JPH11310799A - Method for controlling granule size of granular nonionic detergent and production of granular nonionic detergent composition using the same - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method for controlling the granule size in the step of agitation granulation in order to obtain a granular nonionic detergent which has a narrow granule size distribution, is hardly classified, and is hardly sticky and a process for producing a granular nonionic detergent compsn. using the same. SOLUTION: This method for controlling the granule size is characterized in that in granulating by adding, under stirring, a nonionic surfactant to a powder at least contg. a detergent builder, (a) the first step of adding a part of the nonionic surfactant at a certain rate and (b) the second step of adding the rest of the nonionic surfactant at a rate of 1/2 or lower of the first step are included.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for controlling the particle size of a granular nonionic detergent and a method for producing a granular nonionic detergent composition using the same. More specifically, the present invention relates to a method for obtaining particles having a narrow particle size distribution in stirring granulation of a nonionic detergent. The present invention relates to a control method and a production method for obtaining a granular nonionic detergent composition having a narrow particle size distribution using the method.

[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 deteriorate.

Therefore, in order to improve the flowability and caking resistance of the nonionic detergent composition, the weight ratio and total amount of heavy / light sodium carbonate are specified and added (Japanese Patent Laid-Open No. 2-229894). The nonionic activator / builder mixture is stirred and granulated, and the granulated material is further mixed with a fine powder to coat the surface of the granulated material with the fine powder (JP-A-5-2092).
No. 00), a nonionic surfactant, a nonionic gelling agent and an oil-absorbing carrier are stirred and granulated (JP-A-9-87694).
And the like have been proposed. However, when the agitation granulation is performed, there are disadvantages that the appearance is poor due to a wide particle size distribution, and that classification is easy at the time of filling.

[0004]

SUMMARY OF THE INVENTION Accordingly, the present invention has been made in view of the above-mentioned circumstances of the prior art, and in a stirring granulation method, a granular nonionic detergent which has a narrow particle size distribution, is difficult to classify, and has little adhesion. It is an object of the present invention to provide a particle size control method for obtaining a nonionic detergent composition, and a method for producing a granular nonionic detergent composition which has a narrow particle size distribution, is difficult to classify, and has little adhesion using the particle size control method.

[0005]

Means for Solving the Problems As a result of intensive studies, the present inventors have divided the addition of the nonionic surfactant in the stirring granulation into two stages, and in the second stage, the addition of 1/1 / in the first stage. It has been found that the above object is achieved by adding at a rate of 2 or less, and the present invention has been achieved.

That is, according to the present invention, first, when a nonionic surfactant is added to a powder containing at least a washing builder under stirring to granulate, a) a portion of the nonionic surfactant A second step of adding the remaining nonionic surfactant at a rate equal to or less than の of the first step, and a second step of adding the remaining nonionic surfactant at a constant rate. A control method is provided. Secondly, in the production of a granular nonionic detergent composition containing at least a nonionic surfactant and a washing builder, a method for producing a granular nonionic detergent composition, characterized by using the particle size control method described in the first aspect, 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 is generally contained in the granular nonionic detergent composition in an amount of 10 to 40% by weight, more preferably 12 to 35% by weight, particularly preferably 15 to 30% by weight. If the amount is less than 10% by weight, the obtained detergent particles have a low nonionic surfactant concentration as well as a low bulk density. This is not preferable because it results in a contradiction to compactness, and 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 it becomes difficult to produce stably. Is not preferred.

In the method of the present invention, a builder which is usually used in detergents is used as a washing builder. For example, chelate builders such as zeolite, tripolyphosphate, citrate, succinate, polyacrylate, acrylic acid-maleic acid copolymer, EDTA,
Alkaline builders such as alkali metal carbonates (such as sodium carbonate and potassium carbonate), alkali metal silicates (such as sodium silicate and potassium silicate), and layered polysilicates (such as macatite and kanemite) are included. In addition, powders such as sodium sulfate, silica, calcium carbonate, starch, metal soap and the like can be used.

The washing builder is stirred with the nonionic surfactant in such an amount that it is generally incorporated in the particulate nonionic detergent composition in an amount of from 40 to 80% by weight, preferably from 40 to 75% by weight, more preferably from 50 to 70% by weight. Granulated. If the blending amount of the washing builder is less than 40% by weight, the fluidity is lowered, and if it is more than 80% by weight, the dusting property is deteriorated.

The method for controlling the particle size of a granular nonionic detergent according to the present invention is characterized in that, as described above, a nonionic surfactant is added to a powder containing at least a washing builder while stirring to granulate the powder. A first step of adding a nonionic surfactant at a constant rate; and b) a second step of adding the remaining nonionic surfactant at a rate of 1/2 or less of the first step.

That is, in the particle size control method of the present invention,
The nonionic detergent is granulated by adding the nonionic surfactant to the washing builder-containing powder in two stages under stirring, and by setting the addition speed to 1/2 or less at the time of the second stage addition. The particle size distribution of the particles can be sharpened.

In carrying out the present control method, in the first step, usually, 20 to 8 of nonionic surfactants are used.
0% by weight is added. Preferably 30-70% by weight,
More preferably, it is 40 to 60% by weight. 20 added
If it is less than 80% by weight, the particle size distribution tends to be wide, and conversely 80%
If the amount is more than the weight percentage, coarse particles are easily generated. In the second step, the remainder of the nonionic surfactant is added at a rate of one half or less of the first step. Preferably it is 2/5 or less, more preferably 1/4 or less. First step 2
Addition at a rate exceeding one part widens the particle size distribution.

Next, a method for producing the granular nonionic detergent composition of the present invention utilizing the above-mentioned method for controlling the particle size of the granular nonionic detergent will be described. In the production method of the present invention, a nonionic surfactant is added to the powder containing the cleaning builder under stirring according to the particle size control method, and the mixture is stirred and granulated to produce a granular nonionic detergent composition.

In the production method of the present invention, an oil-absorbing carrier and a nonionic gelling agent, which are blended to prevent exudation of nonions under high temperature and high humidity, and to improve the fluidity and the caking resistance of detergent particles, are stirred and granulated. Very occasional addition is highly preferred. Preferred oil-absorbing carriers include JIS-K622
0 Oil absorption expressed by the test method is 80 ml / 100 g or more, preferably 150 to 600 ml / 100 g, and the bulk density is less than 0.1 g / cc, preferably 0.001 to 0.08 g / A substance that is cc is preferably used. Such oil-absorbing carriers include, for example, amorphous silicic acid, amorphous calcium silicate, amorphous aluminosilicate, magnesium silicate, magnesium carbonate, calcium carbonate, spinel, mullite, cordierite, starch decomposed product, etc. And these can also be used as a mixture.

Preferred nonionic gelling agents include, for example, 12-hydroxystearic acid, dibenzylidene sorbitol, lithium stearate, aluminum palmitate, lithium 2-ethylhexanoate,
Aluminum 2-hydroxystearate, dibutylamide lauroylglutamate, stearylamide lauroylglutamate, dicaproyllysine laurylamide, dicaproyllysine lauryl ester, lauroylphenylalanine laurylamide, polystyrene polybutadiene block copolymer, polyacrylamide-
Examples thereof include an isoparaffin mixture, a block copolymer of a polystyrene block and a polybutadiene block, dextrin palmitate, and the like, or a mixture thereof.

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 stirring granulation process, or the detergent obtained in the stirring granulation process. You may mix | blend with a particle.

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.), a reedige mixer (manufactured by Matsubo Co., Ltd.), etc. have a stirring blade inside the granulator. A washing builder and optionally addable components are introduced into an internal stirring type granulator having a clearance of 30 mm or less between the inner wall of the granulator and a nonionic surfactant at a two-stage rate. A granular nonionic detergent composition can be produced by adding and granulating.

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.

Furthermore, components such as enzymes and fragrances can be added later to the detergent particles thus produced.
The resulting granular nonionic detergent composition generally has an average particle size of 3
00-3000 μm, preferably 350-2000 μm
m, particularly preferably 400 to 1000 μm.

[0027]

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.

<Particle Size Distribution> The weight distribution was measured using a JIS sieve. <Classification> 400 g of detergent was placed in a 500 ml hopper, the outlet of the hopper was inserted into a filling container, and after opening the outlet, half of the detergent was placed in the filling container, and the particle size distribution of the detergent in the container was measured.

<Raw Materials> The nonionic surfactants and powder raw materials used in Examples and Comparative Examples are as follows. Nonionic surfactant C ₁₂ H ₂₅ O (CH ₂ CH ₂ O) ₇ H [Polyoxyethylene lauryl ether obtained by adding an average of 6 moles of ethylene oxide to Connol 20P manufactured by Shin Nippon Rika Co., Ltd.] Powder material (1) Powder material A A-type zeolite [Silton B manufactured by Mizusawa Chemical Co., Ltd.] (2) Powdered raw material B Amorphous silica [Tokuseal N manufactured by Tokuyama Corporation] (3) Powdered raw material C 1/1 of light sodium carbonate and heavy sodium carbonate Mixture of Asahi Glass Co., Ltd.

The following optional components were used. Enzyme: mixture of lipase / protease / cellulase = 1/1/1 (Novo) PC: sodium peroxide [manufactured by Mitsubishi Chemical Corporation] LS: layered silicate (SKS-6 manufactured by Hoechst) CZ: zeolite A [ Mizusawa Chemical Co., Ltd. Shilton B]

Examples 1 to 7 and Comparative Examples 1 and 2 Powder materials A, B and C in the amounts shown in Table 1 were charged into a Lodige mixer [M-20, manufactured by Matsubo Co., Ltd.]. These components were mixed for 30 seconds under stirring with a chopper (200 rpm) and a chopper (6000 rpm). Next, a nonionic surfactant was added at two stages shown in Table 1 and granulated until the average particle diameter became 500 μm. Finally, Table 1
The components (enzyme, PC, LS, CZ) in the amounts shown in (1) were added and mixed for 30 seconds to obtain a granular nonionic detergent composition (average particle size: 500 μm). The evaluation results of the obtained nonionic detergent composition are shown in Table 1 (Example) and Table 2 (Comparative Example).

Comparative Example 3 Powder raw materials A, B, and C in the amounts shown in Table 1 were charged into a Lodige mixer [M-20, manufactured by Matsubo Co., Ltd.], and a main shaft (200 rpm) and a chopper (6000 rpm) were used. The components were mixed for 30 seconds with stirring. Next, the entire amount of the nonionic surfactant shown in Table 1 was added at a constant rate, and the mixture was granulated until the average particle diameter became 500 μm. Finally, the amounts of the optional components (enzyme, PC, LS, C
Z) was added and mixed for 30 seconds to obtain a granular nonionic detergent composition (average particle size: 500 μm). Table 2 shows the evaluation results of the obtained nonionic detergent compositions.

[0033]

[Table 1]

[0034]

[Table 2]

From the results of Tables 1 and 2, according to the method of the present invention, it is possible to obtain a granular nonionic detergent composition having a narrow particle size distribution and difficult to classify, even though the agitation granulation method is employed. We can see that we can do it.

[0036]

According to the method of the present invention, because of the above-mentioned structure, despite the adoption of the stirring granulation method,
A granular nonionic detergent composition having a narrow particle size distribution, difficult to classify, and little adhesion is obtained.

Claims (2)

[Claims] When a nonionic surfactant is added to a powder containing at least a washing builder under stirring to granulate, a) a first step of adding a part of the nonionic surfactant at a constant rate; B) a second step of adding the remaining nonionic surfactant at a rate equal to or less than の of the first step, and a second step of controlling the particle size of the granular nonionic detergent. 2. A method for producing a granular nonionic detergent composition, comprising using the particle size control method according to claim 1 in producing a granular nonionic detergent composition containing at least a nonionic surfactant and a cleaning builder. .