JPH04348196A - Production of high-bulk density detergent composition - Google Patents

Abstract

PURPOSE:To obtain the title high-quality composition in an industrially advantageous way by agitation and granulation of spray-dried powder from a water-base slurry containing an alpha-sulfofatty acid alkyl ester (salt), zeolite and sodium sulfate. CONSTITUTION:A water-base slurry with a pH of <=10 (pref. <=9) containing (A) an alpha-sulfofatty acid alkyl ester or its water-soluble salt, (B) zeolite, and (C) sodium sulfate at the weight ratios A/B = (1:0.5)-(1:5) and A/C = (1:0.3)-(1 :3) with the ingredients A, B and C accounting for >=70 ( pref. >=80)wt.% of the total solid content, is put to spray drying. The resulting dry powder is agitated and granulated together with an alkali builder and binder component using a mixer with agitating blades, thus obtaining the objective composition.

Description

[Detailed description of the invention]

0001

[Industrial Application Field] The present invention provides a high-quality, high-density detergent composition containing an α-sulfo fatty acid alkyl ester or a water-soluble salt thereof as a main active agent. The present invention relates to a method for producing bulk density detergent compositions.

0002

[Prior art and problems to be solved by the invention] Conventionally,
High bulk density detergent compositions are attracting attention because they can wash clothes with a small amount of detergent, and are also excellent in terms of transportability, storage, display, etc., and fully satisfy the needs of consumers. ing. In addition, this high bulk density detergent composition is usually produced by kneading and mixing detergent raw materials, crushing and granulating, etc.
897-9, JP-A-1-318097, JP-A No. 2-
No. 14297, No. 2-29500, No. 2-86700
No. 2-173099, No. 2-245100, No. 2-286799, No. 2-38497, No. 2-14
No. 5699, No. 2-169696, No. 2-23229
9, No. 2-232300, No. 3-33199, etc., various methods are proposed, but among these methods, the spray-dried product of a detergent containing a surfactant and a builder is compacted. Knife cutter that rotates at high speed after processing
A method of performing granulation treatment in the presence of a surface modifier using a crushing granulator that crushes by impact and shear force (Japanese Patent Laid-Open No. 61
69899), a mixer that has a vertical stirring shaft inside a vertical mixing tank and a stirring blade attached to this shaft mixes the powder.
A method of agitating and granulating a detergent spray-dried product containing a detergent in the presence of a surface modifier and a binder (Japanese Patent Laid-Open No. 61-6
No. 9897), after pulverizing the spray-dried product of detergent containing a surfactant and a builder, a stirring shaft protruding from the bottom is placed inside a solid mixing tank, and a stirring blade is attached to this shaft. There is a method in which agitation granulation is carried out in the presence of a surface modifier and a binder using a mixer that mixes powder (Japanese Patent Laid-Open Publication No. 61-69898), and a method using a horizontal mixing tank (Japanese Unexamined Patent Publication No. 61-69898). Publication No. 61-69900)
etc. are considered useful.

On the other hand, water-soluble salts of α-sulfo fatty acid alkyl esters (sulfonate salts of fatty acid lower alkyl esters) are surfactants with excellent detergency, especially hard water resistance, and high bulk density detergents containing them are The composition was published in JP-A-62-5.
This method has been proposed in Japanese Patent Publication No. 97, Japanese Unexamined Patent Publication No. 2-103294, and the like.

However, when a high bulk density detergent composition containing a water-soluble salt of an α-sulfo fatty acid alkyl ester is produced, when this α-sulfo fatty acid alkyl ester salt comes into contact with an alkali, it is hydrolyzed to form an α-sulfo fatty acid dihydride. Performance tends to deteriorate because sodium salt is produced as a by-product. Furthermore, when spray drying raw materials such as water-soluble salts of α-sulfo fatty acid alkyl esters and builders, powder physical properties such as angle of repose and cohesiveness tend to deteriorate, and agglomeration between powders occurs in the drying tower during spray drying. It is difficult to stably manufacture the product industrially due to the following reasons. Therefore, it is difficult to industrially advantageously produce high-quality, high-bulk-density detergent compositions containing water-soluble salts of α-sulfo fatty acid alkyl esters using the conventional methods described above. It would be desirable to develop a method for producing bulk density detergent compositions.

[0005]

[Means and effects for solving the problems] In view of the above circumstances, the present inventors have made intensive studies on the method for producing high bulk density detergent compositions, and as a result, the inventors have determined that α-sulfofatty acid alkyl ester or a water-soluble salt thereof. Bulk density 0.5g as main activator
/cc or more, a method for producing a high bulk density detergent composition containing (1) a water-soluble salt of α-sulfo fatty acid alkyl ester, (2) zeolite, and (3) sodium sulfate in a weight ratio of (1) /(2)=1/0.5~1/5, (1)
/(3) = 1/0.3 to 1/3, and 70% by weight or more of the total solid content is the above (1), (2) and (3).
) by spray-drying an aqueous slurry with a pH of 10 or less, and then stirring and granulating the resulting spray-dried powder with alkali builder and binder components using a stirring mixer using a stirring blade. It has been discovered that the above-mentioned problems during production can be solved and that a high quality, high bulk density detergent composition containing an α-sulfo fatty acid alkyl ester or a water-soluble salt thereof as a main active agent can be produced stably on an industrial scale.

That is, in the present invention, when α-sulfo fatty acid alkyl ester or its salt is used in combination with zeolite and sodium sulfate as a spray-drying powder raw material, and these three components are blended in the above ratio, the spray-drying of the powder raw material is It is possible to obtain a dry powder having satisfactory physical properties such as low cohesiveness through sufficient drying. By adding -, hydrolysis of the α-sulfo fatty acid alkyl ester or its water-soluble salt is prevented as much as possible, and therefore there is almost no by-product of α-sulfo fatty acid disodium salt, and the detergent composition is It was discovered that there was almost no deterioration in performance, and this led to the present invention.

[0007] The present invention will be explained in more detail below. The high bulk density detergent composition of the present invention contains (
1) α-sulfo fatty acid alkyl ester or water-soluble salt thereof, (2) zeolite, (3) sodium sulfate, (4)
It is made by blending an alkali builder, (5) a binder component, etc.

Here, the main active agent of the composition of the present invention (
As the component 1), sulfonic acid salts of fatty acid lower alkyl esters having a fatty acid residue having 8 to 22 carbon atoms, particularly 10 to 18 carbon atoms, are preferably used, and among them, the following general The one represented by formula (1) is preferably used.

[0009]

[Formula 1] (However, in the formula, R1 is an alkyl group having 8 to 22 carbon atoms, R2
is a lower alkyl group having 1 to 3 carbon atoms, and M is an alkali metal atom. )

Examples of water-soluble salts of α-sulfo fatty acid esters of formula (1) include sodium salts of sulfo fatty acid esters produced from natural hydrogenated fatty acids and fatty acid mixtures, such as methyl stearate,
Preference is given to using palmitic acid ethyl ester, hydrogenated palm kernel fatty acid methyl ester or alpha-sulphofatty acid ester salts of hydrogenated tallow fatty acid methyl ester. It should be noted that the α-sulfofatty acid ester salts generally contain dependent amounts of α-sulfofatty acid disalts, which can result from hydrolysis of the ester bonds during industrial post-treatments, for example bleaching with H2O2 or neutralization. This di-salt is usually present in an amount of 3 to 10% by weight in industrial products, without impairing the effectiveness of the product.

[0011] Further, as the α-sulfo fatty acid alkyl ester or its water-soluble salt, those having specific carbon numbers as shown in (a) and (b) below are used, (a)/(b) = 1/9 to 6/4, In particular, it is preferable to combine them in a weight ratio of 2/8 to 5/5 from the viewpoint of solubility of the detergent composition. (a) Those whose aliphatic residues have 12 to 14 carbon atoms (b) Those whose aliphatic residues have 16 to 18 carbon atoms

[0012] As a method for producing the α-sulfo fatty acid alkyl ester or salt thereof of the present invention, any known method may be adopted, but in this case, the α-fatty acid ester serving as the starting material typically has the general formula RCH2COOR' (In the formula, R represents a straight chain or branched alkyl group having 10 to 20 carbon atoms, and R' has 1 to 6 carbon atoms.
(representing a straight chain or branched alkyl group), preferably R has 12 to 18 carbon atoms, and R
' has 1 to 3 carbon atoms.

Sulfonation of α-fatty acid esters can be carried out using a sulfonating agent such as sulfuric anhydride diluted with an inert gas in a molar ratio of 1 to 2, for example, by the method described in JP-A-58-157763. It can be carried out usually at a temperature of 50 to 100°C. As the sulfonation method, any method such as a thin film sulfonation method or a tank sulfonation method can be employed.

[0014] The sulfonated product is aged to complete the sulfonation, but this aging is carried out at 50 to 100°C for 5 to 1 hour.
It is preferable to stir for 20 minutes.

The α-sulfo fatty acid alkyl ester thus obtained was then disclosed in JP-A-50-77317, JP-A-59-25369 and JP-A-59-1687.
Bleaching can be performed by the method described in Publication No. 0. Bleaching can be carried out by first mixing α-sulfo fatty acid alkyl ester and alcohol, and after both are uniformly mixed, hydrogen peroxide is immediately added. In this case, the amount of alcohol added is preferably 5 to 30 parts by weight, more preferably 10 to 20 parts by weight, per 100 parts by weight of the α-sulfo fatty acid alkyl ester. If this amount is less than 5 parts by weight, the bleaching effect may not be sufficient, and if it exceeds 30 parts by weight, the α
- This may cause a decrease in the purity of the sulfo fatty acid alkyl ester. In addition, alcohol has 1 to 1 carbon atoms.
6 is preferably used, specifically methanol,
Examples include ethanol, isopropyl alcohol, and butanol. These alcohols have a low water content;
It is preferable to use one with a purity of 95% by weight or more.

After adding alcohol and stirring to mix uniformly, bleaching is carried out by adding H2O2, and the amount of H2O2 added is preferably 0.2 to 10 parts by weight per 100 parts by weight of α-sulfo fatty acid alkyl ester. parts, more preferably 1 to 5 parts by weight. If this amount is less than 0.2 parts by weight, the bleaching effect may not be sufficient, while if it exceeds 10 parts by weight, the bleaching effect remains the same and economical benefits are unlikely to occur.

[0017] The bleaching temperature is preferably 50 to 100°C, and if bleaching is carried out at this temperature, the bleaching can be completed in 5 to 120 minutes. If it is lower than 50°C, bleaching takes a long time, while if it is higher than 100°C, the color tone may return after bleaching and the color tone may deteriorate.

[0018] In this way, a light-colored α-sulfo fatty acid alkyl ester was obtained, which was disclosed in JP-A-57-7462.
If neutralized with an alkaline aqueous solution using the method described in the publication, α
- A sulfo fatty acid alkyl ester salt can be obtained.

[0019] The blending amount of component (1), α-sulfo fatty acid alkyl ester or water-soluble salt thereof, is preferably 5 to 30% (wt%, hereinafter the same), particularly 8 to 25%, of the entire detergent composition. preferable. If the amount is less than 5%, sufficient detergency may not be obtained, and if it exceeds 30%, manufacturing may become difficult.

In the present invention, surfactants such as LAS, AOS, AES, AS, soap, etc. are used as components (2) and (3) in addition to the above-mentioned α-sulfo fatty acid alkyl ester or water-soluble salt thereof. can be added together to prepare a spray-dried powder. Note that the amount of other activators added is preferably within a range that does not impede the effects of the present invention.

Next, as the zeolite for component (2), for example, those commercially available as A type, X type or amorphous synthetic zeolite can be used. Its content is preferably in the range of 5-35%, more preferably 10-25%. If the zeolite content is less than 5%, the physical properties of the powder during production will be poor, and in addition, satisfactory cleaning power may not be obtained, and if it exceeds 35%, there is a risk that zeolite particles may adhere to the items being washed. occurs.

Furthermore, the component (3), sodium sulfate, is added to the α-sulfo fatty acid alkyl ester or its water-soluble salt and the zeolite, as described below.

Further, as the alkali builder, known ones such as sodium silicate, sodium carbonate, sodium bicarbonate, potassium carbonate, sodium sulfate, sodium sesquicarbonate, powdered sodium silicate, etc. can be used. is preferably used.

[0024] Known binder components can also be used,
Examples include AOS, AS, AES, LAS, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose, polyacrylate, glycerin, ethylene glycol, propylene glycol, sodium silicate, and especially anionic surfactants and nonionic surfactants. , water-soluble polymeric substances, and water are preferably used.

[0025] It is preferable to add a surface modifier to the composition of the present invention, and examples of the surface modifier include inorganic fine powders such as zeolite, silicon dioxide, bentonite, talc, clay, and calcium carbonate, and sodium carbonate. , inorganic powders (finely pulverized) such as sodium sulfate, metal soaps such as calcium stearate, etc., and one or more of these may be used. The average particle diameter of these surface modifiers is preferably 30 μm or less, particularly 10 μm or less, and the amount added is preferably 0 to 20%, particularly 2 to 15% of the total composition.

Furthermore, in addition to the above-mentioned components, other optional components such as enzymes, fragrances, bleaching agents, etc. can be added within the range that does not impede the effects of the present invention.

In the production method of the present invention, when producing a high bulk density cleaning composition containing a water-soluble salt of α-sulfo fatty acid alkyl ester as a main active agent and having a bulk density of 0.5 g/cc or more, first (1 ) An aqueous slurry containing α-sulfo fatty acid alkyl ester or a water-soluble salt thereof, (2) zeolite, and (3) sodium sulfate is spray-dried to prepare a spray-dried powder. When sodium sulfate is added in addition to α-sulfofatty acid alkyl ester or its water-soluble salt and zeolite in this way, these powder particles swell during spray drying, increasing their surface area and improving drying efficiency. Furthermore, the swelling of the dry particles is large and the bulk density is low, so when mixing the dry powder (base powder) into a detergent composition to control the bulk density, it is necessary to Since only a small amount is required, it is possible to prevent increase in dust generation, deterioration in solidification, deterioration in appearance, etc. that occur when a large amount of base powder is mixed. In addition, when the content of α-sulfo fatty acid alkyl ester or its water-soluble salt in a detergent composition increases, dry powder agglomerates, and in severe cases, some undried powder may be discharged from the bottom of the column. However, as mentioned above, addition of sodium sulfate not only leads to a decrease in drying efficiency but also has an adverse effect on the mixing of base powders.However, as mentioned above, adding sodium sulfate improves the drying efficiency and prevents dry powders from adhering to each other. , which can improve the physical properties of dry powder.

Here, the aqueous slurry contains components (2) and (3) in a weight ratio of (1)/(2) to component (1).
=1/0.5 to 1/5, preferably 1/0.6 to 1/3
and (1)/(3)=1/0.3 to 1/3
, preferably in a range of 1/0.4 to 1/2. α of component (1) compared to the amount of components (2) and (3)
- If the amount of the sulfo fatty acid alkyl ester or water-soluble salt thereof is too large, the powder physical properties of the spray-dried particles may deteriorate or agglomeration of the dried particles may occur during spray-drying. Also,
If the amount of zeolite (component (2)) is too large compared to the amount of component (1), the content of α-sulfo fatty acid alkyl ester or its water-soluble salt in the detergent composition cannot be increased; (3) If the amount of sodium sulfate (component) is too large, the load on equipment such as a drying tower will become large, which is economically disadvantageous. Therefore, if the blending ratio of components (1) to (3) is outside the above range, the object of the present invention cannot be achieved.

Furthermore, the above components (1) to (3) are mixed so that the solid content of the aqueous slurry is 70% or more, preferably 80% or more of the above components (1) to (3). be. In this case, other surfactants, fluorescent agents, sodium sulfite, chelate builders such as polyacrylic acid and citric acid, etc. are blended as the remainder of the solid content.

[0030]Although this aqueous slurry can be prepared by a conventional method, it is necessary to adjust its pH to below 10, preferably below 9; if the pH exceeds 10, α-sulfo fatty acid alkyl The ester or its water-soluble salt decomposes and the performance of the detergent composition deteriorates. The pH of the aqueous slurry can be adjusted using conventional methods, such as inorganic and organic acids such as sulfuric acid, citric acid, polyacrylic acid, and alkylbenzenesulfonic acids, sodium hydroxide, potassium hydroxide, and silicic acid. It can be adjusted by adding an alkali such as sodium, sodium carbonate, sodium sulfite, potassium carbonate, etc. Furthermore, it is advisable to add a small amount of alkaline raw materials such as sodium carbonate, potassium carbonate, etc. to the aqueous slurry as a spray-drying raw material within a range where the pH can be maintained at 10 or less, in order to increase the thermal stabilization temperature of the dry powder. It is a good idea and can be added if necessary.

Furthermore, the above aqueous slurry can be spray-dried by a conventional method, for example, using a countercurrent spray drying tower at a hot air temperature of 200 to 300°C.

Next, in the production method of the present invention, the dry powder thus obtained is agitated and granulated with an alkali builder and a binder component using a stirring mixer using a stirring blade.

In this case, the amount of the dry powder used is preferably 40 to 80%, particularly 50 to 70% of the total composition. Furthermore, the amount of alkali builder used is preferably 10 to 50%, particularly 15 to 30%, based on the total amount of powder, and the amount of binder component used is preferably 10 to 50%, particularly 15 to 30%, based on the total amount of powder in the entire composition. It is desirable to set it as 5-25%, especially 5-15%.

The alkali builder and binder components mentioned above are added as dry powders during granulation, but the alkali builder can also be blended into powder after granulation.

[0035] The stirring mixer using a stirring blade used in the production method of the present invention includes a horizontal stirring mixer in which a stirring blade is attached to the inside of a horizontal mixing tank for mixing, a vertical stirring mixer in which a stirring blade is attached to the inside of a horizontal mixing tank, and a stirring mixer in which a stirring blade is attached to the inside of a horizontal mixing tank. A vertical stirring mixer having blades and performing mixing by rotation of the stirring blades is preferably used. Specifically, horizontal stirring mixers include Loedige mixers, ribbon mixers, Spartan dissolvers, pug mills, turbulizers, etc., and vertical stirring mixers include high speed mixers, Henschel mixers, New Gram machines, etc. Examples are Loedige mixer, high speed mixer, etc.
Domixer is preferably used. Note that the stirring and mixing conditions are not particularly limited and may be normal stirring and mixing conditions.

In the method of the present invention, when a surface modifier is used, there are no restrictions on its addition conditions, and it may be used by mixing it with the base powder in advance in order to further improve the physical properties of the base powder. Alternatively, it may be added during the granulation stage or at the final stage. Furthermore, it is also possible to use one or more surface modifiers simultaneously or separately in each step.

[0037] Furthermore, there are no particular restrictions on the conditions for adding other optional ingredients, and they can be added under normal conditions. For example, characterizing agents such as bleach, enzymes, and granule softeners may be sprayed onto the granulated product. and can be mixed. In addition, when adding sodium sulfate as a balance agent to the composition,
It is desirable to add the required amount at the time of granulation, separately from the sodium sulfate blended into the aqueous slurry.

The detergent composition thus obtained has a bulk density of 0.5 g/cc or more, and has a high bulk density.

[0039]

According to the production method of the present invention, a high bulk density detergent composition having a bulk density of 0.5 g/cc or more containing an α-sulfo fatty acid alkyl ester or a water-soluble salt thereof as a main active agent can be produced industrially. It can be stably produced, and the obtained high bulk density detergent composition has very little performance deterioration and is of very high quality.

[0040]

[Examples] The present invention will be specifically explained below with reference to Examples and Comparative Examples, but the present invention is not limited to the following Examples. In addition, in the following examples, parts indicate parts by weight.

[Examples 1 to 5, Comparative Examples 1 to 3] Tables 1 and 2
A slurry of the components shown in 40% moisture was made into a slurry with a water content of 40%, and was spray-dried to a moisture content of 5% using a countercurrent spray dryer at a hot air temperature of 230° C. to prepare a spray-dried powder.

Next, 14 parts of sodium carbonate (pulverized to an average particle size of 50 μm), 7 parts of potassium carbonate (pulverized to an average particle size of 50 μm), and a surface modifier were added to the above spray-dried powder as an alkali builder. 5 parts of silicon dioxide was added as a binder component, and after adding macho acid as a balance agent to a Loedige mixer (manufactured by Matsusaka Trading Co., Ltd.) to make a final product of 100 parts, 70% of the active ingredient was added as a binder component.
4 parts of AOS-K (potassium α-olefin sulfonate) slurry, 3 parts of α-sulfo fatty acid methyl ester sodium salt (C12-C16) slurry containing 70% active ingredient, 84% nonionic surfactant solution (alkyl group (Polyoxyethylene alkyl ether having 13 carbon atoms and an average added mole number of ethylene oxide of 20) and 2 parts of water were added, and after granulation, 2 parts of zeolite powder was added as a surface modifier. Furthermore, the entire amount of the obtained granulated product was pulverized with a speed mill (manufactured by Okada Seiko Co., Ltd.) to adjust the particle size, and then 1 part of zeolite powder, 0.2 parts of fragrance, and 0.1 part of enzyme were added to obtain a high bulk density product. A detergent composition was obtained.

The physical properties of the spray-dried powder and the properties of the obtained high bulk density detergent composition are also listed in Tables 1 and 2.

[0044]

[Table 1]

[0045]

[Table 2]

[0046]

[Chemical 2]

[Example 6] 53.5 parts of the same spray-dried powder as in Example 1, 20 parts of sodium carbonate as an alkali builder, 5 parts of potassium carbonate (pulverized to an average particle size of 50 μm), and 4 parts of zeolite powder and stirred and mixed for 10 minutes using a Loedige mixer (manufactured by Matsusaka Boeki Co., Ltd.).
Furthermore, as a binder component, 3 parts of 84% nonionic surfactant solution (polyoxyethylene alkyl ether, C13, average number of added moles of EO 20), 2 parts of water, and 70 parts of active ingredients were added.
% AOS-K (potassium alpha-olefin sulfonate)
Add 7 parts of slurry and stir for 3 minutes until the average particle size is 3000.
A granulated product of μm size was obtained. To this granulated product, 3 parts of silicon dioxide powder was added as a surface modifier, and the particle size was adjusted by pulverizing with a speed mill (manufactured by Okada Seiko Co., Ltd.) to obtain a 500 μm pulverized product, followed by 0.2 parts of fragrance. , 1 part of enzyme, and 1.3 parts of zeolite powder were added to obtain a high bulk density detergent composition.

The obtained high bulk density detergent composition has a bulk density of 0.
．． 85g/cc, disodium salt content (vs. α-SF)
was 7%, and the product color was 4-5.

[Example 7] 53.5 parts of the same spray-dried powder as in Example 1, 22 parts of sodium carbonate (pulverized to an average particle size of 50 μm) as an alkali builder, and 84% nonionic interface as a binder component. 2 parts of activator solution (polyoxyethylene alkyl ether, C13, average number of added moles of EO 20), 1.5 parts of water, 67% active ingredient A
ES-Na (sodium polyoxyethylene alkyl sulfate, C10 to C16, average number of added moles of EO 3), 7.0
part, silicon dioxide powder (primary particle size 0.0
1μm) and 5 parts using a Loedige mixer.
The mixture was stirred for a minute to obtain a granulated product with an average particle size of 450 μm. Excluding coarse particles of 14 mesh or more in this granulated product, fragrance 0.2
part, enzyme 1.0 part, zeolite powder (primary particle size 1 μm)
2.0 parts were added thereto, and further 0.8 parts of a 50% polyethylene glycol aqueous solution (molecular weight 1000) was added as a dust generation inhibitor to obtain a high bulk density detergent composition.

The resulting high bulk density detergent composition has an average particle size of 4
It had a diameter of 30 μm, a bulk density of 0.80 g/cc, a disodium salt content (relative to α-SF) of 6%, and a product color of 4.

[Examples 8 to 12, Comparative Examples 4 to 6] Table 3,
The components shown in 4 were made into a slurry with a moisture content of 40%, and the slurry was spray-dried to a moisture content of 5% using a countercurrent spray dryer at a hot air temperature of 230°C to prepare a spray-dried powder.

[0052] The obtained spray-dried powder and the average particle size of 50 μm
20 parts of sodium carbonate pulverized to a primary particle size of 0.01
9.6 parts of micron silicon dioxide fine powder was placed in a high speed mixer (manufactured by Fukae Kogyo Co., Ltd.) and pulverized with stirring for 10 minutes. Next, as a binder, 3 parts of an 84% nonionic surfactant solution (polyoxyethylene alkyl ether, C13, average number of added moles of EO 20) and 70% of the active ingredient AOS-
After adding 1 part of K (potassium α-olefin sulfonate) slurry and 4 parts of water and performing stirring granulation, the primary particle size was 1 μm.
The surface was treated by adding 2 parts of aluminosilicate fine powder. This granulated product was taken out from the high-speed mixer and placed in a container rotating mixer, and 0.2 parts of fragrance and 5 parts of dust suppressant were added.
0.5 part of 0% polyethylene glycol 1000 solution was sprayed, 1 part of enzyme was added, and coarse particles were removed using a 14 mesh sieve to obtain a high bulk density detergent composition. The physical properties of the spray-dried powder and the properties of the detergent composition are also listed in Tables 3 and 4.

[0053] In addition, as an additive during granulation, 1
00 parts by further adding sodium sulfate. The addition was made before the stirring and pulverizing step.

[0054]

[Table 3]

[0055]

[Table 4]

[0056]

[C3]

[Example 13] 50.5 parts of the spray-dried powder of Example 11, 30 parts of sodium carbonate (pulverized to an average particle size of 50 μm), silicon dioxide powder (primary particle size of 0.0
After stirring 7.3 parts of 1 μm) for 2 minutes with a high speed mixer (manufactured by Fukae Kogyo Co., Ltd.), 2 parts of 84% nonionic surfactant solution (same as above), 2 parts of water, and 70% active ingredient solution were added. A
3 parts of OS-K (potassium α-olefin sulfonate) slurry and 1 part of 45% sodium silicate solution were added and further stirred to obtain a granulated product with an average particle size of 1500 μm. Adding 3 parts of zeolite powder (primary particle size 1 μm) to this granulated product,
Grind with a speed mill (manufactured by Okada Seiko Co., Ltd.) to an average particle size of 50.
A pulverized product of 0 μm was obtained. Next, 0.2 part of perfume was ground into this ground product in a drum mixer, and 1 part of enzyme was added to obtain a high bulk density detergent composition. The obtained high bulk density detergent composition had an average particle size of 500 μm and a bulk density of 0.83 g/cc.
The disodium salt content (relative to α-SF) was 8%, and the product color was 4-5.

[Example 14] Spray-dried powder 5 of Example 9
8.7 parts and 30 parts of sodium carbonate (pulverized to an average particle size of 50 μm) were stirred for 2 minutes using a high-speed mixer (manufactured by Fukae Kogyo Co., Ltd.), followed by an 84% nonionic surfactant solution (same as above). After further stirring, zeolite powder (primary Particle size 1μ
m) was added to obtain a granulated product with an average particle size of 580 μm. Add 0.2 parts of fragrance to this granulated product using a drum-type mixer.
After spraying 1 part of a 5-part glycerin aqueous solution, 1 part of enzyme was added to obtain a high bulk density detergent composition. The obtained high bulk density detergent composition had an average particle size of 600 μm and a bulk density of 0.8 g/c.
c. The disodium salt content (relative to α-SF) was 8%, and the product color was 4 to 5.

Claims (1)

[Claims] Claim 1: A bulk density of 0.5 g/cc containing α-sulfofatty acid alkyl ester or a water-soluble salt thereof as the main activator.
In the method for producing the above high bulk density detergent composition, (
1) a water-soluble salt of α-sulfo fatty acid alkyl ester;
(2) Zeolite and (3) sodium sulfate in a weight ratio of (1)/(2) = 1/0.5 to 1/5, (1)/(3)
) = 1/0.3 to 1/3, and 70% by weight or more of the total solid content consists of the components (1), (2), and (3), and the liquid property is an aqueous slurry with a pH of 10 or less. - After spray-drying, the obtained spray-dried powder is agitated and granulated with an alkali builder and a binder component using an agitating mixer using an agitating blade. .