WO2009089688A1 - Water soluble granule of fipronil and its preparation - Google Patents

Abstract

The invention provides a water soluble granule of fipronil. It is made from (by wt%) fipronil 0.5-50%, emulsifier 1-30%, dispersing agent 1-10%, wetting agent 1-5%, binder 2-4%, stabilizer 1-3% and the rest is filling material. The invention also provides the preparation method of the soluble granule of fipronil, which comprises kneading, extruding, granulating, vacuum drying at 70°C for 1 hour, screening and packaging. The product of the invention has a high insecticidal effect, is of low cost, is safe and convenient to use and is friendly to environment.

Description

 Insecticidal soluble granule containing fipronil and preparation method thereof

 The invention relates to a fipronil-containing insecticidal soluble granule and a preparation method thereof, in particular to a plant protection insecticide containing fipronil-containing insecticidal soluble granules and a preparation method thereof. Background technique

 With the continuous improvement of people's living standards, people's awareness of environmental protection, and the importance of the Chinese government's ecological environment, the domestic and international markets are efficient, low-toxic, low-residue, and non-polluting for crop pests and diseases. The demand for environmentally friendly bio-pesticide and chemical pesticides is increasing.

 There are many types of insecticides for plant protection, and emulsifiable concentrates and wettable powders are generally used. As we all know, emulsifiable concentrate contains a large amount of organic solvents, which are easy to volatilize and catch fire. It is toxic to humans and plants, pollutes the environment, and is inconvenient to transport. Wettable powders generate a large amount of dust during production and use, pollute the environment and affect the health of operators. .

 The pesticide preparation has been developed in the direction of no solvation, water-based, solidification and multi-functionality, and the insecticidal soluble granules of the present invention have been developed based on this development direction. Summary of the invention

 SUMMARY OF THE INVENTION An object of the present invention is to provide a safe, environmentally friendly, fipronil-containing insecticidal soluble granule for plant protection using the above-mentioned prior art.

 In order to solve the above technical problem, the present invention is achieved by the following technical solutions:

An insecticidal soluble granule containing fipronil consisting of fipronil, an emulsifier, a dispersing agent, a wetting agent, a binder, a stabilizer and a filler, and the composition of the soluble granule is 100% by weight The content is: fipronil 0.5~50%, emulsified Qi ljl~30%, dispersed Qiljl~10%, wetted ljl~5 %, bonded Qi 1J2~4%, stabilizer 1~3 %, the rest is filler. The emulsifier is selected from the group consisting of nonylphenol ethoxylates such as nonylphenol ethoxylates and octylphenol ethoxylates; benzylphenol ethoxylates and the like, such as benzylphenol polyoxygen Vinyl ether and benzyl nonylphenol ethoxylate; fatty alcohol polyoxyethylene ether and the like, such as C _n H _2n+1 0(EO) _m H, wherein n=12~16, m=15~30 , it is a product based on lauryl alcohol; sorbitol fatty acid ester and its epoxy acetamine adduct, such as Span-20, 40, 60, 65, 80, 85, Tween20, 21, 40, 60, 61, 65, 80, 81 and 85, etc.

 The dispersing agent is selected from the group consisting of decylnaphthalene sulfonate, such as pull-open powder BX and pull-open powder AC; bisnaphthalene sulfonate formaldehyde condensate, such as dispersant N and dispersant NO; and lignin sulfonic acid sodium.

 The wetting agent is selected from one or both of the mercaptobenzenesulfonate, the fatty acid amide N-methylsulfonate and the mercaptoaryl polyoxyethylene ether sulfate.

 The binder is selected from one or both of β-cyclodextrin, polyvinyl alcohol, methyl cellulose, glucose, and urea.

 The stabilizer is selected from one of sodium benzoate and glucose.

 The filler is selected from one or both of sodium hydrogencarbonate, anhydrous citric acid, maltose and anhydrous sodium sulfate.

 A method for preparing the above-mentioned fipronil-containing insecticidal soluble granules, comprising the following steps:

1 homogenization: the fipronil original drug is mixed with a binder and a wetting agent in water at 50 to 60 ° C, and stirred and homogenized under a high pressure of 420 to 450 kg/cm ² ;

 2 spraying the above-mentioned liquid mixture after homogenization to form a composite parent drug;

3 kneading: after the emulsifier is thermally dissolved, it is mixed with the dispersing agent, the stabilizer, the filler and the composite parent drug at a temperature of 45 to 50 ° C, and then stirred and kneaded under a pressure of 4 to 6 kg/cm ^{2 to} obtain Group agent

4 extrusion granulation: the group is extruded under the pressure of 6~12 kg / cm ² into columnar particles;

5 The columnar particles were vacuum dried at 70 ° C for 1 hour and sieved and shaped. Fipronil is a phenylpyrazole insecticide with a wide spectrum of insecticides. It is mainly used for stomach poisoning. It has both contact and certain systemic action. Its insecticidal mechanism is to hinder insect γ-aminobutyl. Acid controlled chloride Metabolism. Therefore, it has high insecticidal activity against important pests such as aphids, leafhoppers, planthoppers, lepidopteran larvae, flies and coleoptera, and is harmless to crops. The agent can be applied to the soil or foliar spray. Applying to the soil can effectively control corn roots, golden worms and tigers. When the leaf surface is sprayed, it has high level of control effect on Plutella xylostella, Pieris rapae and rice locust, and has a long-lasting effect.

 Compared with the existing mainstream insecticide dosage forms, the insecticide of the present invention does not contain or contains only a small amount of toxic and flammable aromatic hydrocarbon solvent, thereby avoiding flammable and explosive phenomena during production, storage and transportation. This dosage form has no unpleasant toxic odor, is less irritating to the eyes, reduces environmental pollution, and greatly improves the safety of production, storage, transportation and users. Therefore, after the industrialization is formed, not only the economic benefits are obvious, but also the development of high-tech green pesticide technology is promoted. It has obvious social benefits for promoting environmental protection and is the research direction of sustainable development.

 Soluble granules are a new type of formulation and are a comprehensive product with comprehensive properties in today's pesticide formulations. The successful development of soluble granules will further enhance their safety to the environment, humans and animals. The sources of various raw materials in the formulation are common in the domestic chemical market, and the product cost is low, thus laying a good foundation for the industrial production and popularization of the dosage form. detailed description

 The invention will now be further described in conjunction with specific embodiments.

 Example 1

 The fipronil-containing insecticidal soluble granules of the present invention are prepared as follows:

1 mixing 0.5% of fipronil original drug with 1% polyvinyl alcohol and 4% sodium dodecylbenzenesulfonate in 55 ° C water, and stirring and homogenizing under 420 kg / cm ² high pressure;

 2 spraying the above-mentioned liquid mixture after homogenization to form a composite parent drug;

3 After heat dissolving 3% nonylphenol ethoxylate, with 3% dispersant NO, 1% sodium benzoate, 46% sodium bicarbonate, 41.5% anhydrous citric acid and compound parent drug at 45 Mixing at a temperature of °C, stirring at a pressure of 4 kg/cm ² and kneading uniformly to obtain a bolus;

4 extruding the bolus at a pressure of 6 kg / cm ² into columnar particles; 5 The columnar particles are vacuum dried at 70 ° C for 1 hour and then sieved. The sieved product is packaged after testing; the product that cannot pass through the sieve is repeated after the above process is tested and packaged.

 Formulated according to the above ratio, using 300g per acre, for rice pests, stem borer, stem borer, rice

Example 2

 The fipronil-containing insecticidal soluble granules of the present invention are prepared as follows:

1 Mix 10% of fipronil original drug with 1.2% β-cyclodextrin and 4% fatty acid amide 甲基-methanesulfonate in 50 ° C water, and stir at 430 kg / cm ² high pressure. ;

 2 spraying the above-mentioned liquid mixture after homogenization to form a composite parent drug;

3 After thermally dissolving 6% biphenol polyoxyethylene ether and 2% benzylphenol polyoxyethylene ether, with 0.8% sodium lignosulfonate, 1% borax, 42% sodium hydrogencarbonate, 33% The anhydrous sodium sulfate and the composite parent drug are thermally mixed at a temperature of 45 ° C, stirred at a pressure of 5 kg / cm ² , and kneaded uniformly to obtain a bolus;

4 squeezing the granules into columnar granules under a pressure of 8 kg/cm ² ;

 5 The columnar particles are vacuum dried at 70 ° C for 1 hour, and then sieved. The sieved product is packaged after testing; the product that cannot pass through the sieve is repeated after the above process is tested and packaged.

Formulated according to the above ratio, 14g per acre has good control effect on rice pests, stem borer, stem borer and rice leaf roller, and the control effect is shown in the following table. Preparation of pharmaceutical 10% fipronil water-soluble granules control agent 5% fipronil water dispersion granules dosage 14g / mu 35g / mu

 Rice leaf

 Control object, mites, mites, mites, mites, mites, mites, rice

 Control effect (%) 97.07 98.25 95.13 96.43 97.78 92.25 Example 3

 The fipronil-containing insecticidal soluble granules of the present invention are prepared as follows:

1 Mix 30% of fipronil original drug with 1% methylcellulose, 4% sodium dodecylnaphthalene sulfonate in 60 ° C water, and stir and homogenize under 440 kg / cm ² high pressure;

2 spraying the above-mentioned liquid mixture after homogenization to form a composite parent drug;

3 After thermally dissolving 9% of benzyl nonylphenol ethoxylate, 2% sorbitol fatty acid ester and its epoxy oxime adduct, with 3% pull-open powder BX, 1% borax, 20% maltose, 30% anhydrous citric acid and the composite parent drug are thermally mixed at a temperature of 50 ° C, and then stirred and kneaded under a pressure of 6 kg / cm ^{2 to} obtain a bolus;

4 extruding the bolus into a columnar pellet under a pressure of 10 kg/cm ² ;

 5 The columnar particles are vacuum dried at 70 ° C for 1 hour, and then sieved. The sieved product is packaged after testing; the product that cannot pass through the sieve is repeated after the above process is tested and packaged.

 According to the above ratio, the preparation is 5g, and the control effect of rice worm, rice stem borer, stem borer and rice leaf roller is 5g per acre. The control effect is shown in the following table.

Example 4

The fipronil-containing insecticidal soluble granules of the present invention are prepared as follows: 1 Mix 50% of fipronil with 2% β-cyclodextrin, 4% decyl aryl polyoxyethylene ether sulfate in 55 ° C water, stir at 450 kg / cm ² high pressure quality;

 2 spraying the above-mentioned liquid mixture after homogenization to form a composite parent drug;

3 After heat dissolving 9% of fatty alcohol polyoxyethylene ether and 4% octylphenol polyoxyethylene ether, with 1% of open powder AC, 2% of dispersant N, 1% of borax, 15% Maltose, 12% anhydrous citric acid and the composite parent drug are heat-mixed at a temperature of 45 ° C, stirred at a pressure of 6 kg / cm ² , and kneaded uniformly to obtain a bolus;

4 extruding the bolus at a pressure of 12 kg / cm ² into columnar particles;

 5 The columnar particles are vacuum dried at 70 ° C for 1 hour, and then sieved. The sieved product is packaged after testing; the product that cannot pass through the sieve is repeated after the above process is tested and packaged.

 Formulated according to the above ratio, 3.2g per acre is effective against rice pests, stem borer, stem borer, and rice leaf roller, and the control effect is shown in the following table.

Industrial applicability

 The fipronil water-soluble granule of the present invention has high insecticidal activity against important pests such as aphids, leafhoppers, planthoppers, lepidopteran larvae, flies and coleoptera, and has no phytotoxicity to crops. The agent can be applied to the soil or sprayed on the surface. Applying to the soil can effectively control corn roots, golden worms and tigers. When the leaf is sprayed, it has high level of control effect on Plutella xylostella, Pieris rapae and rice locust, and has a long-lasting effect. Although the present invention has been described in connection with the preferred embodiments, it will be apparent to those skilled in the art that changes and modifications can be made to the selection and ratio of similar compounds. However, as compared with the present invention, such modifications are still within the scope of the present invention as long as their effects are the same as or similar to those of the present invention.

Claims

Rights request

 An insecticidal soluble granule containing fipronil characterized by fipronil, an emulsifier, a dispersing agent, a wetting agent, a binder, a stabilizer and a filler, and the weight of the soluble granule is 100%, the composition content is: fipronil 0.5~50%, emulsifier 1~30%, dispersant 1~10%, wetting agent 1~5 %, binder 2~4%, stabilizer 1 ~3 %, the rest is filler.

 The fipronil-containing insecticidal soluble granule according to claim 1, wherein the emulsifier is selected from the group consisting of nonylphenol ethoxylates, benzylphenol ethoxylates and the like, fat Alcohol polyoxyethylene ethers and the like, and sorbitol fatty acid esters and their epoxy oxime adducts.

 The fipronil-containing insecticidal soluble granule according to claim 2, wherein the nonylphenol ethoxylate is selected from the group consisting of nonylphenol ethoxylates and octylphenol ethoxylates.

 The fipronil-containing insecticidal soluble granule according to claim 2, wherein the benzyl phenol polyoxyethylene ether and the analogue are selected from the group consisting of benzyl phenol polyoxyethylene ether and benzyl nonyl phenol Polyoxyethylene ether.

The fipronil-containing insecticidal soluble granule according to claim 2, wherein the fatty alcohol ethoxylate and the analog are selected from the group consisting of C _n H _2n+1 0 (EO) _m H , wherein , n=12~16, m=15~30.

 The fipronil-containing insecticidal soluble granule according to claim 2, wherein the sorbitol fatty acid ester and its epoxy oxime adduct are selected from the group consisting of Span-20, 40, 60, 65 , 80, 85, Tween20, 21, 40, 60, 61, 65, 80, 81 and 85.

 The fipronil-containing insecticidal soluble granule according to claim 1, wherein the dispersing agent is selected from the group consisting of decylnaphthalene sulfonate, bisnaphthalene sulfonate formaldehyde condensate, and lignin sulfonate. Sodium.

 The fipronil-containing insecticidal soluble granule according to claim 8, wherein the decylnaphthalene sulfonate is selected from the group consisting of a pull-up powder BX and a pull-up powder AC.

 The fipronil-containing insecticidal soluble granule according to claim 8, wherein the bisnaphthalenesulfonate formaldehyde condensate is selected from the group consisting of a dispersant N and a dispersant N O .

10. The fipronil-containing insecticidal soluble granule according to claim 1, characterized in that The wetting agent is selected from one or both of mercaptobenzenesulfonate, fatty acid amide N-methylsulfonate and mercaptoaryl polyoxyethylene ether sulfate.

 The fipronil-containing insecticidal soluble granule according to claim 1, wherein the binder is selected from the group consisting of β-cyclodextrin, polyvinyl alcohol, methyl cellulose, glucose, and urea. One or two.

 The fipronil-containing insecticidal soluble granule according to claim 1, wherein the stabilizer is selected from the group consisting of sodium benzoate and glucose.

 The fipronil-containing insecticidal soluble granule according to claim 1, wherein the filler is selected from one or two of sodium hydrogencarbonate, anhydrous citric acid, maltose and anhydrous sodium sulfate. Kind.

 14. A method of preparing a fipronil-containing insecticidal soluble granule according to any of claims 1-13, comprising the steps of:

1 homogenization: the fipronil original drug is mixed with a binder and a wetting agent in water at 50 to 60 ° C, and stirred and homogenized under a high pressure of 420 to 450 kg/cm ² ;

 2 spraying the above-mentioned liquid mixture after homogenization to form a composite parent drug;

3 kneading: after the emulsifier is thermally dissolved, it is mixed with the dispersing agent, the stabilizer, the filler and the composite parent drug at a temperature of 45 to 50 ° C, and then stirred and kneaded under a pressure of 4 to 6 kg/cm ^{2 to} obtain Group agent

4 extrusion granulation: the group is extruded under the pressure of 6~12 kg / cm ² into columnar particles;

5 The columnar particles were vacuum dried at 70 ° C for 1 hour, and then sieved and shaped.