JPH11302700A - Production of granular nonionic detergent composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a process for producing a granular nonionic detergent compsn. whereby the granulation rate can be increased in granulation by stirring while maintaining a high fluidity of granules. SOLUTION: In producing a granular nonionic detergent compsn. which comprises (A) a nonionic surfactant, (B) an aluminosilicate, (C) heavy sodium carbonate, and (D) a light sodium carbonate and in which the sum of amts. of C and D is 10-60 wt.% and the wt. ratio of C/D is (1/2)-(19/1), ingredients B, C, and D are mixed first; and then the resulting mixture and ingredient A are joined together and subjected to granulation by stirring.

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 nonionic detergent composition, and more particularly, to a granular nonionic detergent composition capable of improving the granulation speed while maintaining good fluidity of particles in stirring granulation. The present invention relates to a method for manufacturing a product.

[0002]

2. Description of the Related Art Nonionic surfactants generally have a low foaming property, and their detergency is hardly affected by the hardness of water. Furthermore, it is an excellent surfactant having good biodegradability, low environmental load, low toxicity and no problem in safety. However, since many nonionic surfactants are liquid at room temperature, there is a disadvantage that the nonionic surfactant gradually exudes from the granular nonionic detergent product, and the fluidity and the caking resistance are deteriorated. By stirring granulation using an activator,
When producing a nonionic surfactant-containing granular detergent, there is also a problem in production that granulation control during stirring granulation is not easy.

[0003] Japanese Patent Application Laid-Open No. 2-229894 proposes a granular nonionic detergent composition in which the weight ratio and total amount of heavy sodium carbonate and light sodium carbonate are specified and added to a nonionic surfactant. Although such a composition improves the caking resistance, there remains a problem that it is difficult to control granulation in stirring granulation.
In JP-A-7-258700, a crystalline aluminosilicate and a porous inorganic oxide powder are blended with a nonionic surfactant, and the weight ratio and the total amount of light sodium carbonate and heavy sodium carbonate are specified. Granular nonionic detergent compositions have been proposed, but such compositions have a sufficiently high dust-preventing effect at the time of production or use. , The device is likely to be overloaded.

[0004]

SUMMARY OF THE INVENTION Accordingly, the present invention has been made in view of the above-mentioned circumstances of the prior art, and it is an object of the present invention to increase the granulation speed while maintaining the fluidity of particles in agitated granulation. It is an object of the present invention to provide a method for producing a granular nonionic detergent composition that can perform granulation (the granulation speed can be adjusted to an appropriate speed that can be easily controlled).

[0005]

Means for Solving the Problems As a result of intensive studies, the present inventors have used nonionic surfactants and aluminosilicates, and further used heavy / light sodium carbonate in a specific ratio and amount. In addition, it has been found that the above object can be achieved by adding a nonionic surfactant after mixing all the powder components and subjecting the mixture to stirring granulation, thereby achieving the present invention.

That is, according to the present invention, at least (a)
Nonionic surfactant, (b) aluminosilicate, (c)
It contains heavy sodium carbonate and (d) light sodium carbonate, and the total amount of components (c) and (d) is (c) +
(D) = 10 to 60% by weight and weight ratio (c) / (d)
In producing a granular nonionic detergent composition in which = 1/2 to 19/1, the components (b), (c) and (d) are mixed, and then the component (a) is added, followed by stirring and granulating. A method for producing a granular nonionic detergent composition is provided.

[0007]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in detail. In the method of the present invention, various nonionic surfactants can be used as the nonionic surfactant. Preferred nonionic surfactants include, for example, the following.

(1) 6 to 22 carbon atoms, preferably 8 to 1 carbon atoms
Polyoxyalkylene alkyl (or alkenyl) obtained by adding an alkylene oxide having 2 to 4 carbon atoms to an aliphatic alcohol having an average of 3 to 30 mol, preferably 5 to 20 mol.
ether. Among them, polyoxyethylene alkyl (or alkenyl) ether and polyoxyethylene polyoxypropylene alkyl (or alkenyl) ether are preferable. (2) Polyoxyethyl alkyl (or alkenyl) phenyl ether.

(3) A fatty acid alkyl ester alkoxylate represented by the following formula wherein an alkylene oxide is added between ester bonds of a long-chain fatty acid alkyl ester. R ¹ CO (OA) n OR ² (R ¹ CO represents a fatty acid residue having 6 to 22, preferably 8 to 18 carbon atoms. OA represents a fatty acid residue having 2 to 4 carbon atoms such as ethylene oxide and propylene oxide, preferably Represents an additional unit of alkylene oxide of 2 to 3. n represents an average number of moles of alkylene oxide added, and generally represents 3 to 3;
0, preferably a number from 5 to 20. R ² has 1 carbon atom
Represents a lower alkyl group which may have 1 to 3 substituents. )

(4) Polyoxyethylene sorbitan fatty acid ester. (5) Polyoxyethylene sorbite fatty acid ester. (6) Polyoxyethylene fatty acid esters. (7) Polyoxyethylene hydrogenated castor oil. (8) Glycerin fatty acid ester.

Among the above-mentioned nonionic surfactants, polyoxyethylene alkyl (or alkenyl) ethers having a melting point of 40 ° C. or lower and an HLB of 9 to 16 and fatty acid methyl ester ethoxylate obtained by adding ethylene oxide to fatty acid methyl ester are particularly preferable. Used for Further, these nonionic surfactants may be used as a mixture.

The nonionic surfactant (a) is generally used in an amount of 10 to 40% by weight, more preferably 12 to 35% by weight, particularly preferably 15 to 35% by weight, in the granular nonionic detergent composition.
30% by weight is contained. If this amount is less than 10% by weight,
The granulation speed is reduced in the stirring granulation. Of course, the nonionic surfactant concentration in the obtained detergent particles is not only low but also low in bulk density, so that a good cleaning effect cannot be obtained unless the amount of the detergent used is increased, and the result is inconsistent with recent compactification, and is preferable. Also, it is not preferable in terms of resource saving. On the other hand, if it exceeds 40% by weight, there is no particular problem in the case of batch-type production, but in the case of continuous production, the amount of adhesion to the granulator increases, and the equipment load increases.
Coarse particles increase, making it difficult to manufacture stably,
Not preferred.

In practicing the present invention, (b) aluminosilicate, (c) sodium bicarbonate and (d) light sodium carbonate are first mixed. As the aluminosilicate of the component (b), those generally used in detergents that can supplement alkaline earth metals in tap water can be used. Preferably, A-type zeolites, P-type zeolites,
X-type zeolites and amorphous zeolites are used. Particularly, those having an average primary particle diameter of 10 μm or less are preferable from the viewpoint of solubility. The compounding amount of the aluminosilicate is generally 5 to 50% by weight, preferably 10 to 45% by weight, more preferably 15 to 40% by weight in the granular nonionic detergent composition.
It is. If the amount is less than 5% by weight, the fluidity may be deteriorated and granulation may not be possible. If the amount is more than 50% by weight, it is difficult to add other components.

The heavy sodium carbonate of the component (c) is sodium carbonate having a high bulk density [trade name: granulated ash (Asahi Kasei Corporation) or the like], and the light sodium carbonate of the component (d) is sodium carbonate having a low bulk density [ Product name: light ash (Asahi Kasei Corporation) etc.]. The bulk density of the heavy sodium carbonate used is generally 1.00 to 1.35 g / ml, preferably 1.00.
１1.30 g / ml, and the bulk density of light sodium carbonate is generally 0.45-0.85 g / ml, preferably 0.50-0.80 g / ml. Further, these sodium carbonates preferably have an average particle diameter of 100 to 1000 μm, and more preferably have an average particle diameter of 150 to 800 μm. If the average particle size is less than 100 μm, dusting properties will be high, and if the average particle size exceeds 1000 μm, the appearance will be poor.

The total amount of heavy sodium carbonate and light sodium carbonate is generally 10 to 60% by weight, preferably 15 to 55% by weight in the granular nonionic detergent composition.
%, More preferably 20 to 50% by weight. 10
If the amount is less than 60% by weight, it is difficult to add other components. (C)
The weight ratio (c) / (d) of the component and the component (d) is generally 1
/ 2 to 19/1, preferably 1/2 to 3/1, more preferably 1/2 to 3/2. If the ratio is less than 1/2, the granulation property deteriorates, the adhesion of the granulation device increases, and the load on the device increases. On the contrary, if it exceeds 19/1, the adhesion of the granulation device increases, and the load on the device increases, Coarse particles increase.

In the method of the present invention, (b)
After mixing the components (c) and (d), the component (a) is added to the mixture, and the mixture is stirred and granulated, whereby:
A granular nonionic detergent composition is obtained. By adding the nonionic surfactant (a) to the mixture consisting of the components (b), (c) and (d), the granulation speed can be increased while maintaining the fluidity of the particles in the stirring granulation. (That is, the speed of granulation can be made an appropriate speed that is easy to control).

In the method of the present invention, the granular nonionic detergent composition may contain, in the detergent composition, a clay mineral and a small amount of components such as a fluorescent agent, an enzyme, a bleaching agent, an antistatic agent, a surface modifier, and an anionic interface. An activator, a re-staining inhibitor, a bulking agent, a fragrance, a reducing agent, and the like can be blended. These components may be blended in the granulation step, or may be added to the detergent particles obtained in the granulation step. You may mix.

The following are specific examples of the components to be mixed in the detergent. (1) Clay minerals: montmorillonite, nontronite,
Beiderite, pyrophyllite, saponite, hectorite, stevensite, talc, etc. (2) Fluorescent agent: bis (triazinylamino) stilbene disulfonic acid derivative, bis (sulfostyryl) biphenyl salt [Tinopearl CBS] and the like. (3) Enzymes: lipase, protease, cellulase, amylase and the like. (4) Bleaching agents: percarbonates, perborates, etc. (5) Antistatic agents: cationic surfactants such as dialkyl-type quaternary ammonium salts. (6) Surface modifier: fine calcium carbonate, fine zeolite, polyethylene glycol and the like. (7) Anionic surfactant: α-sulfofatty acid methyl ester salt, linear alkyl benzene sulfonate, α-olefin sulfonate, alkyl sulfate, fatty acid soap and the like. (8) Anti-redeposition agent: cellulose derivatives such as carboxymethyl cellulose. (9) Extenders: sodium sulfate, potassium sulfate, sodium hydrochloride and the like. (10) Fragrance: (11) Reducing agent: sodium sulfite, potassium sulfite, etc.

In the stirring granulation, as a stirring granulator,
A high-speed mixer (manufactured by Fukae Kogyo Co., Ltd.), a sugi mixer (manufactured by Hosokawa Micron Co., Ltd.), and a reedige mixer (manufactured by Matsubo Co., Ltd.) have a stirring blade inside the granulator. A mixture of the above-mentioned components (b), (c) and (d) and a nonionic surfactant and further optionally added to an internal stirring type granulator having a clearance of 30 mm or less between the inner wall of the granulator and the granulator. A granular nonionic detergent composition can be produced by introducing and treating a component which can be used.

The temperature of the stirring granulation is generally 20 to 60 ° C.,
Preferably 30 to 50 ° C, more preferably 35 to 50 ° C
It is. If the temperature is lower than 20 ° C., granulation is difficult to proceed, which is not preferable. On the other hand, if the temperature is higher than 60 ° C., on the contrary, adhesion to the granulator occurs, and the load tends to be excessive, which is not preferable. In addition, the treatment time in the stirring granulation treatment is usually 1 to 10 minutes, preferably 2 to 8 minutes.
Minutes.

By such agitation granulation, detergent particles having a bulk density of 0.3 to 1.2 g / ml, preferably 0.5 to 1 g / ml can be obtained by the method of the present invention. Further, the detergent particles thus produced may be subjected to a coating treatment by adding a coating agent in a rolling drum, for example. Thereby, the flow characteristics can be improved. As the coating agent, JIS200
Inorganic powders having a mesh sieve passing amount of 50% or more are suitable. As materials, for example, carbonates such as sodium carbonate and calcium carbonate, and silicates such as amorphous silica, calcium silicate, and magnesium silicate And aluminosilicates such as zeolite. The coating agent is generally used in the granular nonionic detergent composition of the present invention in an amount of 0.5 to 15% by weight, preferably 1 to 10% by weight.

Further, to the detergent particles thus produced, components such as alkali builder, other detergent builder, clay mineral, fluorescent agent, enzyme and fragrance can be added. The obtained granular nonionic detergent composition generally has an average particle size of 300 to 3000 μm, preferably 350 to 200 μm.
0 μm, particularly preferably 400 to 1000 μm.

[0023]

The present invention will be described below in more detail with reference to examples and comparative examples. In the examples and comparative examples, each sample was evaluated by the following test methods.

<Evaluation of Granulation Property> In consideration of productivity and controllability in a batch type apparatus, the granulation time is preferably between 1 and 20 minutes. Therefore, the sample during granulation was observed, and if the time required for granulation was too short, it was difficult to control granulation, and if it was too long, the production capacity was inferior. ◎: Time to reach average particle diameter of 400 μm is 5 to 15
Minutes ○: Time to reach an average particle diameter of 400 μm is 1 to 5 minutes or 15 to 20 minutes ×: Time to reach an average particle diameter of 400 μm is less than 1 minute or more than 20 minutes

<Fluidity test> The angle of repose at room temperature was measured by the discharge method based on JIS Z2502, and evaluated according to the following criteria. ：: Less than 60 ゜ △: More than 60 ゜ and less than 65 ゜ ×: More than 65 ゜

<Raw Materials> The nonionic surfactants, aluminosilicates, heavy sodium carbonate and light sodium carbonate used in the examples and comparative examples are as follows.

Component (a): Nonionic surfactant C ₁₂ H ₂₅ O (CH ₂ CH ₂ O) ₇ H [polyoxyethylene lauryl ether obtained by adding an average of 7 moles of ethylene oxide to Connol 20P manufactured by Shin Nippon Rika Co., Ltd.] Component (b): Aluminosilicate P-type zeolite (manufactured by Crossfield) Component (c): Sodium carbonate A Heavy sodium carbonate [Granular ash manufactured by Asahi Glass Co., Ltd.] Component (d): Sodium carbonate B Light sodium carbonate [ Light ash manufactured by Asahi Glass Co., Ltd.]

The following optional components were used. White carbon: amorphous silica [Tokuseal N manufactured by Tokuyama Corporation] Glauber's salt: sodium sulfate [manufactured by Shikoku Chemicals Co., Ltd.] Fluorescent agent: 4,4′-bis (2-sulfostyryl) biphenyl disodium (Ciba Specialty) Chemicals Co., Ltd. Tinopearl CBS-X) Enzyme: lipase / protease / cellulase / alcalase = 1/1/1/1 mixture Perfume: having the composition shown in Table 1.

[0029]

[Table 1] Component content (parts by weight) ────────────────────────────────── 3,7- Dimethyl-1,6-octadien-3-ol 80 3,7-dimethyl-1,6-octadien-3-yl-acetate 60 3,7-dimethyl-6-octen-1-ol 40 β-phenylethyl alcohol 50 p-tert-butyl-α-methylhydrocinnamic aldehyde 70 α-methyl-p-isopropylphenylpropionaldehyde 60 α-n-amylcinnamic aldehyde 20 α-n-hexylcinnamic aldehyde 60 7-acetyl-1,1 , 3,4,4,6-hexamethyltetrahydronaphthalene 80 3- (5,5,6-trimethyl-norbalnan-2-yl) cyclohexane-1-o Reference Signs List 20 belt fix 30 2-ethyl-4- (2,2,3-trimethyl-3-cyclopent-1-yl) -2-butan-1-ol 10% 10 α, α-dimethyl-p-ethylhydrocinamic Aldehyde 40 2,4-dimethyl-3-cyclohexene-1-carboxaldehyde 10 cis-3-hexenol 10 2-trans-3,7-dimethyl-2,6-octadien-1-ol 30 n-decylaldehyde 5 10- Undecene-1-al 5 methylnonylacetaldehyde 5 4- (4-hydroxy-4-methylpentyl) -3-cyclohexene-1-carboxaldehyde 30 naphthalene-2-acetyl-1,2,3,4,6,7, 8-octahydro-2,3,8,8-tetramethyl 30 5- (2-methylene-6 , 6-Dimethyl-cyclohexyl) -4-pentan-3-one 50 2-methoxy-4-propenylphenol 20 allylcyclohexanepropionate 10 6,7-dihydro-1,1,2,3,3-pentamethyl-4 (5H) -Indanone 5 p-Propenylphenyl methyl ether 5 Methyl-2-aminobenzoate 5 Lemon oil 30 Orange oil 20 Lavandin oil 20 Patchouli oil 10 3,7-Dimethyl-2,6-octadienal 30 Methyldihydrojasmo Nate 50 Percentage of perfume components having a boiling point of 230 ° C. (1 atm) in the total perfume (wt%) 66

Examples 1 to 14 and Comparative Examples 1 to 4 Zeolite, granulated ash and light ash in the amounts shown in Table 2 below were charged into a Lodige mixer [M-20, manufactured by Matsubo Co., Ltd.] (200 rpm), chopper (6000 rpm)
The stirring of m) was started. 20 to 40 seconds after the start of stirring, a nonionic surfactant was added for 3 to 6 minutes, followed by stirring and granulation. During the stirring, sampling was conducted over time, and when the average particle diameter became 300 to 500 μm, 5% of zeolite was added as a fluidity improver, and finally, other components such as white carbon, mirabilite, enzymes, fragrances and the like were added. Was added to obtain a granular nonionic detergent composition (average particle size: 350 to 550 μm). Table 2 shows the evaluation results.

Embodiments 15 and 16 In Embodiment 1, a high-speed mixer [manufactured by Fukae Kogyo Co., Ltd.] is used instead of the Lodige mixer (Example 15).
Alternatively, a granular nonionic detergent composition was obtained in the same manner as in Example 1 except that a sugar mixer [manufactured by Hosokawa Micron Corporation] (Example 16) was used. Table 2 shows the evaluation results.

[0032]

[Table 2- (1)]

[0033]

[Table 2- (2)]

From the results in Table 2, according to the method of the present invention,
It can be seen that the granulation speed can be increased while the fluidity of the particles is kept good, the formation of coarse particles is extremely small, the amount of adhesion to the device is small, and the load on the device can be kept low.

[0035]

According to the method of the present invention, the granulation rate can be increased while maintaining the fluidity of the particles, and the formation of coarse particles is extremely small, because of the above constitution.
Moreover, the amount of adhesion to the device can be kept small and the load on the device can be kept low.

Continued on the front page (51) Int.Cl. ⁶ Identification code FI C11D 3/12 C11D 3/12 11/00 11/00

Claims (1)

[Claims] (1) at least (a) a nonionic surfactant,
It contains (b) aluminosilicate, (c) heavy sodium carbonate and (d) light sodium carbonate, and the total amount of components (c) and (d) is (c) + (d) = 10 to 60% by weight. In producing a granular nonionic detergent composition having a weight ratio (c) / (d) = 1/2 to 19/1, (b)
(C) and (d) a method for producing a granular nonionic detergent composition, which comprises mixing the components, adding the component (a), and stirring and granulating.