method includes a step of spray-drying a surfactant-rich slurry and cannot be said to be energy-saving. In addition, Japanese Unexamined Patent Publication No.
No. 81500 discloses a surfactant of at least 50%.
A production method has been reported in which a dough is formed from a surfactant paste containing the above concentrations, and the dough is cooled and then granulated to obtain a high bulk density detergent. However, in this method, since the dough is cooled, the process becomes complicated and the productivity is not sufficient.

Further, Japanese Unexamined Patent Publication No. 6-128596 discloses a production method in which a surfactant and an alkali builder are mixed to obtain a powder compound, and then zeolite and the like are stirred and granulated together. This manufacturing method requires two granulation steps, which complicates the steps. Also, as described above, α
Although -SF is an excellent surfactant, it has a problem that it is easily hydrolyzed during storage after the production of a detergent, which reduces the amount of active ingredient.

[0005] α-SF has been widely used as an active agent having a relatively low concentration and a high detergency in a granular detergent for clothes having a high bulk density. Then, as the granular detergent is further downsized, the content of the detergent in the detergent tends to be increased in order to maximize the use of the characteristics of α-SF. However, when a detergent slurry containing a large amount of α-SF is dried by the conventional spray drying method, the adhesion of α-SF causes strong agglomeration in the tower, which greatly reduces the drying efficiency and makes production difficult. Become. Further, regarding the heat treatment method of α-SF, there are the following conventional techniques, but they are not sufficient because they each have drawbacks.

(1) JP-A-51-416675:
The aqueous surfactant solution is heated in the range of boiling point to 200 ° C., flash-introduced into a thin film evaporator, and concentrated. Although this method substantially includes the preconcentration of the present invention, no clear water content after preconcentration is defined. (2) JP-A-5-331496: Solid content concentration 60
An aqueous slurry of -80% anionic surfactant is dried with a thin film evaporator and scraped to form granules. Since the water content is 20% or more when introduced into the vacuum thin-film evaporator, a large drying capacity is required. (3) JP-B-8-16237: Moisture 20-35%
The paste raw material is dried in a vacuum thin film evaporator to obtain a dried flake. 20% moisture when introduced into vacuum thin film evaporator
As described above, a large drying capacity is required.

[0007]

DISCLOSURE OF THE INVENTION The present invention enables an energy-saving process in a detergent containing α-SF, and
It is an object of the present invention to provide a method for producing a high bulk density detergent composition which can improve the appearance of powder, prevent hydrolysis, and has excellent solubility.

[0008]

The method for producing a high-bulk density detergent composition of the present invention is such that (A) water content is 10% by weight or less when the detergent particles obtained by kneading and pulverizing are 100% by weight. [Alpha] -sulfofatty acid alkyl ester salt-containing concentrate of 10 to 40% by weight (B) Other detergent components: 60 to 90% by weight are directly kneaded and then pulverized to obtain detergent particles.

[0009]

BEST MODE FOR CARRYING OUT THE INVENTION In the present invention, (A) α-sulfofatty acid alkyl ester salt-containing concentrate and (B) other detergent components are directly kneaded and then pulverized to obtain high bulk density detergent particles. Therefore, the process is simplified. In addition, without directly manufacturing the spray-dried product, it can be directly applied to the kneader (A) α
-A sulfo fatty acid alkyl ester salt-containing concentrate and (B)
Since other detergent ingredients are added, the spray-drying process is unnecessary and energy saving can be realized.

In the present invention, the α-sulfofatty acid ester salt is typically represented by the following chemical formula 1.

Embedded image (R ¹ : alkyl group or alkenyl group R ² : lower alkyl group Z: salt-forming group such as sodium)

The α-sulfofatty acid ester salt can be prepared, for example, by the method described in JP-A-4-359098.
It can be obtained by sulfonation of α-sulfo fatty acid ester, aging and bleaching if necessary, and then neutralization. Fatty acid residue (R ¹ C
The carbon number of (HCOO) is preferably 8 to 22, and preferably 12 to 18. The lower alkyl group (R ² ) preferably has 1 to 6 carbon atoms, and preferably 1 to 3 carbon atoms. Then, in the present invention, the neutralized product is concentrated to obtain an α-sulfofatty acid alkyl ester salt-containing concentrate having a water content in the α-sulfofatty acid alkyl ester salt of 10% by weight or less, preferably 2 to 8% by weight. Add to the kneading process. If the water content exceeds 10% by weight, the powder whiteness and the solubility of the resulting detergent particles will decrease, and the α-sulfo fatty acid alkyl ester salt will be hydrolyzed due to the alkaline component that is kneaded together in the manufacturing process. Cause decomposition. Furthermore, the solubility is further improved by adding the nonionic surfactant to the α-sulfofatty acid alkyl ester salt-containing concentrate. Further, an anionic surfactant can be blended, and other components such as potassium carbonate and potassium sulfate can be added as necessary for improving dissolution and the like.

Specific examples of the nonionic surfactant to be added and blended in the component (A) α-sulfofatty acid alkyl ester salt-containing concentrate include the following. (1) A fatty acid polyoxyalkylene alkyl ether represented by the following chemical formula 2.

Embedded image (R₁CO: saturated or unsaturated fat having 6 to 20 carbon atoms
Acid residue AO: C2-C4 oxyalkylene group or it
Mixed oxyalexin group n: shows the average number of moles of added oxyalkylene, 3 to 3
0 (including random and block added) R_Two: Lower alkyl group having 1 to 5 carbon atoms)

(2) A polyoxyethylene alkyl ether having a carbon chain length of 8 to 18 of a saturated or unsaturated linear or branched alcohol and an average addition mole number of oxyethylene of 3 to 30. (3) The carbon chain length of the saturated or unsaturated linear or branched alcohol is 8 to 18, the average number of added moles of oxyethylene is 3 to 30, the average number of added moles of oxypropylene is 2 to 3
0 polyoxyethylene polyoxypropylene alkyl ether.

The content of the nonionic surfactant is as follows:
When (A) the α-sulfofatty acid alkyl ester salt aqueous solution is added and blended, the blending amount is preferably 0.1 to 10% by weight, and preferably 0.1 to 5% by weight. If the amount added exceeds 10% by weight, the physical properties of the product powder will be significantly deteriorated. The addition amount and the addition amount of the anionic surfactant to be described later are numerical values when the detergent particles obtained by kneading and pulverizing are 100% by weight.

Specific examples of the anionic surfactant added and blended in the component (A) α-sulfofatty acid alkyl ester salt-containing concentrate include sulfates, sulfonates and phosphates. Can be exemplified. 1) an α-olefin sulfonate having an average carbon number of 10 to 20; 2) an alkyl sulfate having an average carbon number of 10 to 20; and 3) a linear or branched alkyl group or alkenyl group having an average carbon number of 10 to 20. Alkyl ether sulphate or alkenyl ether sulphate having an average of 0.5 to 8 mol of ethylene oxide, 4) fatty acid lower alkyl having an average carbon number of 8 to 22 (C ₁ to
C ₃ ) ester sulfonates, 5) saturated or unsaturated fatty acid salts having an average carbon number of 10 to 22. Alkali metal salts such as sodium and potassium are usually suitable as counterions in these anionic surfactants.

These anionic surfactants (A) α-
When blended in the sulfo fatty acid alkyl ester salt concentrate, the blending amount is preferably 0.1 to 10% by weight, and preferably 1 to 8% by weight. When the compounding amount deviates from this range, the solubility is remarkably lowered. Other detergent components other than the component (B) include usual detergent components such as anionic and nonionic surfactants, zeolite, inorganic builders such as sodium tripolyphosphate and sodium pyrophosphate, sodium citrate, and ethylenediamine tetrachloride. Sodium acetate, nitrilotriacetic acid salt, sodium polyacrylate, sodium acrylate-sodium maleic anhydride copolymer, calcium builder such as polyacetal carboxylate, alkali builder such as carbonate and silicate, carboxymethyl cellulose, polyethylene glycol, etc. Recontamination inhibitors, enzymes such as protease, lipase, cellulase, amylase, fluorescent agents, fragrances,
A dye or the like can be used.

In the present invention, the above-mentioned (A) α-sulfofatty acid alkyl ester salt-containing concentrate: 10 to 40% by weight
(Preferably 15 to 25% by weight) and (B) other detergent components: 60 to 90% by weight (preferably 65 to 85% by weight) are directly kneaded with a kneader or the like, and then pulverized and granulated (crushed and granulated). ) Do. When the amount of the component (A) is too large in the above mixing ratio of the component (A) and the component (B), the kneading properties are deteriorated and the appearance of the powder is also deteriorated. On the other hand, if the amount of the component (B) is excessive, the detergency will decrease. Further, at the time of pulverization, a pulverization aid such as finely powdered sodium carbonate or zeolite may be added. The obtained detergent particles can be used as they are, or can be powder-mixed with a fluidity improving agent such as zeolite, a detergent enzyme, a bleaching agent, a bleaching activator and the like to obtain a high bulk density detergent composition.

Examples of granulation methods include a KRC kneader (manufactured by Kurimoto Iron Works), a batch type kneader (vertical kneader: manufactured by Dalton), and a crusher is Fitzmill (manufactured by Hosokawa Micron) and speed mill (Okada Seiko). Manufactured by the company) and the like. More efficient crushing can be achieved by using a crushing aid during crushing. The average particle size is 20μ
Inorganic particles of m or less are preferable, zeolite, sodium carbonate, white carbon, etc. are used, and the amount of the auxiliary agent is product 1
1 to 20% by weight is preferable to 2% to 10% by weight
% Is more preferred. If the amount is larger than this amount, the physical properties of the powder are remarkably deteriorated, and if the amount is smaller, the effect is not exhibited. After that, it is possible to add an inorganic compound such as powder zeolite having an average particle size of 10 μm or less as a flow modifier. Further, it is also possible to powder-blend a chelating builder, an enzyme, etc., which is a detergent improving agent. As the chelate builder used here, powder zeolite, layered silicate, maleic acid-
Examples thereof include a copolymer of sodium acrylate and β-alanidin sodium acetate. Treatments such as spraying of a nonionic surfactant or an aqueous solution thereof or spraying of a fragrance for perfuming can be performed in order to suppress dust generation.

For the purpose of developing an efficient method for concentrating α-SF, the evaporation behavior of an aqueous solution containing α-SF was examined as basic data. It was found that there is a region (depending on the composition) that changes in the rate-decreasing drying rate region, and there is a phenomenon in which the evaporation capacity changes extremely in α-SF. That is, in the area where the water content is easily evaporated (constant rate drying area), sufficient evaporation can be performed by vacuum flash evaporation, which consumes less power on the equipment, so that the concentration is performed, and then about 10%.
In the low moisture area below, it is difficult to evaporate only by the flash evaporation method because it is a rate-decreasing area, so it is preferable to use a rotary thin film evaporator that forcibly stirs the surface. It was found to be efficient in terms of reducing the size of the rotary thin film evaporator.

The apparatus and method for concentrating 20% or more of the slurry to 10 to 19% is a method in which the slurry is heated to a boiling point or more in a set vacuum at normal pressure and flash evaporation is performed in an evaporator set to a set vacuum degree. Is preferably used, and the apparatus includes a flash evaporator and the like. The "in-pipe concentration method" is also effective, in which a flash is caused in the pipe into which the raw material is introduced into the thin film evaporator and a gas-liquid multiphase flow is introduced into the thin film evaporator without separately providing an evaporator. SF less than 10%
The apparatus and method for obtaining the contained concentrate is a vacuum thin film evaporator (evaporator: Sakura Seisakusho; Exeba: Shinko Pantex Co., Ltd.) to efficiently evaporate water while suppressing thermal deterioration of the surfactant. A control dryer: manufactured by Hitachi Ltd.) is preferably used. It was also found that the spray-dried product particles were directly kneaded and pulverized with the SF concentrate to have good solubility of the product at low temperatures.

[0021]

EFFECTS OF THE INVENTION According to the present invention, since it can be produced without using a spray drying method, it is possible to save energy, and since the concentrate containing the α-sulfofatty acid alkyl ester salt can be directly added to the kneading step, the whole process is simplified. It Also, α-
The sulfo fatty acid alkyl ester salt-containing concentrate acts as a binder in the detergent particles, and the α-sulfo fatty acid alkyl ester salt can be uniformly mixed, so that the resulting detergent particles have excellent solubility. Further, since the concentrate containing the α-sulfofatty acid alkyl ester salt having a low water content is used, it is possible to prevent deterioration of the appearance of the powder and hydrolysis due to contact with an alkali. Furthermore, a method of concentrating an aqueous solution of an α-sulfofatty acid alkyl ester salt to 10 to 19% by weight and then obtaining a concentrate of 10% by weight or less by using a vacuum rotary thin film evaporator is small and efficient. is there.

Further, as the characteristic constitution of the present invention, the following can be mentioned. (1) At least one nonionic surfactant in the aqueous solution containing the α-sulfofatty acid alkyl ester salt of (A) of claim 1 is 0.1 when the detergent particles are 100% by weight.
The method for producing a high bulk density granular detergent according to claim 1, wherein the high bulk density granular detergent is contained in an amount of 10 to 10% by weight. (2) In the α-sulfofatty acid alkyl ester salt of (A) of claim 1, 0.1-10% by weight of at least one nonionic surfactant and at least one anionic surfactant are contained. The method for producing a high bulk density granular detergent according to claim 1, which is included. (3) The high bulk density granules according to claim 1, wherein after concentrating the aqueous solution containing an α-sulfofatty acid alkyl ester salt to 10 to 19% by weight, a concentrate of 10% by weight or less is obtained by using a vacuum rotary thin film evaporator. Detergent manufacturing method. (4) It can be produced without using a spray drying method.
Alternatively, the method for producing the high bulk density granular detergent according to 2). (5) The method for producing a high bulk density granular detergent according to claim 1 or 2, which further comprises spray-dried particles as the other detergent component.

[0023]

【Example】

Example 1 The composition shown in Table 1 below was used for the KRC kneader (Kurimoto Iron Works Co., Ltd.).
The mixture was kneaded at 60 ° C. with a pellet and molded with a pelletizer.
Finely powdered sodium carbonate as a grinding aid (particle size 15 μm)
Of 8.0 wt% was added and then pulverized, and coated with 2.0 wt% of zeolite as a fluidity improving agent to give an average particle size of 5
A high bulk density granular detergent having a size of 00 μm and a bulk density of 0.80 g / cc was produced. The evaluation results are shown in Table 5 together with the composition and properties.

[0024]

[Table 1] Table 1: Kneaded composition (A) component: α-SF-containing concentrate (water content = 3.6%) * ¹ 18.0wt% (B) component: potassium carbonate 6.0wt% sodium carbonate 25.0wt% powdered zeolite 38.0wt% Sodium sulfite 1.5wt% Fluorescent agent 0.5wt% Nonion * ² 1.0wt% Total 90.0wt% * 1) α-SF: α-sulfo fatty acid (C = 16-18) Methyl ester sodium salt * 2) Nonion: Polyoxyethylene alkyl (C = 13) ether (average number of moles of ethylene oxide added, EOp = 25)

Example 2 The composition shown in Table 2 below was changed to KRC Kneader (Kurimoto Iron Works Co., Ltd.).
The mixture was kneaded at 60 ° C. with a pellet and molded with a pelletizer.
Finely powdered sodium carbonate as a grinding aid (particle size 15 μm)
Of 8.0 wt% was added and then pulverized, and coated with 2.0 wt% of zeolite as a fluidity improving agent to obtain an average particle size of 4
A high bulk density granular detergent having a volume density of 50 μm and a bulk density of 0.81 g / cc was produced. Table 5 shows the evaluation results.

[0026]

[Table 2] Table 2: Kneaded composition (A) component α-SF + nonion concentrate (water = 4.2%) * ¹ 19.3wt% (B) component Potassium carbonate 6.0wt% Sodium carbonate 25.0wt% Powdered zeolite 36.7wt % Sodium sulfite 1.5wt % Fluorescent agent 0.5wt % Nonion * ² 1.0wt% Total 90.0wt% * 1) α-SF: α-sulfo fatty acid (C = 16-18) Methyl ester sodium salt Nonion: Fatty acid (C = 18) Polyoxyethylene methyl ether (average number of moles of ethylene oxide added EOp = 15) [blending amount 2.0 wt%] * 2) Nonion: same as above

Example 3 The composition shown in Table 3 below was changed to KRC Kneader (Kurimoto Iron Works Co., Ltd.).
The mixture was kneaded at 60 ° C. with a pellet and molded with a pelletizer.
Finely powdered sodium carbonate as a grinding aid (particle size 15 μm)
Of 8.0 wt% was added and then pulverized, and coated with 2.0 wt% of zeolite as a fluidity improving agent to obtain an average particle size of 4
A high bulk density granular detergent of 80 μm and a bulk density of 0.79 g / cc was produced. Table 5 shows the evaluation results.

[0028]

[Table 3] Table 3: Kneaded composition (A) component α-SF + nonion + fatty acid sodium concentrate 24.3 wt% (water content = 5.2%) * ¹ Nonion * ² (2.0wt%) Sodium fatty acid (C = 10-18) (4.5wt%) (B) component Potassium carbonate 6.0wt% Sodium carbonate 25.0wt% Powdered zeolite 31.7wt% Sodium sulfite 1.5wt% Fluorescent agent 0.5 wt% nonion * ² 1.0wt% total 90.0wt% * 1) α-SF: α-sulfo fatty acid (C = 16-18) methyl ester sodium salt * 2) Nonion: polyoxyethylene alkyl (C = ₁₃ ) Ether (average number of moles of ethylene oxide added EOp = 25)

Comparative Example 1 The composition shown in Table 4 below was changed to KRC Kneader (Kurimoto Iron Works Co., Ltd.).
The mixture was kneaded at 60 ° C. with a pellet and molded with a pelletizer.
Finely powdered sodium carbonate as a grinding aid (particle size 15 μm)
Of 8.0 wt% was added and then pulverized, and coated with 2.0 wt% of zeolite as a fluidity improving agent to obtain an average particle size of 4
A high bulk density granular detergent having a volume density of 90 μm and a bulk density of 0.80 g / cc was produced. Table 5 shows the evaluation results.

[0030]

[Table 4] Table 4: Kneaded composition (A) component α-SF + nonionic concentrate (water = 11.5%) * ¹ 19.8wt% (B) component Potassium carbonate 6.0wt% Sodium carbonate 25.0wt% Powdered zeolite 36.2wt % Sodium sulfite 1.5wt % Fluorescent agent 0.5wt % Nonion * ² 1.0wt% Total 90.0wt% * 1) α-SF: α-sulfo fatty acid (C = 16-18) methyl ester sodium salt Nonion: Polyoxyethylene Alkyl (C = 13) ether (average addition mole number of ethylene oxide EOp = 25 [blending amount 2.0 wt%] * 2) Nonion: same as above

[0031]

[Table 5] Table 5: Composition, Properties and Evaluation Results Example Comparative Example 1 2 3 1 Main composition (wt%) (A) Component origin: α-SF 18.0 17.3 17.8 17.8 Nonion-2.0 2.0 2.0 Fatty acid salt- − 4.5 − (B) Component origin: Nonion 1.0 1.0 1.0 1.0 Potassium carbonate 6.0 6.0 6.0 6.0 Sodium carbonate 33.0 33.0 33.0 33.0 Zeolite 40.0 38.7 31.7 38.2 Other 2.0 2.0 2.0 2.0 Properties Average particle size (μm) 450 450 480 490 Bulk density (g / cc) 0.80 0.81 0.79 0.80 Angle of repose (°) 40 45 45 45 Manufacturability (-) Good Good Good Good Good quality Powder whiteness * ¹ (b value) 2.4 2.6 2.9 5.8 Solubility * ² (-) 10 ℃ B A A C 5 ℃ B A ~ B A ~ B C Hydrolysis * ³ (-) 5 7 9 23 * 1) Powder whiteness 24 # pass (710μ) to 42 # on (3
The particle size was adjusted to 50 μm and the powder whiteness (b value) was measured with a colorimetric color difference meter model Z-1001DP manufactured by Nippon Denshoku Co., Ltd. * 2) Evaluation method for solubility (cloth adhesion) A washing machine (swirl type, reversal type) was used, and tap water and a dark cotton shirt were used. After immersing the cloth to be washed in tap water having a liquid volume of 30 L, a bath ratio of 1: 3, and a temperature of 10 ° C. or 5 ° C., 50 g of the detergent composition was sprinkled and then washed for 5 minutes. After the washing was completed, the cloth to be washed was dehydrated for 1 minute, and the adhesion of the detergent composition to the cloth was evaluated according to the following criteria. A: No deposit is observed. B: Very little deposit is observed. C: Adhesion is recognized. * 3) Method for measuring the rate of increase in hydrolysis The amount of anionic surfactant is determined by methylene blue back titration, and the total amount M with α-sulfofatty acid di-salt is determined from the preset anionic surfactant blending ratio. Next, the detergent composition was treated with a 90% ethanol solution at pH = 11 and 50 ° C. to separate the α-sulfofatty acid di-salt as an insoluble matter, and the amount of the di-salt was determined by the methylene blue backdrop method. The hydrolysis rate is calculated by the equation (A).

[0032]

[Equation 1] D = (S / M) × 100% (A) By the above operation, the hydrolysis rate immediately after the production of the detergent composition and after standing for 1 month at 60 ° C. is calculated. The rate of increase in hydrolysis is calculated by.

[0033]

[Equation 2] Hydrolysis increase rate (%) = (hydrolysis rate after one month)-(hydrolysis rate immediately after production) (B)

Example 4 The compositions shown in Table 6 below were kneaded using a KRC kneader (Kurimoto Iron Works) at 55 ° C., and then molded by a pelletizer. After adding 8 wt% of finely powdered sodium carbonate as a grinding aid, it is ground and coated with zeolite 2% to have an average particle size of 53
A high bulk density granular detergent with 0 μm and a bulk density of 0.8 g / cc was produced.

[0035]

[Table 6] Table 6: Kneaded composition (A) component α-SF-containing concentrate (water content = 9.2%) 16wt% α-SF: 13wt% nonion: 2wt% potassium sulfate: 1wt% (B) component potassium carbonate 15wt % Sodium carbonate 15wt% Powdered zeolite 23wt% Sodium sulfite 2wt% Fluorescent agent 0.5wt% Soap 8wt% AOS 2wt% Nonion 0.5wt% LAS 8wt% Total 90wt% The quality evaluation results of the above composition are as follows. .

Example 5 The α-SF-containing concentrate was concentrated under the conditions shown in Tables 7 and 8. Flash evaporation is a heating tube (made by Sakuma Seisakusho)
Was concentrated to 15% using a vacuum evaporator and then introduced into a vacuum thin film evaporator (Exeba: Shinko Pattec Co., Ltd.) for further concentration to obtain a 4.2% α-SF-containing concentrate. The α-SF-containing concentrates of Tables 7 and 8 and the component (B) were kneaded at 52 to 54 ° C using a KRC kneader (Kurimoto Iron Works), and then molded with a pelletizer. After adding 8 wt% of finely powdered sodium carbonate as a grinding aid, grinding is performed to obtain zeolite 2
% Coated.

Example 6 The same method as described above was used to prepare the α-SF-containing concentrate. SF-containing concentrates of Tables 7 and 8 above (B)
50 with ingredients using KRC Kneader (Kurimoto Iron Works)
After kneading at ˜55 ° C., it was molded with a pelleter. After adding 8 wt% of finely powdered sodium carbonate as a grinding aid, it was ground and coated with zeolite 2%.

Comparative Example 2 An α-SF-containing aqueous solution was concentrated only with a thin film evaporator.
The SF-containing concentrates of Tables 7 and 8 and the component (B) were kneaded at 50 to 55 ° C using a KRC kneader (Kurimoto Iron Works), and then molded by a pelletizer. After adding 8 wt% of finely powdered sodium carbonate as a grinding aid, it was ground and coated with zeolite 2%. Table 7 and Table 8 above
From the examples and comparative examples, it is understood that the apparatus scale can be made compact by performing the one-step concentration.

[0039]

Table 7: Example 5 Example 6 Comparative Example 2 Raw material composition α-SF wt% 17.3 17.3 17.3 Nonion wt% 3 3 3 Other components wt% (potassium carbonate) 1 (potassium sulfate) 1 (potassium sulfate) ) 1 Raw material moisture% 24.2 24.2 24.2 Concentration condition Single-stage concentration type Flash evaporator Flash evaporator Capacity kg / h 80 80 Temperature ℃ 140 140 None Vacuum degree Torr 100 100 Equipment size * ⁴ m ² / lt 4-6 4-6 1- stage Concentrated water 15 15 − Two-stage concentration model Thin film evaporator Thin film evaporator Thin film evaporator Temperature ℃ 120 120 120 Vacuum degree Torr 100 100 100 Peripheral speed m / s 11 11 11 Equipment size m ² / lt 7〜8 7〜8 23 -25 two-stage concentrated water% 4.2 4.6 4.5 * 1) Linear alkylenebenzenesulfonic acid = 10 wt% -α-olefin sulfonate = 2 wt% Soap = 6 wt% * 2) Linear alkylenebenzenesulfonic acid = 10 wt%・ Α-Olefin sulfonate = 2wt% ・ Soap = 6wt% ・ Zeolite = 18 wt% sodium carbonate = 15 wt%, potassium carbonate = 4 wt%, fluorescent agent = 05 wt% sodium sulfite = 1.5 wt% (seed product water content = 5% bulk density = 0.3 g / cc) * 3) Water temperature of solubility test Was performed with tap water at 5 ° C. * 4) Heat transfer area required to make 1t of α-SF containing concentrate

[0040]

Table 8: Example 5 Example 6 Comparative Example 2 α-SF-containing concentrate composition wt% 21.3 21.3 21.3 B component composition Potassium carbonate wt% 10 5 5 Sodium carbonate wt% 24.7 10.7 10.7 Zeolite wt% 21 6 6 Other wt% 5 − − Other active agents * ¹ wt% 18 − − Spray dried product * ² wt% − 57 57 Properties Average particle size μm 450 500 490 Bulk density g / cc 0.81 0.80 0.80 Angle of repose ° 45 40 40 Quality Powder whiteness b value 1.9 1.8 1.8 Solubility (10 ° C) A A A * ³ (5 ° C) A to B A A Hydrolysis% 799 9 * 1) Linear alkylene benzene sulfonic acid = 10 wt% ・ α -Olefin sulfonate = 2 wt%, soap = 6 wt% * 2) Linear alkylene benzene sulfonic acid = 10 wt%, α-olefin sulfonate = 2 wt%, soap = 6 wt%, zeolite = 18 wt% Sodium carbonate = 15 wt% · potassium carbonate = 4 wt% · fluorescent agent = 05 wt% sodium sulfite = 1. 5 wt% (seed product water content = 5% bulk density = 0.3 g / cc) * 3) The water temperature for the solubility test was 5 ° C. tap water. * 4) Heat transfer area required to make 1t of α-SF containing concentrate

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Tomoki Kubo 1-3-7 Main Office, Sumida-ku, Tokyo Lion Corporation

Claims (2)

[Claims] 1. When the detergent particles obtained by kneading and pulverizing are 100% by weight, (A) an α-sulfofatty acid alkyl ester salt-containing concentrate having a water content of 10% by weight or less: 10 to 40% by weight ( B) Other detergent components: A method for producing a high bulk density granular detergent, which comprises directly kneading 60 to 90% by weight and then pulverizing the detergent particles. 2. The method according to claim 1, wherein the concentrated aqueous solution containing the α-sulfofatty acid alkyl ester salt is concentrated to 10 to 19% by weight, and then a concentrated product of 10% by weight or less is obtained by using a vacuum rotary thin film evaporator. Method for producing bulk density granular detergent.