KR102193709B1 - Agricultural chemical composition of water-dispersible granule type and preparation method thereof - Google Patents

Abstract

The present invention relates to a granular wettable pesticide composition comprising particles adsorbing a first raw agent having a melting point of 30 to 50°C and a water-soluble organic solvent, although the pesticide composition is a granular wettable pesticide composition containing a low melting point raw agent And, the suspension, collapse, and physical properties are not deteriorated, and convenience can be provided to the user. In addition, the present invention provides a step of obtaining a mixture of a first raw agent and a water-soluble organic solvent; Adding water to the member and kneading to form particles; Drying the particles at a temperature exceeding the melting point of the first raw agent; And adsorbing the mixture to the dried particles. According to the manufacturing method, it is possible to prevent the melting of the original agent during the drying process, and thus a low melting point original agent It is an invention that not only can prepare a pesticide composition in the form of a granule hydration agent, but also can prepare a composition that does not deteriorate the suspension, disintegration and physical properties, thus contributing to the pesticide-related industry.

Description

Agrochemical composition of granule type and its manufacturing method TECHNICAL FIELD [AGRICULTURAL CHEMICAL COMPOSITION OF WATER-DISPERSIBLE GRANULE TYPE AND PREPARATION METHOD THEREOF}

The present invention relates to a granular wettable pesticide composition and a method for producing the same.

Regarding the formulation of pesticides, the formulation of pesticides is limited according to the inherent physicochemical properties of the original drug. The agrochemical raw material is required to process the formulation suitable for the original formulation so that the activity of the raw material is effectively revealed and the convenience and stability are secured by using subsidiary materials such as surfactants and extenders. Formulations applied to pesticides can be divided into solid formulations such as wettable powders, powders, granular wettable powders, and granules, and liquid formulations such as emulsions, liquids, liquid wettables, oily wettables, emulsions, and emulsions. Due to the nature of pesticides, it is sometimes possible to directly treat granular herbicides or granules applied to water, but it is a one-shot treatment method in which products manufactured with high concentration are diluted with a certain amount of water and applied to crops. If the agrochemical raw material is water-soluble, it is possible to use a water-soluble product such as a liquid or water-soluble agent, but in the case of a fat-soluble raw material, processing through the formulation is necessary so that it can be mixed with water and mixed evenly.

Emulsions, powders, and hydrating agents were first introduced and used in Korea. Compared to its excellent medicinal properties, preference for emulsions is decreasing due to excessive use of organic solvents, and hydrating agents with relatively low cost and manufacturing processes that only apply mixed pulverization have been developed actively in recent years due to the dust problem that occurs during the hydration process. It doesn't work. Therefore, in order not to use organic solvents and to prevent dust generation like a hydrating agent, the development of a liquid hydrating agent and a granular hydrating agent is considered first in Korea.

Low-melting-point pesticide raw materials are solid at room temperature, but their melting point is low to 30℃ to 50℃ and changes to liquid when heated above the melting point. Therefore, it is developed as a hydrating agent that is pulverized by adsorbing to an emulsion or adsorbent that can be easily manufactured. It is general, and it is difficult to process into other formulations and is limited.

When developing a granular hydrating agent formulation using such a low-melting-point pesticide raw material, it is difficult to develop a granular hydrating agent by allowing the particles to be bonded to each other after melting at a drying temperature of 55 to 80°C when going through the drying process, which is one of the granular hydrating agent manufacturing processes. In order to solve this problem, a method of mixing a low-melting-point pesticide with a non-aqueous solvent such as alkylbenzene was developed, but it was also confirmed that the physical properties of the product were degraded because the non-aqueous solvent inhibited the disintegration property of the granular water agent. .

Korean Patent Publication No. 10-2018-0137003

It is an object of the present invention to provide a granular wettable pesticide composition and a method for producing the same, in which disintegration, suspension and physical properties are not reduced.

1. A granular wettable pesticide composition comprising particles adsorbing the first raw agent having a melting point of 30 to 50°C and a water-soluble organic solvent.

2. In the above 1, the first agent is etopenprox, cycleoxydim, benfurecite, cyhalopopbutyl, diclopopmethyl, dimethoate, dimethachlor, alacrore, esfenvaler Rate, fenvalerate, lambdacyhalothrin, chloropyrophos, tefluthrin, trifluralin, fenpropatrin, and at least one selected from the group consisting of prochloraz, granule hydration agrochemical composition.

3. In the above 1, the water-soluble organic solvent is N-methylpyrrolidone, butanediol, 2-butoxyethanol, dimethyl glycol, dimethyl sulfoxide, 1,4-dioxane, perfuryl alcohol, N, N-dimethylacetamide, propanetriol, pentanediol, propylene glycol, tetrahydrofuran, triethylene glycol, propylene glycol monomethyl ether, dipropylene glycol monomethyl ester, dipropylene glycol monomethyl ether and dipropylene glycol monoethyl ether At least one selected from the group consisting of, granule wettable pesticide composition.

4. In the above 1, the content of the water-soluble organic solvent is 30 to 200 parts by weight compared to the first raw agent, granule wettable pesticide composition.

5. In the above 1, the content of the first raw agent and the water-soluble organic solvent is 5 to 20 parts by weight relative to the particles, granule wettable pesticide composition.

6. In the above 1, wherein the particles will have a particle diameter of 0.5 to 1.1 mm, granule wettable pesticide composition.

7. The method of 1 above, wherein the particles include a member, granule wettable pesticide composition.

8. In the above 7, wherein the member is at least one from the group consisting of a surfactant, a wetting agent, a disintegrant, and a carrier, granule wettable pesticide composition.

9. According to the above 1, wherein the particles adsorbing the first raw agent and the water-soluble organic solvent is prepared by adsorbing a mixture of the first raw agent and the water-soluble organic solvent to the dried particles, granule wettable pesticide composition.

10. In the above 9, wherein the drying is carried out at 55 to 80 ℃, granule wettable pesticide composition.

11. obtaining a mixture of the first raw agent and the water-soluble organic solvent;

Adding water to the member and kneading to form particles;

Drying the particles at a temperature exceeding the melting point of the first raw agent; And

Adsorbing the mixture to the dried particles; method for producing a granular wettable pesticide composition comprising a.

12. In the above 11, wherein the first raw material has a melting point of 30 to 50 ℃, the method for producing a granular wettable pesticide composition.

13. In the above 11, the first agent is etopenprox, cycleoxydim, benfurecite, cyhalopopbutyl, diclopopmethyl, dimethoate, dimethachlor, alacrore, esfenvaler Rate, fenvalerate, lambdacyhalothrin, chloropyrophos, tefluthrin, trifluralin, fenpropatrin, and at least one selected from the group consisting of prochloraz, a method for producing a granular hydration-type pesticide composition .

14. In the above 11, the water-soluble organic solvent is N-methylpyrrolidone, butanediol, 2-butoxyethanol, dimethyl glycol, dimethyl sulfoxide, 1,4-dioxane, perfuryl alcohol, N, N-dimethylacetamide, propanetriol, pentanediol, propylene glycol, tetrahydrofuran, triethylene glycol, propylene glycol monomethyl ether, dipropylene glycol monomethyl ester, dipropylene glycol monomethyl ether and dipropylene glycol monoethyl ether At least one selected from the group consisting of, a method for producing a granular wettable pesticide composition.

15. The method of 11 above, wherein the water-soluble organic solvent is mixed with 30 to 200 parts by weight compared to the first raw agent.

16. The method of 11 above, wherein the adsorption is to adsorb a mixture of 5 to 20 parts by weight relative to the dried particles, a method for producing a granular wettable pesticide composition.

17. The method of 11 above, wherein the member is at least one selected from the group consisting of a surfactant, a wetting agent, a disintegrant, and a carrier.

18. The method of 11 above, further comprising, heating and dissolving the first raw material before mixing the first raw material and the water-soluble organic solvent.

19. In the above 11, the step of pulverizing the member before adding water to the member; further comprising, a method for producing a granular wettable pesticide composition.

20. The method of 11 above, wherein the particles have a particle diameter of 0.5 to 1.1 mm, the method of manufacturing a granular wettable pesticide composition.

21. In the above 11, the temperature exceeding the melting point is 55 to 80 ℃, the method for producing a granular wettable pesticide composition.

22. The method of 11 above, wherein the drying is performed for 5 to 15 minutes.

Although the composition of the present invention is a granular wettable pesticide composition containing a low melting point raw agent, suspension, disintegration, and physical properties do not deteriorate, thereby providing convenience to users. In addition, according to the manufacturing method of the present invention, it is possible to prevent the melting of the raw agent during the drying process, so that not only can the low melting point raw agent be prepared in the form of a granular wettable agent, but also the suspension, disintegration and physical properties are lowered. It is possible to prepare a composition that does not.

Hereinafter, the present invention will be described in detail.

The present invention relates to a wettable granule pesticide composition comprising particles adsorbed with a first raw agent having a melting point of 30 to 50°C and a water-soluble organic solvent.

The composition according to an embodiment of the present invention has excellent disintegration and suspension properties when hydrated in water, and physical properties may not be deteriorated in a state of storage at a high temperature of 50°C or higher or a low temperature of 0°C or lower.

In the case of the first raw agent, it may be used without limitation as long as it is an agrochemical raw agent, but may be, for example, a melting point of 26 to 54°C, specifically 28 to 52°C, and more specifically 30 to 50°C.

Specific examples of the first agent are etopenprox (melting point: 36.4 to 38.0°C), cycle oxidim (melting point: 41°C), benfuricite (melting point: 32 to 35°C), and cyhalopopbutyl ( Melting point: 49.5°C), diclopopmethyl (melting point: 39 to 41°C), dimethoate (melting point: 49°C), dimethachlor (melting point: 4.8 to 46.7°C), alacrore (melting point: 40.5 to 41.5) °C), esfenvalerate (melting point: 38 to 54 °C), penvalerate (melting point: 39.5 to 53.7 °C), lambdacyhalothrin (melting point: 49.2 °C), chloropyrophos (melting point: 42 to 43.5 °C) ), Tefluthrin (melting point: 44.6° C.), triflutraline (melting point: 48.5 to 49° C.), fenpropathrin (melting point: 45 to 50° C.) and prochloraz (melting point: 46.5 to 49.3° C.) It may be at least one selected from the group.

In the case of the etopenprox, it can be applied to pest control such as snap worms, moths, snails, and stink bugs, and can be used in formulations such as emulsions, wettable powders, granules, emulsions, and sleep developing agents, but is not limited thereto.

The content of the first raw agent may be, for example, 0.1 to 20% by weight, preferably 1 to 15% by weight, and more preferably 5 to 10% by weight of the total weight of the composition, but is not limited thereto.

The water-soluble organic solvent has solubility in the first raw agent and may be mixed with water. In addition, the water-soluble organic solvent may have low volatility, and specifically, a boiling point of 80°C or higher, preferably 90°C or higher, and more preferably 100°C or higher, but is not limited thereto.

The water-soluble organic solvent is a water-soluble organic solvent capable of evenly dispersing the first raw agent, improving disintegration when hydrated in water, and improving suspension properties so that precipitation of the first raw agent does not occur at high or low temperatures. , For example, N-methylpyrrolidone, butanediol, 2-butoxyethanol, dimethyl glycol, dimethyl sulfoxide, 1,4-dioxane, perfuryl alcohol, N, N-dimethylacetamide, propane At least selected from the group consisting of triol, pentanediol, propylene glycol, tetrahydrofuran, triethylene glycol, propylene glycol monomethyl ether, dipropylene glycol monomethyl ester, dipropylene glycol monomethyl ether, and dipropylene glycol monoethyl ether It may be one, preferably at least one selected from the group consisting of N-methylpyrrolidone, N, N-dimethylacetamide, propylene glycol monomethyl ether, dipropylene glycol monomethyl ether, and dipropylene glycol monoethyl ether May be, and more preferably, at least one of N-methylpyrrolidone or N, N-dimethylacetamide, but is not limited thereto.

In the case of the N-methylpyrrolidone, N, N-dimethylacetamide, propylene glycol monomethyl ether, dipropylene glycol monomethyl ether and dipropylene glycol monoethyl ether, it is possible to mix with water without a surfactant, and N- In the case of methylpyrrolidone or N, N-dimethylacetamide, oiling may not occur.

The content of the water-soluble organic solvent may be, for example, 0.1 to 15% by weight, preferably 1 to 10% by weight, and more preferably 4 to 6% by weight of the total weight of the composition, but is not limited thereto.

In addition, according to an embodiment of the present invention, the content of the water-soluble organic solvent may be 30 to 200 parts by weight, preferably 40 to 150 parts by weight, more preferably 50 to 100 parts by weight, relative to the first raw agent, It is not limited thereto.

The content of the water-soluble organic solvent takes into account the stability of layer separation, solidification, and precipitation at room temperature and low temperature.If the water-soluble organic solvent is less than 30 parts by weight compared to the first raw agent, the amount of the solvent is small and the original agent is deposited. In addition, when it exceeds 200 parts by weight, it may exceed the adsorption capacity of the granular hydration agent, making it difficult to prepare the granular hydration agent.

Further, according to an embodiment of the present invention, the content of the first raw agent and the water-soluble organic solvent may be 1 to 25 parts by weight, preferably 5 to 20 parts by weight, more preferably 10 to 15 parts by weight, relative to the particles. However, it is not limited thereto.

It is easy to prepare a granular hydration agent without deterioration in physical properties, suspension properties, disintegration properties, etc. within the content range of the first raw agent and the water-soluble organic solvent.

In addition, the particles may have a particle diameter of 0.5 to 1.1 mm, preferably 0.6 to 1.0 mm, more preferably 0.7 to 0.9 mm, but are not limited thereto.

When the particle diameter of the particles is increased, the suspension properties and disintegration properties may be deteriorated, and when the particle diameter is decreased, production of the particles is difficult, which may be undesirable in terms of efficiency.

In addition, the particles may include a member.

The member may be at least one from the group consisting of a surfactant, a wetting agent, a disintegrant and a carrier.

The surfactant may be liquid or solid, and may be a nonionic surfactant, an anionic surfactant, a cationic surfactant, an amphoteric surfactant, or the like.

The nonionic surfactant is, for example, polyoxyalkylene glycol, polyoxyalkylene alkyl ether, polyoxyalkylene alkylaryl ether, polyoxyalkylene fatty acid ester, polyoxyethylene polyoxypropylene block polymer, sorbitan Monoalkylates, alkynols and alkynediols and their alkylene oxide adducts, sorbitan fatty acid esters, polyoxyethylene sorbitan fatty acid esters, sucrose fatty acid esters, polyoxyethylene fatty acid esters, polyoxyethylene resin acid esters, polyoxyethylene Fatty acid diester, polyoxyethylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxyethylene dialkyl phenyl ether, polyoxyethylene alkyl phenyl ether formalin condensate, polyoxyethylene polyoxypropylene block copolymer, alkyl polyoxyethylene poly Propylene block copolymer ether, polyoxyethylene alkylamine, polyoxyethylene fatty acid amide, polyoxyethylene fatty acid bisphenyl ether, polyalkylene benzylphenyl ether, polyoxyalkylene styrylphenyl ether, acetylenediol, polyoxyalkylene addition acetylene Diol, polyoxyethylene ether silicone, ester silicone, fluorine-based surfactant, polyoxyethylene castor oil, polyoxyethylene hydrogenated castor oil may be, but is not limited thereto.

The anionic surfactant is, for example, alpha olefin sulfonic acid, alkyl sulfuric acid, alkyl sulfonic acid, alkyl phosphoric acid, alkyl phosphonic acid, alkyl aryl sulfonic acid, alkyl aryl phosphonic acid, polyoxyalkylene alkyl ether sulfuric acid ester, polyoxyalkylene alkyl Alkali of aryl ether sulfate, polyoxyalkylene alkyl ether phosphate, polyoxyalkylene alkyl aryl ether phosphate, polycarboxylate type polymer, lignin sulfonic acid, aryl sulfonic acid, aryl sulfonic acid formalin condensate, alkylarylsulfonic acid formalin condensate Metal salt, alkaline earth metal salt, ammonium salt, alkyl sulfate, polyoxyethylene alkyl ether sulfate, polyoxyethylene alkylphenyl ether sulfate, polyoxyethylene styrylphenyl ether sulfate, alkylbenzene sulfonate, lignin sulfonate, alkyl sulfosuccinate, Naphthalenesulfonic acid salt, alkylnaphthalenesulfonic acid salt, salt of formalin condensate of naphthalenesulfonic acid, salt of formalin condensate of alkylnaphthalenesulfonic acid, fatty acid salt, polycarboxylate, N-methyl-fatty acid sarcosinate, resin acid salt, polyoxyethylene alkyl It may be an ether phosphate, a polyoxyethylene alkylphenyl ether phosphate, and the like, but is not limited thereto.

The cationic surfactant is, for example, alkylamine, polyalkylamine, alkanolamine, polyalkanolamine, polyalkylene polyamine, alkylpyridine, alkylmorpholine, alkyl hydrazine hydrochloride, sulfate, carboxylate, and Urylamine hydrochloride, stearylamine hydrochloride, oleylamine hydrochloride, stearylamine acetate, stearylaminopropylamine acetate, alkyltrimethylammonium chloride, alkyldimethylbenzalkonium chloride, and the like, but are not limited thereto.

In addition, the amphoteric surfactant may be, for example, an amino acid type or a betaine type, but is not limited thereto. In addition, these surfactants can be used alone or in combination of two or more.

The content of the surfactant may be, for example, 0.1 to 20% by weight, preferably 1 to 15% by weight, more preferably 5 to 10% by weight of the total weight of the composition, and more specifically, the liquid surfactant. In the case, the content thereof may be, for example, 1 to 7% by weight, preferably 2 to 6% by weight, more preferably 3 to 5% by weight of the total weight of the composition, and in the case of a solid surfactant, its The content may be, for example, 0.1 to 6% by weight, preferably 1 to 5% by weight, and more preferably 2 to 4% by weight of the total weight of the composition, but is not limited thereto.

The surfactant may be used for various purposes to improve wettability, dispersibility, and permeability, but is not limited thereto.

The wetting agent may be, for example, a dioctyl sulfo succinate, an alkyl sulfate, a POE alkyl ether, a POE aryl ether, an acetylene diol, or a PO/EO block polymer, but is not limited thereto.

The content of the wetting agent may be, for example, 0.1 to 4% by weight, preferably 1 to 3% by weight, and more preferably 1.5 to 2.5% by weight of the total weight of the composition, but is not limited thereto.

The disintegrant is, for example, carboxymethylcellulose sodium salt, dextrin, water-soluble starch, xanthan gum, guacid gum, sucrose, polyvinylpyrrolidone, polyvinyl alcohol, sodium polyacrylate, polyacrylate with an average molecular weight of 6000 to 5 million. It may be oxyethylene, urea-formaldehyde resin, etc., but is not limited thereto.

In addition, the content of the disintegrant may be 0.1 to 10% by weight, preferably 2 to 8% by weight, more preferably 4 to 6% by weight of the total weight of the composition, but is not limited thereto.

The carrier may be a solid carrier or a liquid carrier.

The solid carrier is, for example, mineral soil, such as silica gel, silicate, talc, ataclay, limestone, lime, chalk, church clay, ocher, clay, dolomite, diatomaceous earth, calcium sulfate, magnesium sulfate, magnesium oxide, crushed Synthetic substances, fertilizers such as ammonium sulfate, ammonium phosphate, ammonium nitrate, urea, and products of vegetable origin, such as grain meal, bark meal, wood meal and nutshell meal, cellulose powder, bentonite, kaolin, sericite, talc, acidic It may be clay, pumice, zeolite, vermiculite, pearlite, calcium carbonate, silica sand, white carbon, and the like.

In addition, the liquid carrier is, for example, monohydric alcohols such as methanol, ethanol, propanol, isopropanol, butanol, ethylene glycol, diethylene glycol, propylene glycol, hexylene glycol, polyethylene glycol, polypropylene glycol, glycerin, etc. Polyhydric alcohols, polyhydric alcohol compounds such as propylene glycol ether, ketones such as acetone, methyl ethyl ketone, methyl isobutyl ketone, diisobutyl ketone, and cyclohexanone, ethyl ether, dioxane, ethylene glycol monoethyl ether, di Ethers such as propyl ether and tetrahydrofuran, aliphatic hydrocarbons such as normal paraffin, naphthene, isoparaffin, kerosene and mineral oil, aromatic hydrocarbons such as benzene, toluene, xylene, solvent naphtha, alkylbenzene, and alkyl naphthalene, Halogenated hydrocarbons such as dichloromethane, chloroform, and carbon tetrachloride; esters such as ethyl acetate, diisopropylphthalate, dibutylphthalate, dioctylphthalate, and dimethyl adipate; lactones such as γ-butyrolactone; dimethylformamide , Diethylformamide, dimethylacetamide, amides such as N-alkylpyrrolidinone, nitriles such as acetonitrile, sulfur compounds such as dimethyl sulfoxide, vegetable oils such as soybean oil, rapeseed oil, cottonseed oil, and castor oil , Water, etc., but is not limited thereto. The carrier may be used alone or in combination of two or more.

The content of the carrier may be, for example, 40 to 70% by weight, preferably 45 to 65% by weight, more preferably 50 to 60% by weight of the total weight of the composition, but is not limited thereto.

In addition, according to an embodiment of the present invention, the particles may further include a second raw agent.

The second agent may be a known pesticide or pesticide agent such as an insecticide, a fungicide, or a herbicide.

The pesticides are, for example, acrinathrin, acetamiprid, acephate, amitraz, alanikab, arimarua, alumigelure, isoxacion, imidacroprid, phosphorus Doxacarb MP, uwabarua, ethylthiomethone, ethoxazole, etopenprox, emamectin benzoate, oxamyl, orifurua, sodium oleate, carbamate ammonium salt, carbamate sodium salt, cardusafos , Cartap hydrochloride, carbosulfan, clotianidine, clopentezine, chromafenozide, chloropicrin, chlorpyriphos, chlorpyrophosmethyl, chlorfenapyr, chlorfluazuron, diatomaceous earth, fenbuta Tin oxide, dienochlor, cycloprothrin, dinotephran, cyhalothrin, cyfluthrin, diflubenzrone, cypermethrin, fatty acid glyceride, dimethoate, methyl bromide, silafofen, chlor Margin, spinosad, spirodiclofen, sulpropos, diazinone, diamolure, thiaclopride, thiamethoxam, thiodicarb, thioclam, thiometone, cheritoria, tetra Dipon, Tetradecenyl Acetate, Tebufenozide, Tefufenpyrad, Tefluthrin, Teproubenjuron, Tralomethrin, Tolfenpyrad, Nitenpyram, Pastria Penetrance, Halfenprox, Peach Peachflure, phytoamirua, bifenazate, bifenthrin, pymetrozine, pyraclofos, pyridapentione, pyridaben, pyridaryl, pyrimarua, pyrimidifen, pyri Mifosmethyl, pyrethrin, fipronil, phenothiocarb, fenvalerate, fenproxymate, fenpropathrin, buprofezin, prathiocarb, fluacrypyrim, flucitrinate, fluvalinate , Fluphenoxrone, prothiophos, propaphos, propylene glycol fatty acid ester, propenophos, hexythiazox, permethrin, bensultap, benzoepine, benpracarb, fosalone, postizate, machine oil (machine oil), marathon, milbemectin , Mesomyl, metaaldehyde, methyl isothiocyanate, methoxyfenozide, litlure, lufenuron, rotenone (derris), BPMC, BPPS, BRP, BT, CYAP, DD, DCIP, DDVP , DEP, DMTP, ECP, EPN, MEP, MPP, NAC, PAP, XMC, etiprol, etc., but are not limited thereto.

In addition, the fungicides are, for example, azoxystrobin, amorphine, sulfur, isoprothiorane, ifconazole, iprodione, imine octadine albecylate, imine octadine acetate, imibenconazole, ecromesol, Oxadicil, oxytetracycline, oxpoconazole fumarate, oxonic acid, kasugamycin, capropamide, kinoxarine, captop, cresoxime methyl, cyazofamide, shiitake mushroom mycelium extract, dietopencarb, diclo Cymet, Diclomedin, Dititanone, Cyfenoconazole, Cyproconazole, Cyflufenamide, Cyprodinil, Simeconazole, Dimethomorph, Simoxanil, Pseudomonas bacteria CAB-02 strain, Jiram, Strept Mycin, lime sulfur compound, dazomet, potassium hydrogen carbonate, sodium hydrogen carbonate, thiadiazine, thiadinil, thiabendazole, thiuram, thiophanate methyl, thifluzamide, teclophthalam, tebuconazole, Tetraconazole, basic copper chloride, basic copper sulfate, cupric hydroxide, triadimephone, triazine, tricoderma atropiride SKT-1, tricyclazole, triprumisol, trifoxystrobin, tripoline , Triclofosmethyl, rapeseed oil, copper nonylphenolsulfonic acid, Bacillus subtiris (live bacteria), validamycin, bitertanol, hydroxyisoxazole, non-pathogenic ervinia cartovora, pyriphenox, pyribencarb, fatigue Quilon, famoxadon, phenarimol, phenoxanil, perimuzol, ferimzone, fenbuconazole, fenhexamide, phthalide, blasticidin S, flametpyr, fluazinam, fluorimide , Fludioxonil, flusulfamide, flutoranil, prochloraz, procymidone, propamocarb hydrochloride, propiconazole, propineb, probenazole, hexaconazole, benomyl, peprazo Eight, Pensichron, Benthiavalicarb Isopropyl, Fosetyl, Polyoxine, Polycarbamate, Manzeb, Mannev, Mildiomycin, Anhydrous Copper Sulphate, Metalaxyl, Metominostrobin, Mepanipyrim, Mepro Neil, organo-copper, DBEDC, EDDP, IBP, TPN, boscalid, etc. may be, preferably pyribencarb, bentiavalicarbisopropyl, iminoxine albecylate, mepanipyrim, mepronil. , It is not limited thereto.

The herbicides are, for example, ioxynil, azimsulfuron, ashlam, atrazine, anilofos, arachrol, isoxaben, isouron, imazamox ammonium salt, imazosulfuron, indanophane , Esprocarb, ethoxysulfuron, ethobenzanide, chlorate, oxadizone, oxaziclomefon, carfenstrol, carbutylate, chizalohofethyl, cumyluron, glyphosate ammonium salt, gla Iposate sodium salt, glufosinate, clethodim, clomeprof, cyanazine, sodium cyanate, cyclosulfamuron, diquat#183#dibromide, cidurone, cyhalofopbutyl, diflufeny Can, Dimethamethrin, Dimethenamide, Cymethrin, Dimepiperate, Cetoxydim, Terbacil, Dimuron, Thifensulfuronmethyl, Desmedipam, Tenylchlor, Tebuthiuron, Tepraoxidim ( tepraloxydim), triflularine, nicosulfuron, paraquat, halosulfuronmethyl, bialaphos, bispyribac sodium salt, bifenox, pyrazoxyfen, pyrazosulfuronethyl, pyrazolate, pyraflufenethyl, Pyriphthalide, Pyributicarb, Pyrimisluphan, Pyriminobakmethyl, Pyroxasulfone, Fenoxapropethyl, Pentrazamide, Penmedipam, Butacrol, Butamifos, Plaza Sulfuron , Fluazifop P, Pretyracrol, Bromasyl, Promethrin, Bromobutide, Bensulfuronmethyl, Benzobicyclone, Benzofenaf, Bentazone, Benthiocarb, Pendimetharine, Pentoxazone, Benpure Sate, metamitron, metracrole, metribuzin, mefenacet, morinate, reneuron, and the like, but are not limited thereto.

The content of the second raw agent may be, for example, 5 to 30% by weight, preferably 10 to 25% by weight, more preferably 15 to 20% by weight of the total weight of the composition, but is not limited thereto.

In one embodiment of the present invention, the particles adsorbing the first raw agent and the water-soluble organic solvent may be prepared by adsorbing a mixture of the first raw agent and the water-soluble organic solvent on the dried particles.

The composition of the present invention does not deteriorate the suspension properties, disintegration properties, and physical properties by not including the first raw agent in the process of drying the particles.

Further, according to an embodiment of the present invention, the drying may be performed at 55 to 80°C, preferably 57 to 70°C, and more preferably 59 to 65°C, but is not limited thereto.

In addition, the composition according to an embodiment of the present invention may include other additives or adjuvants such as a binder, a thickener (extender), and an anti-decomposition agent of the original agent in order to improve the stability or functionality of the first agent in addition to the member. It is not limited.

The binder is, for example, carboxymethylcellulose sodium salt, dextrin, water-soluble starch, xanthan gum, guacid gum, sucrose, polyvinylpyrrolidone, polyvinyl alcohol, polyacrylate sodium salt, polyoxygen having an average molecular weight of 6000 to 5 million. It may be ethylene or the like, but is not limited thereto. These binders can be used alone or in combination of two or more.

In addition, the thickener (extender) is, for example, xanthan gum, guar gum, carboxymethylcellulose, polyvinylpyrrolidone, carboxyvinyl polymer, acrylic polymer, vegetable powder (soybean flour, tobacco powder, wheat flour, wood flour, etc.) ) Or organic acids (citric acid, succinic acid, maleic acid, etc.) or salts, urea, and water-soluble substances such as sugars [lactose (lactose), glucose, sucrose, etc.], mineral powders or inorganic powders (fumed silica, white carbon (White carbon)), kaolin, bentonite), acid clay, clay such as clay, talc, pyrophyllite, talc, diatomaceous earth, dolomite, silica, minerals such as alumina, processing materials such as sulfur, activated carbon, potassium chloride, It may be an inorganic salt such as ammonium sulfate, calcium carbonate, sodium hydrogen carbonate, sodium sulfate, magnesium carbonate, etc., and preferably minerals or clays. However, it is not limited thereto. These thickeners can be used alone or in combination of two or more. The thickener may be used to improve the physical properties of the first raw agent or to control the concentration, but is not limited thereto.

In addition, the decomposition inhibitor may be, for example, a zeolite, quicklime, a drying agent such as magnesium oxide, a phenol compound, an amine compound, a sulfur compound, an antioxidant such as a phosphoric acid compound, a salicylic acid compound, a UV absorber such as a benzophenone compound, etc. It is not limited thereto. These decomposition inhibitors may be used alone or in combination of two or more.

In addition, the present invention provides a step of obtaining a mixture of a first raw agent and a water-soluble organic solvent; Adding water to the member and kneading to form particles; Drying the particles at a temperature exceeding the melting point of the first raw agent; And adsorbing the mixture on the dried particles.

According to an embodiment of the present invention, it is possible to overcome the difficulty in preparing a granular wettable pesticide composition of a low melting point raw agent due to the phenomenon that the first raw agent melts and aggregates as the drying temperature exceeds the melting point of the first raw agent. .

In an embodiment of the present invention, the first raw agent may be, for example, a melting point of 26 to 54°C, preferably 28 to 52°C, more preferably 30 to 50°C, but is limited thereto. It is not.

In addition, the first agent is etopenprox, cycleoxydim, benfurecite, cyhalopopbutyl, diclopopmethyl, dimethoate, dimethachlor, alacrore, esfenvalerate, penvalerate , Lambdacyhalothrin, chloropyrophos, tefluthrin, trifluralin, fenpropatrin, and prochloraz may be at least one selected from the group consisting of, but is not limited thereto.

In addition, in one embodiment of the present invention, the water-soluble organic solvent is N-methylpyrrolidone, butanediol, 2-butoxyethanol, dimethyl glycol, dimethyl sulfoxide, 1,4-dioxane, perfuryl Alcohol, N, N-dimethylacetamide, propanetriol, pentanediol, propylene glycol, tetrahydrofuran, triethylene glycol, propylene glycol monomethyl ether, dipropylene glycol monomethyl ester, dipropylene glycol monomethyl ether and dipropylene May be at least one selected from the group consisting of glycol monoethyl ether, preferably N-methylpyrrolidone, N, N-dimethylacetamide, propylene glycol monomethyl ether, dipropylene glycol monomethyl ether, and dipropylene glycol It may be at least one selected from the group consisting of monoethyl ether, more preferably at least one of N-methylpyrrolidone or N, N-dimethylacetamide, but is not limited thereto.

In one embodiment of the present invention, the water-soluble organic solvent may be a mixture of 30 to 200 parts by weight, preferably 40 to 150 parts by weight, more preferably 50 to 100 parts by weight, relative to the first raw agent. It is not limited.

The mixing ratio of the water-soluble organic solvent takes into account the stability of layer separation, solidification, and precipitation at room temperature and low temperature, and when the water-soluble organic solvent is less than 30 parts by weight, the content of the solvent is small and the original agent may be precipitated. If it exceeds a part by weight, it may exceed the adsorption capacity of the granular hydrating agent, making it difficult to prepare the granular hydrating agent.

According to an embodiment of the present invention, the adsorption may be to adsorb a mixture of 1 to 25 parts by weight, preferably 5 to 20 parts by weight, more preferably 10 to 15 parts by weight, based on the dried particles. It is not limited.

It is easy to prepare a granular hydrating agent without deterioration in physical properties, suspension properties, disintegration properties, etc. within the ratio of the dried particles and the mixture.

According to an embodiment of the present invention, a surfactant may be mixed together in the step of mixing the first raw agent and the water-soluble organic solvent, but is not limited thereto.

In addition, in the manufacturing method according to an embodiment of the present invention, the member may be at least one selected from the group consisting of a surfactant, a wetting agent, a disintegrant, a thickener, and a carrier. The member may be within the above-described range.

According to an embodiment of the present invention, when water is added to the member, a second raw agent may be further added. The second raw material may be within the above-described range.

In addition, the manufacturing method according to an embodiment of the present invention may further include heating and dissolving the first raw material before mixing the first raw material and the water-soluble organic solvent.

By heating the first raw material before mixing, the degree of mixing of the first raw material and the water-soluble organic solvent may be improved.

The heating may be heating at a temperature exceeding the melting point of the first raw agent.

In addition, the manufacturing method according to an embodiment of the present invention may further include pulverizing the member before adding water to the member.

The manufacturing of the particles may be facilitated through the process of pulverizing the member.

In addition, in an embodiment of the present invention, the particles may have a particle diameter of 0.5 to 1.1 mm, preferably 0.6 to 1.0 mm, more preferably 0.7 to 0.9 mm, but are not limited thereto.

When the particle diameter of the particles is increased, the suspension properties and disintegration properties may be deteriorated, and when the particle diameter is decreased, production of the particles is difficult, which may be undesirable in terms of efficiency.

In one embodiment of the present invention, the temperature exceeding the melting point may be 55 to 80°C, preferably 57 to 70°C, and more preferably 59 to 65°C, but is limited thereto. It is not.

In addition, the drying may be performed for 1 to 20 minutes, preferably for 5 to 15 minutes, more preferably for 8 to 12 minutes, but is not limited thereto.

Hereinafter, examples will be described in detail to illustrate the present invention in detail.

Example

1. Manufacturing example

(1) Comparative Example 1

The pesticide raw material was prepared using etopenprox with a low melting point at 45°C. Etopenprox original agent (8.6% by weight) was heated (60°C) and adsorbed to zeolite (thaw, 30% by weight), and then pulverized three times using a hammer mill to prepare an adsorption unit. Buprofezin (17% by weight), Tersperse 2700 (Huntsman, 4% by weight), Terwet 1004 (Huntsman, 2% by weight), UF-100F (Yusung Hwayeontech, 5% by weight) and Kaolin (Bunam) were mixed, The mixture was mixed with the pulverized adsorption unit, crushed with a hammer mill, and then granulated and dried at 60°C for 10 minutes. The content of each component of Comparative Example 1 was as shown in Table 1 below.

ingredient weight% Etofenprox 8.6 Buprofezin 17.0 Tersperse 2700 4.0 Tewet 1004 2.0 CR-UF100F 5.0 Zeolite 30.0 Kaoline 33.4 Total 100

When prepared according to Comparative Example 1, due to the nature of the low melting point pesticide with a low melting point, the pulverization was not smooth due to the melting phenomenon of the original Etopen Prox, and a phenomenon that did not collapse from the application of a drying temperature of 40°C after granulation and molding occurred. Processing of the granular water agent was difficult.

(2) Comparative Examples 2 and 3

5% by weight of alkylbenzene (Comparative Example 2) or methyl oleate (Comparative Example 3), which are oil-soluble solvents, together with PCO2 (Geoyoung, 3% by weight) by heating (60°C) Etopenprox original agent (8.6% by weight) The liquid portion was prepared using. As an assembly part, viewprofezin (17% by weight), Tersperse 2700 (Huntsman, 4% by weight), Terwet 1004 (Huntsman, 2% by weight), UF-100F (Yoosung Hwayeontech, 5% by weight), white carbon (Jeosil, 8% by weight) and kaolin (bunam) were mixed and pulverized in total, and then added together with the liquid portion to be granulated into 0.8mm, and dried at 40°C and 50°C to within 2.5% moisture content, respectively. The contents of each component of Comparative Examples 2 and 3 were shown in Table 2 below.

ingredient Comparative Example 2 Comparative Example 3 Etopenprox 8.6 8.6 Beauprofezin 17.0 17.0 Alkylbenzene 5.0 - Methyl oleate - 5.0 AG-PCO2 3.0 3.0 T-2700 4.0 4.0 T-1004 2.0 2.0 CR-UF100F 5.0 5.0 White carbon 8.0 8.0 Kaolin 47.4 47.4 Sum 100 100

When manufactured according to the conventional techniques of Comparative Examples 2 and 3, there was no problem in the drying temperature, but when stored for 1 week at low temperature (refrigerated storage), there was a problem that the disintegration property was lowered. After all of the collapse proceeded, it was confirmed that oil remnant occurred in the wet sieve test through a 325 mesh sieve.

(3) Comparative Examples 4 and 5

It was carried out in the same content ratio (Table 2) in Comparative Examples 2 and 3. 5% by weight of each of alkylbenzene (Comparative Example 4) or methyl oleate (Comparative Example 5), which are oil-soluble solvents, together with PCO2 (geoyoung, 3% by weight) by heating (8.6% by weight) of etopenprox The liquid portion was prepared using. As an assembly part, viewprofezin (17% by weight), Tersperse 2700 (Huntsman, 4% by weight), Terwet 1004 (Huntsman, 2% by weight) and UF-100F (Yoosung Hwayeontech, 5% by weight), white carbon (Jeosil, 8% by weight) and kaolin (bunam) were mixed and pulverized in total, and then hydrolyzed and granulated into 0.8 mm, dried at 60° C. for 10 minutes, and then prepared by adsorbing the liquid portion to the drying unit.

When prepared according to Comparative Examples 4 and 5, even when the mixture of the low melting point raw agent of the same composition ratio is adsorbed to the granular assembly, there is a problem that the disintegration property decreases as time elapses in low temperature storage at 0°C. I did. After all of the decay proceeded, it was confirmed that oil remnant occurred in the wet sieve test through a 325 mesh sieve.

(4) Examples 1 to 5

Etopenprox original agent (8.6% by weight) was heated (60°C), and N-methylpyrrolidone (Example 1), N, N-dimethylacetamide (Example 1), a water-soluble solvent together with PCO2 (geoyoung, 3% by weight), was heated (60°C). Example 2), propylene glycol monomethyl ether (Example 3), dipropylene glycol monomethyl ether (Example 4), and dipropylene glycol monoethyl ether (Example 5) 5% by weight, respectively, to prepare a liquid portion It was prepared in the same manner as in Comparative Examples 4 and 5. The content ratio of each component of Examples 1 to 5 was shown in Table 3 below.

ingredient Example 1 Example 2 Example 3 Example 4 Example 5 Etopenprox 8.6 8.6 8.6 8.6 8.6 Beauprofezin 17.0 17.0 17.0 17.0 17.0 N-methylpyrrolidone 5.0 - - - - NN-diacetamide - 5.0 - - - Propylene glycol monomethyl ether - - 5.0 - - Dipropylene glycol monomethyl ether - - - 5.0 - Dipropylene glycol monoethyl ether - - - - 5.0 AG-PCO2 3.0 3.0 3.0 3.0 3.0 T-2700 4.0 4.0 4.0 4.0 4.0 T-1004 2.0 2.0 2.0 2.0 2.0 CR-UF100F 5.0 5.0 5.0 5.0 5.0 White carbon 8.0 8.0 8.0 8.0 8.0 Kaolin 47.4 47.4 47.4 47.4 47.4 Sum 100 100 100 100 100

When prepared according to Examples 1 to 5, the liquid portion prepared using a solvent did not precipitate at room temperature on the day of manufacture, but propylene glycol monomethyl ether (Example 3) and dipropylene glycol monomethyl ether (Example 4), Dipropylene glycol monoethyl ether (Example 5) was separately confirmed that precipitation started after 24 hours at room temperature due to insufficient amount of solvent, but there was no problem in manufacturing a product with the same content.

2. Experimental example

(1) Physical property test of manufactured products

It is shown in Table 4 below for the disintegration, suspension, and grease occurrence of the pesticide compositions prepared according to Examples 1 to 5, and the occurrence of sebum after refrigeration at 0 to 4°C.

division Example 1 Example 2 Example 3 Example 4 Example 5 Disintegration Metropolitan Episode 25 Metropolitan City Episode 23 Metropolitan Episode 28 Metropolitan Episode 27 Inverted 30 times Suspension 86% 85% 83% 85% 80% Occurrence of retention Not occurring Not occurring Occurrence of trace amounts (less than 0.05%) Occurrence of trace amounts
(0.05% or less) Occurrence of trace amounts
(Less than 0.1%) Oiling occurs after refrigeration (0~4℃) Not occurring Not occurring Occurrence of trace amounts (less than 0.1%) Occurrence of trace amounts
(Less than 0.1%) Occurrence of trace amounts
(Less than 0.1%)

Each of the processed final products (Examples 1 to 5) had good disintegration and suspension properties, and even after one week of low temperature storage, the change in the amount of oil sediment did not show a significant change.

(2) Gaon abuse stability test

In the heating abuse stability test of Example 1, changes with time (Table 5) at intervals of 0, 2, 4, 6, and 8 weeks at 54±1°C were confirmed. As shown in Table 5 below, the decomposition rate of the original agent was less than 2%, showing that the decomposition rate was low and stable. In addition, the disintegration and suspension properties during hydration of Example 1 were good, and no seizure occurred.

Original title 0 weeks 2 weeks 4 weeks 6 weeks 8 weeks Etopenprox 8.28 8.26 (0.24%) 8.23
(0.6%) 8.20
(0.97%) 8.16
(1.45%) Beauprofezin 15.4 15.32 (0.52%) 15.28
(0.78%) 15.26
(0.91%) 15.21
(1.23%)

(3) Verification of insecticidal effect

In order to verify the insecticidal effect of Example 1, each test was performed in a pear test package in Anseong-si. Pear test varieties were reported, and the test method was repeated three times in a completely randomized design, and the control drug was diluted 1000 times in the same manner as in Example 1 using Amitraz. (Table 6, 7). In order to know the density of snapworms before treatment, the pre-density of snapworms (head/gut) was 63.0 for the test drug treatment, 54.7 for the control, and 55.3 for the no treatment (Tables 6 and 8). Branches for which the pre-density was investigated were separately marked, and the test drugs were applied respectively. In the investigation of the drug efficacy, the viability of podworm was investigated around the indicated branches 7 and 14 days after treatment.

Test drugs Original agent content (%) Drug efficacy test Weakness test Dilution factor and usage When and how to process Reference quantity Double Beauprofezin
.Etopenprox granular water hydration agent 23
(15+8) 1,000 times Foliage treatment twice every 7 days at the beginning of occurrence 1,000 times 500 times Amitraz.buprofezin emulsion (control) 25 1,000 〃 - - No treatment - - - - -

division Treated water Number of repetitions Total number Shares per ward Number of weeks required Total number of weeks required Drug efficacy 3 3 9 1 week 9 weeks 15 weeks Weak 3×2 3 18 1/3 week 6 weeks

division Survey items Number of investigations Date of investigation Investigation method Medicinal effect Viability Episode 2 14 Aug, 21 Aug, 28 Aug Investigation of the number of viable insects in 10 per mouth before and after 7 and 14 days of drug treatment Weak Weakness in appearance 3rd time 17 Aug, 19 Aug, 21 Aug After 3, 5, and 7 days of drug treatment, an investigation into whether there is any weakness in appearance

As a result of investigating the viability of podworm 7 days after drug treatment in the pear test package, 7.4, 7.9 of the control, and 109.0 of the non-treatment were found to be alive, and the control effect of 93.2% of the drug-treated and 92.8% of the control was observed. Shown (Table 9).

As a result of investigating the virulence rate of snapworms after 14 days, 9.4 animals in the test packaged treatment group, 9.8 animals in the control group, and 127.3 animals in the untreated group were found to be alive. (Table 10). In addition, the weakening of the improving drug did not show weakening in the reference amount and the double amount (Table 11). Based on the test results, it was confirmed that the improved buprofezin.etopenprox granular water hydration agent did not have any problems in terms of medicinal efficacy and weakness, and it was confirmed that it exhibited excellent effects in controlling pear insects.

Test drug Prior density
(Mari/go) Vitality rate (%) Significant difference
(DMRT) Control
(%) I repeat II repeat III repeat Average Beauprofezin
.Etopenprox granular water hydration agent 63.0 6.6 7.0 8.5 7.4 b 93.2 Amitraz.buprofezin emulsion (control) 54.7 9.3 7.4 7.1 7.9 b 92.8 No treatment 55.3 110.3 109.6 107.1 109.0 a

CV(%) ---------------------------------------------- ------- 3.2

Test drug Prior density
(Mari/go) Vitality rate (%) Significant difference
(DMRT) Control
(%) I repeat II repeat III repeat Average Beauprofezin
.Etopenprox granular water hydration agent 63.0 8.2 8.8 11.3 9.4 b 92.6 Amitraz.buprofezin emulsion (control) 54.7 7.4 13.0 8.9 9.8 b 92.3 No treatment 55.3 124.1 132.7 125.0 127.3 a

CV(%) ---------------------------------------------- ------ 6.8

Test drug Test crop
(kind) Weak degree (0-5) Remark Reference quantity Double Buprofezin. Etopenprox granular water hydration agent Apple
(Fuji, Hongro) 0 0 No weakness
(Daejeon, Anseong test packaging)

Claims (22)

delete delete delete delete delete delete delete delete delete delete Obtaining a mixture of a first raw agent and a water-soluble organic solvent;
Adding water to the member and kneading to form particles;
Drying the particles at a temperature exceeding the melting point of the first raw agent; And
Including; adsorbing the mixture to the dried particles,
The first raw agent is a method for producing a granular wettable pesticide composition having a melting point of 30 to 50°C.
delete The method of claim 11, wherein the first agent is etopenprox, cycleoxydim, benfuricite, cyhalopopbutyl, diclopopmethyl, dimethoate, dimethachlor, alacrore, esfenvalerate, Penvalerate, lambdacyhalothrin, chloropyrophos, tefluthrin, trifluralin, fenpropathrin and at least one selected from the group consisting of prochloraz, a method for producing a wettable pesticide composition.
The method according to claim 11, wherein the water-soluble organic solvent is N-methylpyrrolidone, butanediol, 2-butoxyethanol, dimethyl glycol, dimethyl sulfoxide, 1,4-dioxane, furfuryl alcohol, N, N- Consisting of dimethylacetamide, propanetriol, pentanediol, propylene glycol, tetrahydrofuran, triethylene glycol, propylene glycol monomethyl ether, dipropylene glycol monomethyl ester, dipropylene glycol monomethyl ether and dipropylene glycol monoethyl ether At least one selected from the group, a method for producing a granular wettable pesticide composition.
The method of claim 11, wherein the water-soluble organic solvent is mixed with 30 to 200 parts by weight compared to the first raw agent.
The method of claim 11, wherein the adsorption is to adsorb a mixture of 5 to 20 parts by weight based on the dried particles.
The method of claim 11, wherein the member is at least one selected from the group consisting of a surfactant, a wetting agent, a disintegrant, and a carrier.
The method of claim 11, further comprising heating and dissolving the first raw agent before mixing the first raw agent and the water-soluble organic solvent.
The method of claim 11, further comprising pulverizing the member before adding water to the member.
The method of claim 11, wherein the particles have a particle diameter of 0.5 to 1.1 mm.
The method of claim 11, wherein the temperature exceeding the melting point is 55 to 80°C.
The method of claim 11, wherein the drying is performed for 5 to 15 minutes.