JPH05906A - Coating type granular formulation controlled in eluting property and its production - Google Patents

Abstract

PURPOSE:To control elution of agricultural chemical ingredients into water by coating an essential ingredient consisting of active ingredient of agricultural chemical and bentonite by using a mixture of poval, vinyl acetate resin emulsion, etc., with water as a binder to formulate an undisintegrable granule. CONSTITUTION:A bentonite capable of promoting disintegration and spreading of film in water and accelerating elution rate of the agricultural active ingredient is added to an agricultural chemical product and the mixture is pulverized to give a raw powder. The proper amount of an undisintegrating material for controlling elution rate of the agricultural chemical active ingredient such as saccharire, dextrin, hydroxypropyl cellulose, carboxy methyl cellulose, sodium alginate, polyvinyl alcohol, vinyl acetate emulsion and acrylic resin emulsion combined with water is used as the binder to provide a coating type granule capable of controlling elution of active ingredient of agricultural chemical to water. Thereby the coating type granule capable of favorably controlling elution of the active ingredients can be economically and readily produced.

Description

Detailed Description of the Invention

[0001]

FIELD OF THE INVENTION The present invention relates to a granule in which elution of an agrochemical active ingredient into water is controlled, and a method for producing the same. More specifically, the present invention relates to an agrochemical active ingredient, bentonite, and optionally other carrier, Surfactant,
Stabilizers, etc. of pesticide active ingredients are mixed and crushed into powder, water,
Alternatively, one or more selected from the group consisting of sugars, dextrin, hydroxypropyl cellulose, carboxymethyl cellulose, sodium alginate, polyvinyl alcohol, vinyl acetate resin emulsion, and acrylic resin emulsion in combination with water is used as a binder. The present invention relates to a coated granule having a controlled elution property, which comprises coating a powder on a non-disintegrating carrier, and a method for producing the same.

[0002]

2. Description of the Related Art Agricultural chemicals are usually formulated into powders, granules, wettable powders, emulsions and the like and sprayed, and the formulation method is devised by the solubility of the active ingredient in water. In the case of an insoluble or sparingly soluble drug substance, how quickly it can be dispersed in water to exert its effect, and conversely, in the case of an easily soluble drug, how much dissolution can be suppressed to eliminate waste is necessary. There is. In granules, for example, when the active ingredient is easily soluble in water, the active ingredient is eluted in a short period of time in wet soil containing a large amount of water as well as in water, causing chemical damage,
In addition, the effect may be short-lived due to washout. In order to improve such a defect, the active ingredient has a salt structure (Japanese Patent Publication No. 42-21495), or the active ingredient is microencapsulated (JP-A-48-4643).
No.), a first layer of liquid resin and a powder for preventing caking are formed in the second layer (Japanese Patent Publication No. 41-19080),
Including a lipophilic base material that is solid at room temperature (Japanese Patent Application Laid-Open No. 55-
No. 4356) has been carried out, but the manufacturing method is complicated, the manufacturing cost is high, and the elution control is insufficient, so that the desired effect is not manifested and sustained. .

[0003]

It is an object of the present invention to provide a novel industrially useful coated granule having a controlled elution property and a method for producing the same.

[0004]

The present inventors have conducted various studies in order to achieve the above-mentioned object, and as a result, have been able to conveniently and economically and easily provide a coated granule which can conveniently control the elution of the active ingredient. It was possible to manufacture. Generally used as a binder for coated granules, polyvinyl alcohol, vinyl acetate resin emulsions or acrylic resin emulsions have a slow dissolution rate in water, or almost do not dissolve, so Elution is significantly suppressed.

According to the present invention, bentonite, which accelerates the disintegration / spreading of a film in water and accelerates the elution rate of the active ingredient of pesticide, is added to the bulk of the active ingredient of the pesticide and pulverized to obtain water or the active ingredient of the pesticide. Saccharide controlling the elution rate of, dextrin, hydroxypropyl cellulose, carboxymethyl cellulose, sodium alginate, polyvinyl alcohol, vinyl acetate resin emulsion, a combination of water and an appropriate amount of an acrylic resin emulsion, etc. as a binder, the bulk powder A coated granule which is coated on non-disintegrating granules to control the elution rate of an active ingredient of an agricultural chemical into water, and a method for producing the same. The granules of the present invention contain 1 to 30% by weight of bentonite.
Including 0.1 to 30% by weight of a binder other than water,
If necessary, it further contains an appropriate amount of amorphous silica having a high oil absorption property, a carrier such as clay, a surfactant, a stabilizer of an agrochemical active ingredient, and the like.

The pesticidal active ingredient applicable to the present invention preferably has a solubility in water at 20 ° C. of 100 ppm or less, and if it is a pesticide having the above-mentioned solubility, insecticide, fungicide, herbicide, etc. It doesn't matter. Examples of pesticides that can be used in the present invention include organic phosphorus-based, carbamate-based,
Examples of urea-based, heterocyclic-based, acid amide-based compounds and specific examples thereof are shown below, but the invention is not limited thereto, and the agrochemical active ingredient may be a single composition of two or more kinds.

O, O-dimethyl-O- [3-methyl-4
-(Methylthio) phenyl] thiophosphate (generic name: phenthion), (2-isopropyl-4-methylpyrimidyl-6) -diethylthiophosphate (generic name: diazinon), O, O-diethyl-S-2- (ethylthio) ) Ethyl phosphorodithioate (generic name: ethyl thiomethone), O-2,4-dichlorophenyl O-
Ethyl S-propyl phosphorodithioate (generic name:
Prothiophos), O-ethyl-S, S-diphenyldithiophosphate (generic name: hinozane),

N- [1- (4-chlorophenyl) -ethyl] -2,2-dichloro-1,3,3-trimethylcyclopropanecarboxamide, N- [1- (4-chlorophenyl) -ethyl] -2, 2-dichloro-1-ethyl-
3-methylcyclopropanecarboxamide, N- [1-
(4-Chlorophenyl) -ethyl] -2,2-dichloro-1-isopropylcyclopropanecarboxamide, N
-[1- (4-Bromophenyl) -ethyl] -2,2-
Dichloro-1-isopropylcyclopropanecarboxamide, N- [1- (4-chlorophenyl) -ethyl]-
2,2-dichloro-1-methyl- (trans) -3-methylcyclopropanecarboxamide, N- [1- (4-
Chlorophenyl) -ethyl] -2,2-dichloro-1-
Ethyl-3,3-dimethylcyclopropanecarboxamide, N- (R)-[1- (4-chlorophenyl) -ethyl] -2,2-dichloro-1-ethyl-3t-methyl-
A mixture of diastereomers of 1r-cyclopropanecarboxamide,

N- (R)-[1- (4-chlorophenyl) -ethyl]-(1S) -2,2-dichloro-1-ethyl-3t-methyl-1r-cyclopropanecarboxamide, N- [1- (4-Bromophenyl) -ethyl]-
Diastereo of 2,2-dichloro-1,3,3-trimethylcyclopropanecarboxamide, N- (R)-[1- (4-chlorophenyl) -ethyl] -2,2-dichloro-1-isopropylcyclopropanecarboxamide Mixture of mers, N- (R)-[1- (4-chlorophenyl) -ethyl]-(1S) -2,2-dichloro-1-isopropylcyclopropanecarboxamide, 1- (4-
Chlorophenoxy) -3,3-dimethyl-1- (1,
2,4-triazol-1-yl) -2-butanone (generic name: triadimefon), O-methyl O- (2-nitro-4-methylphenyl) N-isopropylphosphoramide thioate (generic name: amipro) Phosmethyl), 2-
Benzothiazol-2-yloxy-N-methylacetanilide (generic name: mefenacet)

The method for producing the coated granules of the present invention is shown below. As the core of the coated granule, silica sand, calcium carbonate, clay granules, granulated non-disintegrating granules, etc. are used, and water, or sugar, dextrin, hydroxypropyl cellulose, carboxymethyl cellulose, sodium alginate, polyvinyl is used for this core. An appropriate amount of alcohol, vinyl acetate resin emulsion, acrylic resin emulsion or the like combined with water is mixed as a binder. Next, bentonite and, if necessary, amorphous silica having high oil absorption, a carrier such as clay, a surfactant, a stabilizer of the pesticide active ingredient, etc. are added to the pesticide active ingredient and mixed and pulverized to prepare the raw material of the pesticide active ingredient. Add powder and mix well, then dry to make the product.

The core of the coated granules that can be used in the present invention is a non-disintegrating carrier, such as silica sand, calcium carbonate, pumice, clay granules and granulated non-disintegrating granules. It is not limited to this. Examples of the binder include water, sugar, dextrin, hydroxypropyl cellulose, carboxymethyl cellulose, sodium alginate, polyvinyl alcohol, vinyl acetate resin emulsion, acrylic resin emulsion, acrylic styrene copolymer resin emulsion, but are not limited thereto. Not something. Further, as the surfactant, alkyl sulfate ester salts, aryl sulfonates, polyoxyethylene glycol ethers,
Examples thereof include polyhydric alcohol esters, dialkyl sulfosuccinate salts, polycarboxylic acid type surfactants, etc., but are not limited thereto. Next, examples will be given to prove the usefulness of the present invention, but the present invention is not limited thereto. The granule of the present invention was prepared by the following method.

[0012]

【Example】

Example 1 Surfactant (0.50 parts by weight) and polyvinyl alcohol (0.40 parts by weight) dissolved in an appropriate amount of water were sprayed on silica sand (93.10 parts by weight) and stirred. Wet evenly. Bentonite (2.0
0 parts by weight) and pesticide active ingredient (I) (4.00 parts by weight) are added to the powder mixture, and the mixture is stirred and mixed, and then dried. The same was prepared for Examples 2 to 4.

[0013]

[Table 1]

Test Example Dissolution test in water Granules prepared according to the formulations of Examples 1 to 4 were placed in a beaker containing 1 liter of water, and 50 mg of each of the granules was poured from the center of the beaker at regular intervals. A part was collected, the content of the active ingredient was analyzed, and the dissolution rate was calculated.

[0015]

[Table 2]

Example 5 A silica sand (93.10 parts by weight) prepared by dissolving a surfactant (0.50 parts by weight) and polyvinyl alcohol (0.40 parts by weight) in an appropriate amount of water was sprayed, Stir to evenly wet. Bentonite (2.0
0 parts by weight) and pesticide active ingredient (II) (4.00 parts by weight) are added and mixed with stirring, and then dried. The same was prepared for Examples 6 to 8.

[0017]

[Table 3]

Example 9 Surfactant (0.50 parts by weight) and carboxymethyl cellulose (1.00 parts by weight) were added to silica sand (92.50 parts by weight) together with an appropriate amount of water, and the mixture was stirred to evenly wet. Let To this, a bulk powder comprising bentonite (2.00 parts by weight) and the agricultural chemical active ingredient (III) (4.00 parts by weight) is added, mixed with stirring, and then dried. Examples 10-12
Was similarly prepared.

[0019]

[Table 4]

Example 13 Surfactant (0.50 parts by weight) and vinyl acetate resin emulsion (0.40 parts by weight) were added to silica sand (93.10 parts by weight) together with an appropriate amount of water, and the mixture was stirred to homogeneity. Moisten. To this is added a bulk powder consisting of bentonite (2.00 parts by weight) and pesticide active ingredient (IV) (4.00 parts by weight), stirred and mixed, and then dried. The same was prepared for Examples 14 to 16.

[0021]

[Table 5]

Example 17 Surfactant (0.50 parts by weight) and acrylic resin emulsion (0.40 parts by weight) were added to silica sand (93.10 parts by weight) together with an appropriate amount of water, and stirred to homogenize. Moisten. To this is added a bulk powder consisting of bentonite (2.00 parts by weight) and an agricultural chemical active ingredient (V) (4.00 parts by weight), and the mixture is stirred, mixed and dried. Examples 18 to 20 were similarly prepared.

[0023]

[Table 6]

Test Example Dissolution test in water Granules prepared according to the formulations of Examples 5 to 20 were used, each containing 50 mg.
The solution was placed in a beaker containing liters of water, a part of the solution was sampled from the center of the beaker at regular intervals, the content of the active ingredient was analyzed, and the dissolution rate was calculated.

[0025]

[Table 7]

[0026]

[Table 8]

[0027]

[Table 9]

[0028]

[Table 10]

(Note) The pesticide active ingredients (I) to (V) in each example are as follows. (I): 2-benzothiazol-2-yloxy-N-
Methyl acetanilide (II): N- [1- (4-chlorophenyl) -ethyl]
-2,2-Dichloro-1-ethyl-3-methylcyclopropanecarboxamide (III): N- [1- (4-chlorophenyl) -ethyl]
-2,2-Dichloro-1-isopropylcyclopropanecarboxamide (IV): N- (R)-[1- (4-chlorophenyl)-
Ethyl] -2,2-dichloro-1-ethyl-3t-methyl-1r-cyclopropanecarboxamide diastereomeric mixture (V): N- (R)-[1- (4-chlorophenyl)-
Ethyl] -2,2-dichloro-1-isopropylcyclopropanecarboxamide diastereomeric mixture

As is clear from the above examples and test examples, the present invention promotes the disintegration and spread of the film in the coating of the non-disintegrating carrier of the agrochemical active ingredient and the dissolution rate of the agrochemical active ingredient. By changing the composition ratio of the accelerated bentonite and the binder that significantly suppresses the elution of the active ingredient into water, the elution of the pesticide active ingredient can be controlled, and the desired concentration in water and the duration of the medicinal effect can be measured. Therefore, the active ingredient can be used for a long period of time within a concentration range that does not cause phytotoxicity. This allows the chemicals to be sprayed in the seedling raising box, which is indispensable for mechanical transplantation, which is the mainstream of rice cultivation at present, and it contributes to labor saving of spraying.

Claims (2)

[Claims] 1. A dissolution control granule, which is obtained by mixing and pulverizing a pesticide active ingredient and bentonite as essential ingredients to obtain a bulk powder.
As a binder, water or a combination of water or one or more selected from the group consisting of sugar, dextrin, hydroxypropyl cellulose, carboxymethyl cellulose, sodium alginate, polyvinyl alcohol, vinyl acetate resin emulsion, and acrylic resin emulsion, A coated granule having a controlled elution property, which comprises coating the above-mentioned bulk powder on a non-disintegrating carrier. 2. In a dissolution controlling granule, a pesticide active ingredient and bentonite are mixed and pulverized as essential ingredients to obtain a bulk powder,
As a binder, water or a combination of water or one or more selected from the group consisting of sugar, dextrin, hydroxypropyl cellulose, carboxymethyl cellulose, sodium alginate, polyvinyl alcohol, vinyl acetate resin emulsion, and acrylic resin emulsion, A method for producing a coated granule having a controlled elution property, which comprises coating the above powder with a non-disintegrating carrier.