JPH07126106A - Granular agrochemical composition - Google Patents

Abstract

PURPOSE:To provide the composition excellent in disintegrability through dispersion in water, suspension rate and powderiness, also advantageous in its industrial continuous production because of having a composition favorable in extrusion granulativity. CONSTITUTION:The composition comprising (A) an agrochemical active ingredient solid at normal temperatures, (B) a sulfosuccinic diester-type surfactant and (C) at least one kind of surfactant selected from the other sulfonic acid-type surfactants and unsaturated carboxylic acid-type surfactants.

Description

Detailed Description of the Invention

[0001]

FIELD OF THE INVENTION The present invention relates to a granular pesticide composition.

[0002]

BACKGROUND OF THE INVENTION Granular wettable powders of agricultural chemicals are used by suspending them in water. However, from the viewpoints of distribution such as transportation and ease of use, the agricultural chemical active ingredient is used. It has been desired to develop a granular wettable powder containing a high concentration of water. Generally, when an attempt is made to produce a granular pesticidal composition containing a solid pesticidal active ingredient having a relatively low melting point, for example, a pesticidal active ingredient having a melting point of 60 to 120 ° C., the granulation property is deteriorated, and extrusion granulation or the like is performed. However, there is a problem in that the production may be difficult with the simple granulation method. The present invention has been made for the purpose of providing a granular pesticidal composition containing a high concentration of an agrochemical active ingredient, excellent in disintegration dispersibility in water, and having a high strength and therefore less disintegration during transportation or storage. It is a thing.

[0003]

The present invention comprises: a) an agrochemical active ingredient which is solid at room temperature, b) a sulfosuccinic acid diester type surfactant, and c) another sulfonic acid type surfactant and an unsaturated carboxylic acid type interface. Granular pesticide composition containing one or more surfactants selected from active agents (hereinafter,
It is referred to as the composition of the present invention. ) Is provided, and examples of the agrochemical active ingredient include the following. (1) O- (2,6-dichloro-4-methoxyphenyl) O, O-dimethylphosphorothioate [torchrophosmethyl] (2) Isopropyl 3,4-diethylphenylcarbamate [dietofencarb] (3) Pentyl 2-chloro-4 -Fluoro-5-
(3,4,5,6-Tetrahydrophthalimide) phenoxyacetate [flumicrolacpentyl] (4) O, S-dimethyl-N-acetylphosphoramidothioate These pesticidal active ingredients may be used alone or in combination. The above may be mixed and used. The pesticidal active ingredient is usually contained in the composition of the present invention in an amount of 5 to 90% by weight, preferably 20 to 90% by weight, based on the total weight of the composition.

The sulfosuccinic acid diester type surfactant used in the present invention is generally known as a sulfosuccinate dialkyl ester surfactant, and the alkyl group is a heptyl group, an octyl group or a nonyl group. And the like, and an alkyl group having 6 or more carbon atoms, preferably 7 to 12 are exemplified, and examples of the salt-forming cation of the sulfonic acid moiety include alkali metal cations such as sodium salt and potassium salt. Specific representative examples of the sulfosuccinic acid diester type surfactant include diheptyl sodium sulfosuccinate, dioctyl sodium sulfosuccinate, and dinonyl sodium sulfosuccinate. The sulfosuccinic acid diester type surfactant is generally contained in the composition of the present invention in an amount of 0.1 to 7% by weight, preferably 0.3 to 5%.
It is contained by weight%.

Examples of the sulfonic acid type surfactants other than the sulfosuccinic acid diester type surfactants used in the present invention include aryl sulfonic acid type surfactants, alkyl sulfonic acid type surfactants, lignin sulfonic acid type surfactants. The aryl sulfonic acid type surfactant is an alkyl benzene sulfonic acid type surfactant (for example, an alkali metal salt of dodecyl benzene sulfonic acid,
Ammonium salt), cresol sulfonic acid type surfactant (for example, cresol sulfonic acid formalin condensate, its alkali metal salt), styrene sulfonic acid type surfactant (for example, a copolymer of methacrylic acid and styrene sulfonic acid) Alkali metal salt, ammonium salt), naphthalene sulfonic acid type surfactant (for example, naphthalene sulfonic acid formalin condensate, its alkali metal salt, alkaline earth metal salt, ammonium salt, methyl naphthalene sulfonic acid formalin condensate, its alkali metal Salt, alkaline earth metal salt, ammonium salt, butyl naphthalene sulfonic acid formalin condensate, alkali metal salt thereof, alkaline earth metal salt, ammonium salt, alkyl naphthalene sulfonic acid), etc., and alkyl sulfonic acid type surfactant Is normal para Insuruhon acid type surfactants (e.g., alkali metal salts of normal paraffin sulfonic acid,
Ammonium salt) and the like, and the ligninsulfonic acid type surfactant means an alkali metal salt, ammonium salt, etc. of ligninsulfonic acid. The unsaturated carboxylic acid type surfactant means a copolymer of maleic acid and an olefin such as isobutylene or diisobutylene, an alkali metal salt or an ammonium salt thereof. These surfactants may be used alone or in admixture of two or more, and are usually contained in the composition of the present invention in an amount of 5 to 30% by weight, preferably 7 to 25% by weight.

In the composition of the present invention, other surfactants such as polyoxyethylene styryl phenyl ether, polyoxyethylene alkylaryl ether, polyoxyethylene alkyl ester, polyoxyethylene sorbitan alkyl ester and sorbitan alkyl ester are also included. It is also possible to add a nonionic surfactant such as polyoxyethylene polyoxypropylene block copolymer, and an anionic surfactant such as polyoxyethylene alkylaryl ether sulfate ester salt.

The composition of the present invention usually contains a carrier for formulation such as a mineral carrier, a water-soluble carrier and a vegetable carrier. Examples of the mineral substance carrier include kaolin, diatomaceous earth, roeseki, montmorillonite, acid clay, activated clay, attapulgite,
Examples include pyrophyllite, bentonite, calcium carbonate, sericite, zeolite, wollastonite, calcium silicate, and the like. Examples of water-soluble carriers include ammonium sulfate, urea, dextrin, lactose, salt, mirabilite, sodium carbonate, sodium bicarbonate, maleic acid. , Citric acid, fumaric acid, malic acid, polyethylene glycol having an average molecular weight of 6000 to 20000, and the like, and plant carriers include, for example, wheat flour, wood flour, starch, bran, chaff powder, soybean flour, and the like. Hydrous silicon dioxide or the like is also used as a carrier for the preparation. The content of the pharmaceutical carrier in the composition of the present invention is generally 0.1 to 85% by weight, preferably 0.5 to 75% by weight. In the composition of the present invention, in addition to the above, solvents such as propylene glycol and ethylene glycol, hydroxypropyl cellulose, water-soluble polymers such as sodium carboxymethyl cellulose, stabilizers, potency enhancers, phytotoxicity reducing agents, coloring agents, fragrances and builders. Etc. may be contained.

The composition of the present invention is produced, for example, as follows. Pesticide active ingredient only, or solid ingredients and / or ingredients such as carriers for pharmaceuticals added to this, are pulverized with a dry pulverizer such as jet mizer, pin mill, hammer mill, etc., and average particle size is 30 μm or less. ,Preferably
The particle size is 10 μm or less, and other components are added if necessary, followed by thorough mixing, and then water is added and kneaded, followed by extrusion granulation. Alternatively, the pesticide active ingredient, the surfactant, the water and the like may be pulverized with a wet pulverizer such as a bead mill or a sand grinder to be granulated. In the extrusion granulation, the extrusion diameter is preferably 0.3 to 1.0 mm, and more preferably 0.3 to 0.7 mm, from the viewpoint of disintegration dispersibility in water of the composition of the present invention. After being granulated as described above, the composition of the present invention is usually dried at a temperature lower than the melting point of the agrochemical active ingredient by 10 ° C. or more, preferably 20 ° C. or more. Further, if necessary, operations such as sieving are performed, but the particle size at that time is usually 70-
It is 1200 μm, preferably 100 to 1000 μm.

The present invention will be described below with reference to production examples and test examples, but the present invention is not limited to the examples described below. First, a production example is shown. In the examples described below, parts and% represent parts by weight and% by weight. The compounds are represented by the above compound numbers. Production Example 1 75 parts of compound (1), Morwet D425 (sodium salt of naphthalenesulfonic acid formalin condensate manufactured by De Soto) 1
0 parts, Morwet EFW (alkyl Sodium Naphthalene Sulfonate manufactured by De Soto, etc.) 1.5 parts and calcium carbonate 11.5 parts were mixed well with a juice mixer and then pulverized with a jet mizer. The average particle size of the obtained ground premix was measured using a Coulter Counter TAII type.
was μm. 98 parts of the obtained crushed premix was placed in a mortar, 2 parts of air roll CT-1 (70% solution of dioctyl sulfosuccinate manufactured by Toho Kagaku) was added and well mixed with a pestle, and 6 parts of water was further added and kneaded. did. Kneading
When granulated with a small extrusion granulator equipped with a 0.5 mmφ screen, the granulation property was good. Granulate 1 at 40 ℃
After drying for 5 minutes, the particles were sized to obtain a granular wettable powder having a particle size of 300 to 710 μm.

Production Example 2 Compound (1) 75 parts, Morwet D425 10 parts, Morwet E
After thoroughly mixing 3 parts of FW and 10 parts of kaolin clay with a juice mixer, the mixture was ground with a jet mizer. The average particle size of the obtained ground premix was 5.1 μm as measured with a Coulter Counter TAII type. 98 parts of the obtained ground premix was put in a mortar, 2 parts of air roll CT-12 was added and well mixed with a pestle, and 6 parts of water was further added and kneaded. When the kneaded product was granulated with a small extrusion granulator equipped with a 0.5 mmφ screen, the granulation property was good. The granulated product was dried at 40 ° C. for 15 minutes and then sized to obtain a granular wettable powder having a particle size of 300 to 710 μm.

Production Example 3 75 parts of compound (1), 10 parts of Reax 85 A (sodium lignin sulfonate manufactured by Westvaco), 8 parts of Reax 88 B
3 parts (Westvaco sodium lignin sulfonate) and 9 parts calcium carbonate were thoroughly mixed with a juice mixer and then pulverized with a jet mizer. The average particle size of the obtained ground premix was 4.9 μm as measured with Coulter Counter TAII type. Put 97 parts of the obtained ground premix in a mortar and air roll CT-1
3 parts was added and mixed well with a pestle, and 6 parts of water was further added and kneaded. When the kneaded product was granulated with a small extrusion granulator equipped with a 0.5 mmφ screen, the granulation property was good. The granulated product was dried at 40 ° C. for 15 minutes and then sized to obtain a granular wettable powder having a particle size of 300 to 710 μm.

Production Example 4 75 parts of Compound (1), 10 parts of Morwet D425, Morwet E
After thoroughly mixing 1.5 parts of FW and 11.5 parts of calcium carbonate with a juice mixer, the mixture was ground with a jet mizer. The average particle size of the obtained ground premix was 8.8 μm as measured with Coulter Counter TAII type. 98 parts of the obtained crushed premix was put in a kneader, 2 parts of air roll CT-12 was added and well mixed with a pestle, and 6 parts of water was further added and kneaded. 20 kg of kneaded product 0.5
Granulation was carried out by a basket type extrusion granulator equipped with a screen of mmφ. Put the granulated material in the fluid bed dryer, 2
After drying at 0 ℃ for 30 minutes, the particles are sized and the particle size is 300-850.
A μm granular wettable powder was obtained.

Production Example 5 75 parts of Compound (1), 12.5 parts of Demol EP powder (Kao's unsaturated carboxylic acid type surfactant) and 10.5 parts of calcium carbonate were thoroughly mixed with a juice mixer and then pulverized with a jet mizer. The average particle size of the obtained pulverized premix was measured by using Coulter Counter TAII type and found to be 5.2 μm. 98 parts of the obtained ground premix was placed in a mortar, 2 parts of Neocor YSK (70% solution of dioctyl sulfosuccinate manufactured by Daiichi Kogyo Seiyaku Co., Ltd.) was added and mixed well with a pestle, and 6 parts of water was further added and kneaded. did. When the kneaded product was granulated with a small extrusion granulator equipped with a 0.5 mmφ screen, the granulation property was good. The granulated product is dried at 40 ° C for 15 minutes and then sized to give a particle size of 300
A granular wettable powder of ˜710 μm was obtained.

Next, a production example of a comparative composition used in a comparison test described below will be shown as a comparative production example. Comparative Production Example 1 Compound (1) 75 parts, Morwet D425 10 parts, Morwet E
After thoroughly mixing 1.5 parts of FW and 13.5 parts of calcium carbonate with a juice mixer, the mixture was ground with a jet mizer. The average particle size of the obtained crushed premix was 4.6 μm as measured with a Coulter Counter TAII type. 100 parts of the obtained ground premix is put in a mortar,
6 parts of water was added and kneaded well. When the kneaded product was granulated with a small extrusion granulator equipped with a 0.5 mmφ screen, the granulation property was not good. The obtained granulated product was dried at 40 ° C. for 15 minutes and then sized to obtain a granular wettable powder having a particle size of 300 to 710 μm.

Comparative Production Example 2 75 parts of the compound (1), 12.5 parts of demole EP powder and 12.5 parts of calcium carbonate were mixed well with a juice mixer and then pulverized with a jet mizer. The average particle size of the obtained ground premix was 5.5 μm as measured with a Coulter counter TAII type. 100 parts of the obtained crushed premix was put in a mortar, 6 parts of water was added and kneaded well. When the kneaded product was granulated with a small extrusion granulator equipped with a 0.5 mmφ screen, the granulation property was not good. The obtained granulated product was dried at 40 ° C. for 15 minutes and then sized to obtain a granular wettable powder having a particle size of 300 to 710 μm.

Next, a test example will be shown. Test Example 1 Each of the granular wettable powders obtained in Production Examples 1 to 5 and Comparative Production Examples 1 and 2 was measured for disintegration disintegration in water, suspension rate and fineness by the following methods. The measuring method is as follows. A 250 ml cylinder with double stopper 250 ml of hard water was placed in a constant temperature water bath at 20 ° C. Put 500 mg of each granular wettable powder into the cylinder and repeat the inversion of the cylinder once every 2 seconds to disperse the number of inverted cylinders in water until the granular wettable powder completely disintegrates and disperses. Expressed as collapsible. However, the maximum number of times the cylinder was inverted was 30. Then, this cylinder
After standing still in the constant temperature water tank of 15 minutes, 25 ml of each was sampled from the center of the cylinder after 15 minutes, the water was evaporated, and the agricultural chemical active ingredient was analyzed by gas chromatography to determine the suspension rate. Also, 5 g of each granular wettable powder was weighed in a 300 ml beaker, 100 ml of tap water was added thereto, and the mixture was placed in an ultrasonic cleaner for 15 minutes. The obtained solution was put into a sieve of 45 μm, and tap water was further thoroughly flowed, and the residue was recovered and dried. The ratio of passing through the sieve was calculated from the weight of this residue and expressed as the fineness. The results are summarized in Table 1.

[0017]

[Table 1]

[0018]

INDUSTRIAL APPLICABILITY The pesticidal composition of the present invention has a disintegrating property in water,
The composition is excellent in suspension rate and fineness, and is also advantageous in industrial continuous production because it has a composition with good extrusion granulation property.

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Claims (4)

[Claims] 1. One or more selected from a) an agricultural chemical active ingredient which is solid at room temperature, b) a sulfosuccinic acid diester type surfactant, and c) other sulfonic acid type surfactants and unsaturated carboxylic acid type surfactants. A granular pesticidal composition comprising a surfactant. 2. A pesticidal active ingredient which is 20 to 90% by weight at room temperature and solid at room temperature, b) 0.3 to 5% by weight of sulfosuccinic acid diester type surfactant, and c) 7 to 25% by weight of other sulfone. A granular agricultural chemical composition comprising one or more surfactants selected from an acid type surfactant and an unsaturated carboxylic acid type surfactant. 3. The granular agricultural chemical composition according to claim 1, wherein the agricultural chemical active ingredient is tolclofos-methyl. 4. A pesticide active ingredient which is solid at room temperature, a sulfonic acid type surfactant other than the sulfosuccinic acid diester type, and / or
Alternatively, an unsaturated carboxylic acid type surfactant, and optionally a carrier for an agrochemical formulation, and a sulfosuccinic acid diester type surfactant and water are added thereto, and the mixture is kneaded for granulation. Method of making the composition.