JP3192470B2 - Method for producing granular composition containing nonionic activator - Google Patents

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 composition containing a nonionic activator, which has a high bulk density and is excellent in powder flow characteristics and non-caking properties.

[0002]

2. Description of the Related Art A method for producing a granular detergent composition containing a nonionic activator includes:
A production method has been proposed in which a nonionic activator is blended into a detergent slurry and this is spray-dried to obtain a granular detergent composition. However, in this method, the equipment cost is large, consumes a large amount of energy, and the nonionic activator is decomposed by hot air during drying, generating pollutants, reducing the content of nonionic activator, and reducing the properties of the activator. Problems such as changes may occur. In order to solve these problems, the type and amount of the nonionic activator are limited (JP-A-61-85499), and additives that do not contribute to cleaning are blended (JP-A-56-22394). No.).

[0003] Japanese Patent Publication No. 60-21200 proposes a production method in which builder base beads are prepared by spray drying and a nonionic activator is supported on the base beads.
However, in this method, since the anhydrous phosphate builder salt is used as a base material, the method is limited to only a phosphorus-based particulate composition, and a phosphorus-free particulate composition cannot be produced. In addition, the operation of producing a substrate bead having a porous outer surface and a skeleton internal structure is complicated.

In Japanese Patent Publication No. 61-21997, a washing active salt is hydrated and wetted by using an agglomerator and the like, and then stirred in a closed vessel. A method for producing a granular detergent which does not cause caking even when stored for a long period of time by impregnating and drying is proposed. However, in this method, a drying step is required after granulation in order to impregnate the active agent into the agglomerate of the washing active salt which has been hydrated and wet, and the step is not simple. )
Has the problem that it is complicated.

In Japanese Patent Application Laid-Open No. 3-26795, an agglomeration forming apparatus is used to form a zeolite agglomerate from a zeolite and a filler with a binder containing water, and a detergent containing the agglomerate and a surfactant. A method for producing a granular detergent having good fluidity, solubility and dispersibility by forming a detergent agglomerate and drying the component has been proposed. However, in order to obtain a detergent agglomerate, at least five operations are required, and the operation in production is complicated.

[0006] In JP-A-62-263299, a nonionic activator and a builder are uniformly kneaded to form a solid detergent,
Then, a production method for obtaining a granular detergent composition by crushing has been proposed. However, this method has a problem that it is difficult to obtain a nonionic activator-containing granular composition having good flowability, and that an undesirably large amount of fine powder is generated.

In Japanese Patent Application Laid-Open No. 61-89300, after mixing a water-soluble powder and silica powder, a nonionic activator is sprayed on the mixture, and then zeolite or calcium carbonate powder is added. A method for producing a nonionic surfactant-containing granulate is described. However, in this method, a high-bulk-density nonionic surfactant-containing granulated product cannot be produced because the granulation is performed by a drum-type granulator in which a drum rotates. In addition, all of these methods have a low content of a nonionic activator, have various restrictions on production, and the production method is complicated.

Accordingly, it is an object of the present invention to provide a method for easily producing a granular composition containing a nonionic active agent having a high bulk density. It is a further object of the present invention to provide a method for producing a nonionic activator-containing granular composition having excellent powder flow properties and non-caking properties.

[0009]

Means for Solving the Problems The inventors of the present invention have conducted intensive studies to solve the above-mentioned problems, and as a result, have prepared a blended component containing a porous oil-absorbing carrier and a nonionic activator into a specific stirring-type mixer. The present invention has found that a granulated composition containing a nonionic activator can be produced simply and energy-saving by mixing the obtained granulated product and fine powder and coating the surface of the granulated product. Was completed. That is, the preparation of the nonionic active agent-containing granular composition of the present invention, 1. the pore volume by a mercury intrusion porosimetry 100~600cm ³ / 100g, BET
The specific surface area is 20 to 700 m ² / g according to the method, and the oil absorption in JIS K 5101 is 1
15 to 70 parts by weight of a porous oil-absorbing carrier that is 00 ml / 100 g or more,
A mixing component containing the nonionic activator in a proportion of 30 to 85 parts by weight has a stirring shaft equipped with a stirring blade at the center of the inside, and when the stirring blade rotates, a clearance is provided between the stirring blade and the vessel wall. By stirring and mixing with a stirring type mixer to form,
A powder adhesion layer is formed on the wall of the stirrer-type mixer, granulated while increasing the bulk density of the powder with a stirring blade, and then the obtained granulated material and fine powder are mixed, and the granulated material is mixed. The surface is coated with the fine powder to obtain a granular composition having a bulk density of 0.6 to 1.2 g / ml.

Further, a preferred embodiment of the present invention is as follows:
As shown in FIG. 2. After granulation, fine powder is added to 0.5 to 100 parts by weight of granulated material.
3. The method for producing a nonionic activator-containing granular composition according to claim 1, wherein 30 parts by weight are added to coat the surface of the granulated product. 3. The method for producing a nonionic activator-containing granular composition according to item 1, wherein the average clearance of the agitated mixer is 1 to 30 mm. 4. The method for producing a nonionic activator-containing granular composition according to item 1, wherein the granulation is performed under the condition that the Froude number based on the rotation of the stirring blade of the stirring mixer is 1 to 4. 5. The method for producing a nonionic activator-containing granular composition according to claim 1, wherein the granulation is performed for a granulation time of 0.5 to 20 minutes. 6. The method for producing a nonionic activator-containing granular composition according to item 1, wherein the granulation is performed by a stirring mixer having a stirring shaft at the center of the horizontal cylinder and a stirring blade on the stirring shaft. 7. The method for producing a nonionic activator-containing granular composition according to item 1, wherein the granulation and the surface coating of the granulated material with the fine powder are performed by the same apparatus.

8. The nonionic surfactant is a polyoxyethylene alkyl ether having an average ethylene oxide addition mole number of 5 to 15 of a linear or branched, primary or secondary alcohol having 10 to 20 carbon atoms. A method for producing the nonionic activator-containing granular composition according to claim 1. 9. The method for producing a nonionic activator-containing particulate composition according to item 1, wherein the porous oil-absorbing carrier is an amorphous silica derivative. 10. The method for producing a nonionic activator-containing particulate composition according to item 9, wherein the amorphous silica derivative is an amorphous aluminosilicate. 11. The method for producing a nonionic activator-containing granular composition according to item 1, wherein the fine powder is a fine powder having an average primary particle diameter of 10 μm or less.

Item 12. The fine powder having an average primary particle size of 10 μm or less is one or a mixture of two or more selected from silicate compounds such as aluminosilicates and amorphous silica derivatives. A method for producing a granular composition containing a nonionic activator.

13. The first particle having an average particle size of 250 to 800 μm.
The method for producing a nonionic activator-containing granular composition according to the above item. 14. The process for producing a nonionic activator-containing particulate composition according to item 1, which has a fluidity such that the fluidity time is 10 seconds or less. 15. The method for producing a nonionic activator-containing granular composition according to item 1, which has a caking property of a sieve passing rate of 90% or more.

In the practice of the present invention, the method of charging the blended components into the stirring type mixer is not particularly limited, and various methods such as the following (a) to (d) are employed. be able to. The methods (a) to (c) are performed while rotating the stirring blade of the stirring mixer. (A) First, a porous oil-absorbing carrier is charged into a stirring-type mixer, and then a nonionic activator is added. (B) Charge the porous oil-absorbing carrier and the nonionic activator little by little into a stirring mixer. (C) After a part of the porous oil-absorbing carrier is charged into the stirring mixer, the remaining porous oil-absorbing carrier and the nonionic activator are charged little by little into the stirring mixer. (D) A mixture obtained by previously mixing a porous oil-absorbing carrier and a nonionic activator is charged into a stirring-type mixer. Among these methods, it is particularly preferable to put a porous oil-absorbing carrier into a stirring mixer, add a nonionic activator, and perform compaction and tumbling granulation. The nonionic activator is preferably supplied by spraying. The porous oil-absorbing carrier used in the present invention, the pore volume of the mercury porosimetry 100 ~600cm ^3/10
0 g, specific surface area by BET method is 20-700 m ² / g, and JIS K 51
Oil absorption at 01 is 100ml / 100g or more. This oil absorption is the amount of boiled linseed oil absorbed by the porous oil-absorbing carrier based on the method described in JIS K 5101. The average particle size is preferably 0.5 to 500 μm, more preferably 1 to 200 μm, as aggregated particles. If the average particle size of the porous oil-absorbing carrier is 100 μm or more, use a standard JIS Z 8801 sieve.
It is measured from the weight fraction according to the size of the sieve after shaking for a minute. When the average particle size is 100 μm or less, the average particle size can be measured by a method using light scattering, for example, by using a particle analyzer (manufactured by Horiba, Ltd.). The amount of the porous oil-absorbing carrier is preferably 15 to 70 parts by weight. If the amount is less than 15 parts by weight, the flow characteristics and the non-caking properties decrease, whereas if it exceeds 70 parts by weight, the effective concentration of the nonionic activator decreases, which is not preferable. The following are examples of such a porous oil-absorbing carrier.

1) Amorphous silica derivative A derivative having silica as a main skeleton is preferable. As the second component, Al ₂ O ₃ , M ₂ O (where M is an alkali metal), MeO (where Me is an alkaline earth Metals) are preferred. Further, not only two elements but also three elements, four elements and the like are preferably used. Specifically, the following substances (i) to (iii) are exemplified. (i) Examples of those containing silica as a main component include Tokusil NR, PR, AL-1 manufactured by Tokuyama Soda Co., Ltd., Nip Seal NS, Nip Seal NA-R, Nip Seal ES, manufactured by Nippon Silica Co., Ltd., and Degussa SIPERNAT 22, SIPERNAT 50
, DUROSIL, ZEOSIL 45, TIXOSIL 3 manufactured by Korea and France
8. Carplex 100 manufactured by Shionogi Pharmaceutical Co., Ltd. (ii) As those containing calcium silicate as a main component,
HUBERSORB ^R 600 manufactured by Huber. (iii) As those having an aluminosilicate as a main component,
AluminumSilicate P820 manufactured by Degussa, and TIXOLEX 25 manufactured by Korea-France Chemical Company. Particularly, those represented by the following general formula are preferred. Further, these are characterized in that they have ion exchange ability. (1) x (M ₂ O) · Al ₂ O ₃ · y (SiO ₂ ) · w (H ₂ O) (where M represents an alkali metal such as sodium or potassium, and x, y and w are as follows: Represents the number of moles of each component within the numerical range of 0.2 ≦ x ≦ 2.0 0.5 ≦ y ≦ 10.0 w (any positive number including 0) (2) x (MeO) · y (M ₂ O) ) ・ Al ₂ O ₃・ z (SiO ₂ ) ・
w (H ₂ O) (Me in the formula represents an alkaline earth metal such as calcium and magnesium, M represents an alkali metal such as sodium and potassium, and x, y, z, and w are within the following numerical ranges. 0.001 ≤ x ≤ 0.1 0.2 ≤ y ≤ 2.0 0.5 ≤ z ≤ 10.0 w: any positive number including 0) 2) Calcium silicate Fluorite R manufactured by Tokuyama Soda Co., Ltd. No. 3) Calcium carbonate Callite KT manufactured by Shiroishi Kogyo Co., Ltd. may be mentioned. 4) Magnesium carbonate Magnesium carbonate TT manufactured by Tokuyama Soda Co., Ltd. 5) Pearlite (Perlite) Perlite 4159 manufactured by Daikarite Orient Co., Ltd. is exemplified. Among these porous oil-absorbing carriers, amorphous silica derivatives are more preferred, and amorphous aluminosilicates are particularly preferred.

In the present invention, the amount of the nonionic activator is from 30 to 85 parts by weight, preferably from 40 to 75 parts by weight, per 100 parts by weight of the granular composition.
Parts by weight. If the added amount of the nonionic activator is less than 30 parts by weight, an effective concentration of the nonionic activator cannot be obtained, while if it exceeds 85 parts by weight, optimal flow characteristics cannot be obtained, which is not preferable.

The nonionic activator used in the present invention is not particularly limited, but is a liquid or paste at 40 ° C.
Further, those having an HLB in the range of 9.0 to 16.0 are excellent in removing stains, foaming, and removing bubbles, and thus are preferable. HLB here
Is defined as follows. That is, JTDvies
and EKRideal, Interfacial Phenomena, Academic Pr
According to ess, New York, 1963, Page 371-383, it was determined as HLB = 7 + Σ (number of hydrophilic groups) −Σ (number of hydrophobic groups). Here, the radix of each atomic group used for HLB calculation is as shown in Table 1.

[0018]

[Table 1]

Specific examples of the nonionic activator include polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene sorbite fatty acid ester, polyethylene glycol fatty acid ester,
Polyoxyethylene polyoxypropylene alkyl ether, polyoxyethylene castor oil, polyoxyethylene hydrogenated castor oil, polyoxyethylene alkylamine,
Examples include glycerin fatty acid esters, higher fatty acid alkanolamides, alkyl glycosides, and alkylamine oxides. Above all, carbon number as main nonionic activator
10 to 20, preferably 10 to 15, more preferably 12 to 14 linear or branched primary or secondary alcohol, ethylene oxide average addition mole number of 5 to 15, preferably 6 to 12,
More preferably, it is desirable to use 6 to 10 polyoxyethylene alkyl ethers. In addition, the polyoxyethylene alkyl ether generally contains a large amount of an alkyl ether having a low addition mole number of ethylene oxide, and a polyoxyethylene alkyl ether having a 0 to 3 mole addition product of 35% by weight or less, preferably 25% by weight or less. It is desirable to use.

In order to promote granulation at the time of granulation, it is also possible to add a binder simultaneously with the addition of the nonionic activator or after the nonionic activator is added. Examples of the binder that can be used in the present invention include carboxymethyl cellulose, polyethylene glycol, water-soluble polymer solutions such as polycarboxylates such as sodium polyacrylate, polyoxyethylene alkyl ether, fatty acid monoethanolamide, fatty acid diethanolamide, and the like. Nonionic substances, fatty acids, aqueous sodium silicate solutions, water and the like can be mentioned. The amount of the binder is preferably from 0.1 to 10 parts by weight, particularly preferably from 0.5 to 5 parts by weight, per 100 parts by weight of the granulated raw material (components).

In order to prevent oxidation of the nonionic activator, the following antioxidants may be added. As antioxidants, tertiary butylhydroxytoluene, 4,4′-butylidenebis- (6-tert-butyl-3-methylphenol), 2,2 ′
-Butylidenebis- (6-tert-butyl-4-methylphenol), monostyrenated cresol, distyrenated cresol, monostyrenated phenol, distyrenated phenol, 1,1'-bis- (4-hydroxyphenyl) cyclohexane, etc. No.

In the practice of the present invention, a fine powder is added as a surface modifier to coat the surface of the granulated material in order to improve fluidity and non-caking properties after granulation. Fine powder is
If it is added in the initial or middle stage of granulation, it is taken into the inside of the granulated product and does not contribute to the improvement of the fluidity and non-caking properties of the granulated product. The term "after granulation" as used herein refers to a point in time when the granulated product is granulated to a desired average particle size within a range of 250 to 1000 µm. The amount of fine powder to be added to the granulated material is 100 parts by weight of the granulated material.
It is preferably 0.5 to 30 parts by weight, more preferably 1 to 25 parts by weight. The fine powder preferably has an average primary particle size of 10 μm or less. As fine powder, aluminosilicate having an average primary particle size of 10 μm or less, silicon dioxide,
Bentonite, talc, clay, amorphous silica derivatives,
Inorganic fine powders such as silicate compounds having high ion exchange capacity of 100 to 500 (CaCO ₃ mg / g) (for example, silicate compounds of soda silica type and potassium silica type) can be used. The average particle size of the primary particles is 10 μm
The following metal soaps can be used as well. If the amount of the fine powder added to the granulated material is less than 0.5 part by weight, it is difficult to obtain a powder having good fluidity, while if it exceeds 30 parts by weight, the fluidity is reduced, dust is generated and consumption occurs. May impair the usability of the user. Average primary particle size is 10μm
The average particle diameter of the following fine powder is determined by a method using light scattering, for example, a particle analyzer (manufactured by Horiba, Ltd.)
And by microscopic observation.

The stirring type mixer used at the time of granulation in the present invention has a stirring shaft provided with stirring blades at the center of the inside thereof, and a clearance is provided between the stirring blades and the vessel wall when the stirring blades rotate. It is important to form Average clearance is 1
~ 30 mm is preferred. Examples of the stirring type mixer having such a structure include a Henschel mixer [manufactured by Mitsui Miike Kakoki Co., Ltd.] and a high speed mixer [Fukae Kogyo Co., Ltd.]
And a vertical granulator [manufactured by Powrex Corporation]. Particularly preferred is a horizontal mixing tank having a stirring shaft at the center of a cylinder, and a stirring blade attached to the shaft to mix powder. Mixers of the single type or continuous type, for example, Redige mixer [Matsuzaka Giken Co., Ltd.
And Blowshare Mixer (manufactured by Taiheiyo Kiko Co., Ltd.).

The apparatus used for mixing the granulated material and the fine powder and coating the surface of the granulated material with the fine powder is not particularly limited, and a known mixer can be used. Devices used during granulation are preferred. However, when performing surface coating, the above clearance may not be 1 to 30 mm.
As an operation method, granulation and surface coating may be performed by the same device, or may be performed by separate devices. Further, if an apparatus having a structure capable of continuously supplying the blending component (granulated raw material) and discharging the granulated material is used, one or both of the granulation and the surface coating can be continuously performed.

The purpose of using the stirring type mixer having the above-mentioned structure at the time of granulation is as follows. In the present invention, even if the compounded component of the present invention containing a nonionic activator having a weak binding force is granulated to form an adhesion layer on the wall of the mixer, the overpower (overload) of the mixer and the granulation Decrease (generation of coarse particles)
Granules having a high density can be produced without occurrence of the above. This phenomenon is considered as follows. The adhered layer formed by the compounding component (granulated raw material) containing the nonionic activator having a weak binding force has an adhered substance having a high pressure density due to the contact with the stirring blade on the stirring blade side. The deposit has as low a pressure density as possible, and therefore, this deposit has a moderate elasticity. For this reason, it becomes possible to take in the granulated raw material into the adhesion layer by the stirring effect, and the mixer is not overpowered. The granulated raw material taken in between the adhesion layer and the stirring blades is compacted and spheroidized by the rolling operation, and is separated from the adhesion layer. Furthermore,
This detached material is spheroidized by the rolling operation in the mixing section in the mixer. That is, it is presumed that in the mixer, the compacting and rolling granulation of the granulated raw material can be favorably performed by the consolidation action and the rolling operation in the adhesion layer portion and the rolling operation in the mixing portion. In order to perform such compaction and tumbling granulation, it is important that a clearance is formed between the wall of the mixer and the stirring blade when the stirring blade rotates, and the average of the clearance is one. Preferably, the average clearance is 3 to 10 mm. The average clearance is 1
When the thickness is less than mm, the deposit having a high pressure density becomes dominant in the deposit, and the mixer tends to be overpowered. On the other hand, if the average clearance exceeds 30 mm, the consolidation efficiency decreases, and the particle size distribution becomes broad. In addition, the granulation time is prolonged, and the productivity is reduced.

Preferred granulation conditions for performing such granulation are as follows. (1) Froude number = Fr The Froude number defined by the following formula is preferably from 1 to 4, and more preferably from 1.2 to 3. If the Froude number is less than 1, consolidation is not promoted, which is not preferable. Also 4
If the ratio exceeds the above range, the adhesion layer is not sufficiently formed, and the particle size distribution is undesirably wide. Fr = V / (R × g) ^0.5 where V: peripheral speed [m / s] of the tip of the stirring blade R: rotation radius [m] of the stirring blade g: gravitational acceleration [m / s ² ] (2) Granulation time The granulation time in batch granulation to obtain suitable granules and the average residence time in continuous granulation are from 0.5 to
It is preferably 20 minutes, more preferably 3 to 10 minutes. still,
If it is less than 0.5 minute, the granulation time is too short to control the granulation to obtain a suitable average particle size and bulk density, and the particle size distribution becomes broad. On the other hand, if it exceeds 20 minutes, the granulation time is too long and the productivity is reduced.

(3) Amount of Granulated Raw Material Charged into Stirred Mixer The charged amount is preferably 70% by volume or less of the total internal volume of the mixer, more preferably 15 to 40% by volume. 70% by volume
If the ratio exceeds the above, the mixing efficiency of the granulated raw material in the mixer is reduced, so that suitable granulation cannot be performed. (4) Temperature The mixer preferably has a structure provided with a jacket, and the temperature of the medium passing through the jacket is preferably 5 to 40 ° C, more preferably 10 to 20 ° C. By setting the temperature in this range, the compaction action and the rolling operation in the adhesion layer portion are promoted, the granulation time for obtaining a suitable granulated product is shortened, the productivity is improved, and the particle size distribution is sharpened. Further, the porous oil-absorbing carrier may be supplied at a normal temperature and the nonionic activator may be supplied at a molten temperature, and the temperature in the mixer need not be particularly controlled. The temperature of the granulated product is usually 30 to 60 ° C. depending on the temperature of the raw material, heat of stirring and the like.

By performing granulation under these conditions,
The above-mentioned consolidation action and rolling operation proceed, and it is possible to produce granules having a high bulk density. On the other hand, if a mixer such as a Nauta mixer or a V blender is used during granulation, an adhered layer of granulated raw material can be formed on the vessel wall, but in the adhered area, both compacted granulation and tumbling granulation are satisfied. Therefore, it is not possible to obtain a granulated material having a high bulk density.
The wall of the stirring mixer used for granulation in the present invention may be any one of the top, side, and bottom inside the mixer.

As the physical properties of the nonionic activator-containing granular composition according to the present invention, the following are suitable. (1) Bulk density: 0.6 to 1.2 g / ml, preferably 0.7 to 1.0 g / m
l (If it exceeds 1.2 g / ml, the solubility tends to deteriorate.) (2) Average particle size: 250 to 800 μm, preferably 300 to 600 μm
The μm average particle size is measured from the weight fraction based on the size of the sieve after vibrating for 5 minutes using a JIS Z 8801 standard sieve.
(If it is less than 250 μm, dust is generated, while if it exceeds 800 μm, the solubility tends to deteriorate.) (3) Fluidity: Flow time is 10 seconds or less (If it exceeds 10 seconds, the handling property of the granular composition is exceeded) (4) Caking property: The sieve passing rate is 90% or more (If it is less than 90%, caking occurs during storage, which is not preferable.) The average particle size of the granulated product after granulation is 250. The average particle diameter of the nonionic activator-containing granular composition of the present invention is preferably from 250 to 800 μm. ADVANTAGE OF THE INVENTION According to this invention, there exists an advantage that the aggregate particle | grains produced at the time of granulation at the time of surface coating using a fine powder are disintegrated and it becomes a preferable particle size.

The nonionic activator-containing granular composition of the present invention obtained as described above has a high bulk density and excellent flow characteristics and non-caking properties of the powder. It can also be used as a mixture with a granular detergent. Also, a builder powder, a surfactant powder, and other additives used in general detergents can be mixed to form a detergent.

[0031]

EXAMPLES Hereinafter, the present invention will be described in detail with reference to examples, but the present invention is not limited to these examples. Example 1 A ready-made mixer (manufactured by Matsuzaka Giken Co., Ltd., capacity: 20 liters, clearance of 5.0 mm between a stirring blade and a vessel wall) was mixed with amorphous silica having an average particle size of 25 μm (SiO ₂ 98.8% by weight, pore volume 35).
0cm ³ / 100g, specific surface area 210m ² / g, oil absorption 280ml / 100g) 35
Put the weight part, spindle (200rpm) and chopper (4000rpm)
Was started. There, the nonionic activator shown in Table 2
65 parts by weight were charged in 2 minutes, and stirring was stopped after 4 minutes. Next, 2 parts by weight of the above-mentioned amorphous silica (average particle size of primary particles: 60 nm) was charged, and the mixture was stirred for 30 seconds and discharged. The total charge was 4 kg. The bulk density, average particle size, fluidity, and caking properties of the granules thus obtained were measured. Table 2 shows the results.

Here, the bulk density of the powder was measured by the method described in JIS K 3362. The fluidity of the powder was measured by measuring the time required for 100 ml of the powder to flow out of a hopper for bulk density measurement specified in JIS K 3362, and it was determined that the shorter the time, the better the fluidity. The test method of the caking property is as follows. Caking test method Filter paper (Toyo filter paper No.2) 10.2 cm long x 6.2 cm wide x 4 high
Make a box with no cm top, and staple the four corners.
A 50 g sample is put in this box, and a total of 15 g + 250 g of an acrylic resin plate and a lead plate (or iron plate) is placed thereon. This is left in a thermo-hygrostat at a temperature of 30 ° C. and a humidity of 80%, and after 7 days, the caking state is judged. The judgment was made by obtaining the pass rate as follows. <Passing rate> The sample after the test was screened with a wire mesh (or a sieve, mesh 5 mm × 5
mm), weigh the powder that has passed through the wire gauze, and determine the transmittance for the sample after the test.

[0033]

(Equation 1)

Example 2 A granulated product was prepared in the same manner as in Example 1, and the same evaluation as in Example 1 was performed. However, as the porous oil-absorbing carriers include magnesium carbonate having an average particle size of 8.0 .mu.m (pore volume 180cm ^3/1
00g, specific surface area 35 m ² / g, oil absorption 150 ml / 100 g). Table 2 shows the composition and evaluation results. In Examples 1 and 2, when the inside was observed from the upper nozzle portion of the Loedige mixer during granulation, an adhesion layer of the nonionic activator-containing composition was formed between the wall of the Loedige mixer and the stirring blade. It had been.

Comparative Example 1 35 parts by weight of the amorphous silica used in Example 1 was charged into a Nauta mixer (manufactured by Hosokawa Milon Co., Ltd., capacity: 30 liters), and stirring (20 rpm) was started. Thereto, 65 parts by weight of the nonionic activator shown in Table 2 was added for 8 minutes, and after 15 minutes, stirring was stopped and the mixture was discharged. Incidentally, the total charged amount was 5 kg. The physical properties of the granules thus obtained were evaluated in the same manner as in Example 1. Table 2 shows the results. The Nauta mixer is a device that performs mixing by revolving and revolving around a shaft parallel to the container wall while a screw rotates along a conical container.

Comparative Example 2 100 parts by weight of the granulated product obtained in Comparative Example 1 and 2 parts by weight of the amorphous silica used in Example 1 were charged into a V blender, mixed for 5 minutes, stopped and discharged. Incidentally, the total charged amount was 5 kg. The physical properties of the granules thus obtained were evaluated in the same manner as in Example 1. Table 2 shows the results.

[0037]

[Table 2]

[0038]

EFFECTS OF THE INVENTION By using the method for producing a nonionic activator-containing granular composition of the present invention, a granular composition having a high nonionic activator content, a high bulk density, and excellent powder flow characteristics and non-caking properties is obtained. The composition can be obtained simply and energy-saving.

Continuation of the front page (72) Inventor Koji Toyoda 1130 Nishihama, Nishihama, Wakayama-shi, Wakayama Prefecture (56) References JP-A-62-86099 (JP, A) JP-A-62-158800 (JP, A) Hei 2-229894 (JP, A) JP-A-61-85499 (JP, A) JP-A-51-41708 (JP, A) (58) Fields investigated (Int. Cl. ⁷ , DB name) C11D 17 / 06 C11D 11/00

Claims (2)

(57) [Claims] 1. A pore volume of 100 to 600 cm ³ / mercury intrusion method.
100 g, the specific surface area by the BET method is 20 to 700 m ² / g, and the oil absorption in JIS K 5101 is 100 ml / 100 g or more.
A mixing component containing 70 parts by weight and a nonionic activator in a proportion of 30 to 85 parts by weight has a stirring shaft equipped with a stirring blade at the center of the inside, and when the stirring blade rotates, the stirring blade and the container wall In the meantime ,
By stirring and mixing with a stirring mixer that forms a clearance of 1 to 30 mm on average , a powder adhesion layer is formed on the wall of the stirring mixer, and granulation is performed while increasing the bulk density of the powder with stirring blades. Then, the obtained granules and the fine powder are mixed, and the surface of the granules is coated with the fine powder, and the bulk density is 0.6 to
A method for producing a granular composition containing a nonionic activator, comprising obtaining a granular composition having a concentration of 1.2 g / ml. 2. The nonionic activator-containing composition according to claim 1, wherein after granulation, 0.5 to 30 parts by weight of a fine powder is added to 100 parts by weight of the granulated material to coat the surface of the granulated material. A method for producing a granular composition.