Dinotefuran water dispersible granule and preparation process thereof

Abstract

The invention discloses dinotefuran water dispersible granules and a preparation process thereof, and relates to the technical field of medicament production, and the dinotefuran water dispersible granules comprise dinotefuran raw medicine, a dispersing agent, a wetting agent, an auxiliary agent, a cosolvent, a synergist, a binder, a water-based carrier and a filler in a weight ratio of (10-50): (10-20): (1-3): (2-5): (5-10): (1-3): (2-5): (10-30): (1-3). The preparation method of the binder comprises the following steps: reacting hydroxyethyl cellulose with lauryl sodium sulfate at 60-80 DEG C for 2-4 hours to obtain a grafted product; and carrying out a cross-linking reaction on the grafted product and a calcium citrate complex at 60-90 DEG C for 1-3 h, cooling the reaction product to room temperature, and successively carrying out filtration and centrifugation treatment to obtain the binder. The stability and dispersity of the medicament are greatly improved, and the efficacy of the medicament is improved.

Description

Technical Field

[0001] The invention relates to the technical field of pharmaceutical production, and in particular to a dinotefuran water dispersible granule and a preparation process thereof. Background Art

[0002] As a third-generation nicotinoid insecticide, dinotefuran has contact, stomach poison and systemic activity. It has excellent control effects on various pests including aphids, planthoppers, whiteflies, etc., and is widely needed in agricultural production. However, the traditional dinotefuran formulations have problems such as poor dispersibility, low suspension rate and easy deliquesce, which limit its full efficacy and convenience in field application. As an environmentally friendly pesticide formulation, water-dispersible granules have the advantages of wettable powders and suspensions, and have the characteristics of no dust pollution, good fluidity, easy metering and convenient use. They have gradually become one of the important directions for the development of pesticide formulations. However, due to certain physical and chemical properties of dinotefuran technical, such as limited solubility in water and low melting point, the preparation of dinotefuran water-dispersible granules with high stability, high dispersibility and high efficacy is challenging. Therefore, it is of great practical significance to develop a dinotefuran water-dispersible granule with excellent performance and its preparation process. Summary of the invention

[0003] The first technical problem to be solved by the present invention is: in view of the deficiencies in the prior art, a dinotefuran water dispersible granule is provided, which has high dispersibility and stability and good efficacy.

[0004] To solve the first problem of the above technology, the technical solution of the present invention is: A dinotefuran water dispersible granule, comprising dinotefuran technical, a dispersant, a wetting agent, an adjuvant, a cosolvent, a synergist, a binder, an aqueous carrier and a filler in a weight ratio of (10-50): (10-20): (1-3): (2-5): (5-10): (1-3): (2-5): (10-30): (1-3); The preparation method of the binder is: Heat the ethanol in the reactor to 40-50°C, slowly sprinkle the hydroxyethyl cellulose powder into it, and stir at 100-150rpm for 30-60min until it is completely dissolved to form a uniform and transparent solution, then slowly add the sodium dodecyl sulfate solid and continue stirring for 15-30min; Slowly add a 5-15%wt ammonium persulfate solution into the reactor, and the adding time is controlled within 30-60min. After the adding is completed, the temperature of the reactor is raised to 60-80°C, and the reaction is continued at 100-150rpm for 2-4h to obtain a grafted product. Continue to add calcium citrate complex to the grafted product, continue to react at 60-90°C for 1-3h, wait for the cross-linking reaction to be completed, cool to 30-50°C, add hyaluronic acid, adjust the stirring speed to 200-300rpm, stir for 30-90min, after the reaction is completed, cool the reaction product to room temperature, filter and centrifuge to obtain a binder.

[0005] Preferably, the mass ratio of the hydroxyethyl cellulose to ethanol is 1-10:30, the amount of the sodium lauryl sulfate added is 5%-30% of the mass of the hydroxyethyl cellulose, the amount of the ammonium persulfate added is 0.5%-5% of the mass of the hydroxyethyl cellulose, the amount of the calcium citrate complex added is 1%-5% of the mass of the hydroxyethyl cellulose, and the amount of the hyaluronic acid added is 3%-15% of the mass of the hydroxyethyl cellulose.

[0006] The preparation method of the calcium citrate complex is as follows: dissolving citric acid and calcium salt in deionized water at a molar ratio of 2:1-1.15, and heating at 50-60°C for 1-2h to fully complex citric acid with calcium ions to form a calcium citrate complex crosslinker.

[0007] Preferably, the preparation method of the aqueous carrier is: Place a styrene-acrylic acid emulsion with a solid content of 30%-60% w / w in a reaction kettle, add propylene glycol at 40-50°C and 300-800rpm, stir for 10-30min, continue to heat to 60-90°C, and add glycidyl methacrylate dropwise under a nitrogen atmosphere, maintain the drop rate at 0.5-2mL / min, and control the drop time at 30-90min. After the drop addition is completed, continue the reaction for 2-6h; Continue to add aziridine and react at 70-95° C. for 1-3 hours. After the reaction is completed, cool the reactor to room temperature. The obtained product is filtered and dialyzed using a dialysis bag for 24-72 hours to obtain an aqueous carrier.

[0008] Preferably, the amount of propylene glycol added is 5%-20% of the mass of the styrene-acrylic emulsion, the amount of glycidyl methacrylate added is 3%-15% of the mass of the styrene-acrylic emulsion, and the amount of aziridine added is 1%-5% of the mass of the styrene-acrylic emulsion.

[0009] Preferably, the dispersant is obtained by mixing lignin sulfonate, naphthalene sulfonate polycondensate and fatty alcohol polyoxyethylene ether in a mass ratio of 1:1-2:1-1.5.

[0010] Preferably, the preparation method of the dispersant is: lignin sulfonate and fatty alcohol polyoxyethylene ether are put into a spiral air flow mill and crushed to obtain a mixture with a particle size of 20 to 40 μm; The mixed material and the naphthalenesulfonate polycondensate are put into a spiral air flow mill and stirred at 150-220 rpm to obtain a dispersant.

[0011] Preferably, the feeding pressure of the spiral airflow mill is 0.50-0.55 MPa, and the grinding pressure is 0.45-0.50 MPa; The stirring time of the mixed material and the naphthalenesulfonate polycondensate is 20 to 30 minutes.

[0012] Preferably, the wetting agent is one of fatty alcohol polyoxyethylene ether or alkylphenol polyoxyethylene ether; The auxiliary agent includes a preservative and an antioxidant, and the mass ratio of the preservative to the antioxidant is 1:1-2; The cosolvent is one of nicotinamide and acetamide; The synergist is one of N-octyl bicycloheptene dicarboximide or piperonyl butoxide; The filler is a mixture of white carbon black and mica powder, wherein the mass ratio of white carbon black to mica powder is 1:1-1.15.

[0013] The second technical problem to be solved by the present invention is: in view of the shortcomings of the prior art, a preparation process of dinotefuran water dispersible granules is provided, and the obtained dinotefuran water dispersible granules have high dispersibility and stability and good efficacy.

[0014] To solve the second problem of the above technology, the technical solution of the present invention is: A preparation process of dinotefuran water dispersible granules comprises the following steps: A. Add dinotefuran technical, dispersant, wetting agent, adjuvant, cosolvent, synergist, binder and filler into a mixer in proportion and mix them evenly to obtain a premix, wherein the mixing motor frequency of the three-dimensional mixer in step A is 30-45 Hz and the mixing time is 10-30 min; B. Add the premix into a jet mill for pulverization to make the particle size reach 30-50 μm; C. Transfer the crushed material to a kneader, add purified water and knead for 15-30 min at a kneading temperature of 30-40°C and a rotation speed of 80-120 rpm; D. The kneaded material is granulated by an extrusion granulator to form granules, wherein the die temperature of the extrusion granulator is 80-100° C., the extrusion pressure is 2-10 MPa, the screw speed is 20-80 rpm, and the cutter speed is 180-200 rpm; E. Dry the particles in a fluidized bed dryer for 1-3 hours to reduce the moisture content to less than 3%, wherein the inlet air temperature of the fluidized bed dryer is 100-150°C, the outlet air temperature is 70-140°C, the fluidizing wind speed is 0.5-5m / s, and the drying time is 10-60min; F. The dried particles are sieved to remove unqualified large particles and fine powder to obtain the finished product dinotefuran water-dispersible granules with a particle size of 40-50 μm.

[0015] Due to the adoption of the above technical solution, the beneficial effects of the present invention are: 1. The grafted sodium dodecyl sulfate in the binder can significantly reduce the surface tension of water, making it easier for water to spread on the surface of the dinotefuran water-dispersible granules. The water molecules are in more complete contact with the drug powder, which accelerates the initial stage of dissolution and enables the drug to be dispersed and dissolved in the water more quickly and evenly, thus reducing the amount of co-solvent used, avoiding the reduction of the effective ingredients and stability of dinotefuran due to excessive use of co-solvent, and reducing production costs.

[0016] 2. Ammonium persulfate decomposes to produce free radicals, which capture the hydrogen atoms adjacent to the hydroxyl groups on the hydroxyethyl cellulose molecular chain to form macromolecular free radicals, which then react with the sodium dodecyl sulfate molecules to achieve grafting. Hydroxyethyl cellulose itself contains abundant hydroxyl groups. Even after grafting with sodium dodecyl sulfate, there are still a large number of hydroxyl groups that do not participate in the grafting reaction. These hydroxyl groups provide active sites for the subsequent cross-linking reaction and can react with calcium citrate to form a three-dimensional network structure. The grafted sodium dodecyl sulfate contains sulfate ions, and its ability to directly participate in cross-linking is limited. However, its presence can change the spatial distribution and charge characteristics of the molecular chain of the entire grafted product, and synergize with the ionic calcium citrate complex cross-linker, making it easier for ionic interactions to occur during the cross-linking process, promoting the formation of a cross-linking network, indirectly assisting the cross-linking reaction, and enhancing the adhesion of the dinotefuran water-dispersible granules. Dinotefuran can better adhere to the surface of crops, slowly release its efficacy, extend the effective period of the agent, and reduce the number of applications. In addition, dinotefuran can better adhere to the surface of pests, increase the chances of pests contacting and ingesting the agent, and improve the contact and stomach poison effects on pests. Dinotefuran adheres more firmly to the surface of crops, reducing the loss of pesticides caused by factors such as rain erosion, reducing the risk of pollution to soil, water bodies and other environments, helping the agent to stay accurately on target crops and pest activity areas, and improving the utilization rate of pesticides.

[0017] 3. Sodium dodecyl sulfate has a good effect of reducing surface tension. After being grafted onto hydroxyethyl cellulose, it can improve the wettability of hydroxyethyl cellulose, making it easier to spread and infiltrate the surface of the adherend, thereby improving the adhesion effect and reducing the amount of wetting agent used, thereby avoiding the reduction of stability and efficacy of dinotefuran water-dispersible granules due to the amount of wetting agent used, causing pollution to the environment.

[0018] 4. The aqueous carrier of the present invention increases the active adsorption sites of the carrier by introducing the functional monomer glycidyl methacrylate for copolymerization, promotes the formation of a cross-linked network structure between molecular chains, enhances the mechanical strength and stability of the carrier, and greatly increases the loading amount of other components in the dinotefuran water dispersible granules compared with traditional aqueous carriers.

[0019] 5. Lignin sulfonate has good water solubility and steric hindrance effect, which can prevent the agglomeration of particles; naphthalene sulfonate polycondensate has strong electrostatic repulsion, which can charge the surface of particles and increase the repulsive force between particles; fatty alcohol polyoxyethylene ether has good wettability and emulsification properties, which can reduce the surface tension of liquid and make particles more easily dispersed in liquid. The synergistic effect of the three can significantly enhance the dispersion effect, improve the suspension rate and stability of the agent in water, ensure the uniform dispersion of the agent, and avoid precipitation and agglomeration. It enables dinotefuran to cover the surface of plants or pests, pathogens and other control objects more evenly, increases the contact opportunities between the agent and the control object, and thus improves the efficacy. At the same time, the mixed dispersant can also improve the permeability of the agent, making it easier for the agent to enter the interior of the control object and play a better control role.

[0020] 6. Silica relies on its huge specific surface area and strong adsorption to provide particles with charge or steric repulsion to prevent agglomeration; the flaky structure of mica powder is like tiny "layers" that further expand the distance between particles. The combination of the two allows the dinotefuran particles to disperse more evenly and quickly in the water, and can quickly form a uniform and stable suspension. Both silica and mica powder have a certain adsorption capacity and can carry more dinotefuran. When the particles enter the water, the two rely on different release mechanisms to allow the agent to be released steadily and continuously, extending the effective time of the agent in the action area, ensuring that pests have more opportunities to come into contact with lethal doses of the drug, and improving the prevention and control effect. DETAILED DESCRIPTION

[0021] The present invention will be further described below in conjunction with the embodiments.

[0022] Example 1 A preparation process of dinotefuran water dispersible granules comprises the following steps: A. Add dinotefuran technical, dispersant, wetting agent, adjuvant, cosolvent, synergist, binder and filler into a mixer in proportion and mix them evenly to obtain a premix, wherein the mixing motor frequency of the three-dimensional mixer in step A is 30-45 Hz and the mixing time is 10-30 min; B. Add the premix into a jet mill for pulverization to make the particle size reach 30-50 μm; C. Transfer the crushed material to a kneader, add purified water and knead for 15-30 min at a kneading temperature of 30-40°C and a rotation speed of 80-120 rpm; D. The kneaded material is granulated by an extrusion granulator to form granules, wherein the die temperature of the extrusion granulator is 80-100° C., the extrusion pressure is 2-10 MPa, the screw speed is 20-80 rpm, and the cutter speed is 180-200 rpm; E. Dry the particles in a fluidized bed dryer for 1-3 hours to reduce the moisture content to less than 3%, wherein the inlet air temperature of the fluidized bed dryer is 100-150°C, the outlet air temperature is 70-140°C, the fluidizing wind speed is 0.5-5m / s, and the drying time is 10-60min; F. The dried particles are sieved to remove unqualified large particles and fine powder to obtain the finished product dinotefuran water-dispersible granules with a particle size of 40-50 μm.

[0023] Example 2 A dinotefuran water dispersible granule is prepared according to the process in Example 1, wherein: Dinotefuran technical: 10g Dispersant: 10g, prepared by mixing lignin sulfonate, naphthalene sulfonate polycondensate and fatty alcohol polyoxyethylene ether in a mass ratio of 1:1:1. First, lignin sulfonate and fatty alcohol polyoxyethylene ether were put into a spiral air flow mill, and ground at a feeding pressure of 0.50MPa and a grinding pressure of 0.45MPa to obtain a mixture with a particle size of 20μm; then the mixture and naphthalene sulfonate polycondensate were put into the mill, and stirred at 150rpm for 20min to obtain a dispersant.

[0024] Wetting agent: 1g, fatty alcohol polyoxyethylene ether.

[0025] Additives: 2g, including 1g preservative and 1g antioxidant.

[0026] Co-solvent: 5g, niacinamide is selected.

[0027] Synergist: 1g, N-octylbicycloheptene dicarboximide is selected.

[0028] Binder: 2g, preparation method is as follows: Add 30g of ethanol into the reactor, heat to 40°C, slowly sprinkle 1g of hydroxyethyl cellulose powder into it, and stir at 100rpm for 30min until it is completely dissolved. Then slowly add 0.05g of sodium dodecyl sulfate solid, and continue stirring for 15min.

[0029] 0.005 g of 5% wt ammonium persulfate solution was slowly added dropwise into the reactor for 30 min. After the addition was completed, the temperature was raised to 60°C and the reaction was continued at 100 rpm for 2 h to obtain the grafted product.

[0030] 0.01 g of calcium citrate complex was added to the grafted product, and the reaction was continued at 60° C. for 1 h. After the cross-linking was completed, the temperature was lowered to 30° C., 0.03 g of hyaluronic acid was added, and the mixture was stirred at 200 rpm for 30 min. The mixture was cooled to room temperature, filtered, and centrifuged to obtain a binder.

[0031] The preparation method of the calcium citrate complex is as follows: dissolving citric acid and calcium chloride in deionized water at a molar ratio of 2:1, and heating at 50° C. for 1 hour to allow citric acid to fully complex with calcium ions to form a calcium citrate complex crosslinker.

[0032] Aqueous carrier: 10 g, preparation method: place styrene-acrylic acid emulsion with a solid content of 30% w / w in a reactor, add propylene glycol accounting for 5% of the mass of the emulsion at 40°C and 300 rpm, stir for 10 minutes, heat to 60°C, and under nitrogen protection, add 3% of the mass of the emulsion glycidyl methacrylate dropwise at a rate of 0.5 mL / min, add for 30 minutes, and react for another 2 hours; then add 1% of the mass of the emulsion aziridine, react at 70°C for 1 hour, cool to room temperature, filter and dialyze for 24 hours to obtain an aqueous carrier.

[0033] Filler: 10g, a mixture of white carbon black and mica powder in a mass ratio of 1:1.

[0034] Example 3 A dinotefuran water dispersible granule is prepared according to the process in Example 1, wherein: Dinotefuran technical: 30g Dispersant: 15g, made by mixing lignin sulfonate, naphthalene sulfonate polycondensate and fatty alcohol polyoxyethylene ether in a mass ratio of 1:1.5:1.25. Crushing and stirring conditions are: feeding pressure 0.52MPa, grinding pressure 0.47MPa, mixed material particle size 30μm, stirring at 180rpm for 25min.

[0035] Wetting agent: 1.5g, alkylphenol polyoxyethylene ether.

[0036] Additives: 3.5g, including 1.5g preservative and 2g antioxidant.

[0037] Cosolvent: 7.5g, acetamide is selected.

[0038] Synergist: 2g, piperonyl butoxide is used.

[0039] Binder: 3.5g, preparation method: Add 45 g of ethanol to the reactor, heat to 45°C, sprinkle in 5 g of hydroxyethyl cellulose powder, stir at 125 rpm for 45 min to dissolve, add 1.5 g of sodium dodecyl sulfate, and stir for another 22 min.

[0040] 0.25 g of 10% wt ammonium persulfate solution was added dropwise for 45 min, the temperature was raised to 70°C, and the reaction was carried out at 125 rpm for 3 h to obtain the grafted product.

[0041] Add 0.25 g of calcium citrate complex, react at 75° C. for 2 h, cool to 40° C., add 0.75 g of hyaluronic acid, stir at 250 rpm for 60 min, and cool to obtain a binder.

[0042] The preparation method of the calcium citrate complex is as follows: dissolving citric acid and calcium chloride in deionized water at a molar ratio of 2:1.05, and heating at 55° C. for 1.5 hours to allow citric acid to fully complex with calcium ions to form a calcium citrate complex crosslinker.

[0043] Aqueous carrier: 20 g, preparation: solid content 45% w / w styrene-acrylic emulsion, add 12.5% ​​by mass of propylene glycol at 45°C and 550 rpm, stir for 20 min, heat to 75°C, nitrogen atmosphere, add 8% by mass of glycidyl methacrylate at 1 mL / min, add for 60 min, and react for 4 h; add 3% by mass of aziridine, react at 85°C for 2 h, cool, filter, and dialyze for 48 h.

[0044] Filler: 20g, mass ratio of white carbon black and mica powder is 1:1.05.

[0045] Example 4 A dinotefuran water dispersible granule is prepared according to the process in Example 1, wherein: Dinotefuran technical: 40g Dispersant: 18g, lignin sulfonate, naphthalene sulfonate polycondensate and fatty alcohol polyoxyethylene ether mass ratio 1:2:1.5. Spiral airflow mill feeding pressure 0.54MPa, grinding pressure 0.49MPa, mixed material particle size 35μm, 200rpm stirring for 28min.

[0046] Wetting agent: 2g, fatty alcohol polyoxyethylene ether.

[0047] Additives: 4g, preservative 1.5g, antioxidant 2.5g.

[0048] Cosolvent: 8g, niacinamide.

[0049] Synergist: 2.5g, N-octylbicycloheptene dicarboximide.

[0050] Binder: 4g, Preparation: Heat 60g of ethanol to 48°C, add 8g of hydroxyethyl cellulose, stir at 140rpm for 50min to dissolve, add 2.4g of sodium dodecyl sulfate, and continue stirring for 25min.

[0051] 0.4 g of 12% wt ammonium persulfate solution was added dropwise over 50 min, the temperature was raised to 75°C, and the reaction was carried out at 140 rpm for 3.5 h to obtain the grafted product.

[0052] Add 0.4 g of calcium citrate complex, react at 80° C. for 2.5 h, cool to 45° C., add 1.2 g of hyaluronic acid, stir at 280 rpm for 70 min, and obtain a binder.

[0053] The preparation method of the calcium citrate complex is as follows: dissolving citric acid and calcium chloride in deionized water at a molar ratio of 2:1.15, and heating at 60° C. for 2 hours to allow citric acid to fully complex with calcium ions to form a calcium citrate complex crosslinker.

[0054] Aqueous carrier: 25g, preparation: 50% w / w styrene-acrylic acid emulsion, 48℃, 700rpm, add 15% mass propylene glycol and stir for 25min, heat to 80℃, add 12% mass glycidyl methacrylate at 1.5mL / min under nitrogen, add for 75min, and react for 5h; add 4% mass aziridine, react at 90℃ for 2.5h, cool and dialyze for 60h.

[0055] Filler: 25g, white carbon black and mica powder 1:1.1.

[0056] Example 5 A dinotefuran water dispersible granule is prepared according to the process in Example 1, wherein: Dinotefuran technical: 50g Dispersant: 20g, mixed with lignin sulfonate, naphthalene sulfonate polycondensate and fatty alcohol polyoxyethylene ether in a mass ratio of 1:2:1.5, crushing and stirring parameters are feeding pressure 0.55MPa, grinding pressure 0.50MPa, mixed material particle size 40μm, stirring at 220rpm for 30min.

[0057] Wetting agent: 3g, alkylphenol polyoxyethylene ether.

[0058] Additives: 5g, preservatives 2g, antioxidants 3g.

[0059] Cosolvent: 10g, acetamide.

[0060] Synergist: 3g, piperonyl butoxide.

[0061] Binder: 5g, Preparation: Heat 90g of ethanol to 50℃, sprinkle in 10g of hydroxyethyl cellulose, stir at 150rpm for 60min to dissolve, add 3g of sodium dodecyl sulfate, and stir for another 30min.

[0062] 0.5 g of 15% wt ammonium persulfate solution was added dropwise over 60 min, and the temperature was raised to 80° C. and reacted at 150 rpm for 4 h to obtain the grafted product.

[0063] 0.5 g of calcium citrate complex was added, reacted at 90° C. for 3 h, cooled to 50° C., 1.5 g of hyaluronic acid was added, stirred at 300 rpm for 90 min, and a binder was obtained after treatment.

[0064] The preparation method of the calcium citrate complex is as follows: dissolving citric acid and calcium chloride in deionized water at a molar ratio of 2:1.1, and heating at 55° C. for 2 hours to allow citric acid to fully complex with calcium ions to form a calcium citrate complex crosslinker.

[0065] Aqueous carrier: 30 g, preparation: 60% w / w styrene-acrylic emulsion, add 20% mass propylene glycol at 50°C and 800 rpm and stir for 30 min, heat to 90°C, nitrogen atmosphere, add 15% mass glycidyl methacrylate at 2 mL / min, add for 90 min, and react for 6 h; add 5% mass aziridine, react at 95°C for 3 h, cool, filter, and dialyze for 72 h.

[0066] Filler: 30g, mass ratio of white carbon black and mica powder is 1:1.15.

[0067] Comparative Example 1 The binder was replaced with hydroxyethyl cellulose, and the remaining components and preparation method were exactly the same as those in Example 5.

[0068] Comparative Example 2 The aqueous carrier was replaced with styrene-acrylic emulsion, and the remaining components and preparation method were exactly the same as those in Example 5.

[0069] Comparative Example 3 Only lignin sulfonate is used in the dispersant, and the remaining components and preparation method are exactly the same as those in Example 5.

[0070] Comparative Example 4 Only naphthalenesulfonate polycondensate is used in the dispersant, and the remaining components and preparation method are exactly the same as those in Example 5.

[0071] Comparative Example 5 Only fatty alcohol polyoxyethylene ether is used in the dispersant, and the remaining components and preparation method are exactly the same as those in Example 5.

[0072] Comparative Example 6 Only white carbon black is used as the filler, and the other components and preparation method are exactly the same as those in Example 5.

[0073] Comparative Example 7 Only mica powder is used as filler, and the other components and preparation method are exactly the same as those in Example 5.

[0074] The performance of the dinotefuran water dispersible granules obtained in Examples 2-5 and Comparative Examples 1-7 was tested, and the results are shown in the following table: Table 1

[0075] It should be understood that these embodiments are only used to illustrate the present invention and are not used to limit the scope of the present invention. In addition, it should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms also fall within the scope limited by the appended claims of the application.

Claims

1. A dinotefuran water dispersible granule, characterized in that: The invention comprises a dinotefuran technical, a dispersant, a wetting agent, an adjuvant, a cosolvent, a synergist, a binder, an aqueous carrier and a filler in a weight ratio of (10-50): (10-20): (1-3): (2-5): (5-10): (1-3): (2-5): (10-30): (1-3); The preparation method of the binder is: Heat the ethanol in the reactor to 40-50°C, slowly sprinkle the hydroxyethyl cellulose powder into it, and stir at 100-150rpm for 30-60min until it is completely dissolved to form a uniform and transparent solution, then slowly add the sodium dodecyl sulfate solid and continue stirring for 15-30min; Slowly add a 5-15%wt ammonium persulfate solution into the reactor, and the adding time is controlled within 30-60min. After the adding is completed, the temperature of the reactor is raised to 60-80°C, and the reaction is continued at 100-150rpm for 2-4h to obtain a grafted product. Continue to add calcium citrate complex to the grafted product, continue to react at 60-90°C for 1-3h, wait for the cross-linking reaction to be completed, cool to 30-50°C, add hyaluronic acid, adjust the stirring speed to 200-300rpm, stir for 30-90min, after the reaction is completed, cool the reaction product to room temperature, filter and centrifuge to obtain a binder.

2. The dinotefuran water dispersible granules according to claim 1, characterized in that: The mass ratio of the hydroxyethyl cellulose to the ethanol is 1-10:30, the added amount of the sodium lauryl sulfate accounts for 5%-30% of the mass of the hydroxyethyl cellulose, the added amount of the ammonium persulfate accounts for 0.5%-5% of the mass of the hydroxyethyl cellulose, the added amount of the calcium citrate complex accounts for 1%-5% of the mass of the hydroxyethyl cellulose, and the added amount of the hyaluronic acid accounts for 3%-15% of the mass of the hydroxyethyl cellulose.

3. The dinotefuran water dispersible granules according to claim 1, characterized in that: The preparation method of the aqueous carrier is: Place a styrene-acrylic acid emulsion with a solid content of 30%-60% w / w in a reaction kettle, add propylene glycol at 40-50°C and 300-800rpm, stir for 10-30min, continue to heat to 60-90°C, and add glycidyl methacrylate dropwise under a nitrogen atmosphere, maintain the drop rate at 0.5-2mL / min, and control the drop time at 30-90min. After the drop addition is completed, continue the reaction for 2-6h; Continue to add aziridine and react at 70-95° C. for 1-3 hours. After the reaction is completed, cool the reactor to room temperature. The obtained product is filtered and dialyzed using a dialysis bag for 24-72 hours to obtain an aqueous carrier.

4. The dinotefuran water dispersible granules according to claim 3, characterized in that: The amount of propylene glycol added is 5%-20% of the mass of the styrene-acrylic emulsion, the amount of glycidyl methacrylate added is 3%-15% of the mass of the styrene-acrylic emulsion, and the amount of aziridine added is 1%-5% of the mass of the styrene-acrylic emulsion.

5. The dinotefuran water dispersible granules according to claim 1, characterized in that: The dispersant is obtained by mixing lignin sulfonate, naphthalene sulfonate polycondensate and fatty alcohol polyoxyethylene ether in a mass ratio of 1:1-2:1-1.

5.

6. The dinotefuran water dispersible granules according to claim 5, characterized in that: The preparation method of the dispersant is as follows: lignin sulfonate and fatty alcohol polyoxyethylene ether are put into a spiral air flow mill and crushed to obtain a mixture with a particle size of 20 to 40 μm; The mixed material and the naphthalenesulfonate polycondensate are put into a spiral air flow mill and stirred at 150-220 rpm to obtain a dispersant.

7. The dinotefuran water dispersible granules according to claim 6, characterized in that: The feeding pressure of the spiral air flow mill is 0.50-0.55MPa, and the grinding pressure is 0.45-0.50MPa; The stirring time of the mixed material and the naphthalenesulfonate polycondensate is 20 to 30 minutes.

8. The dinotefuran water dispersible granules according to claim 1, characterized in that: The wetting agent is one of fatty alcohol polyoxyethylene ether or alkylphenol polyoxyethylene ether; The auxiliary agent includes a preservative and an antioxidant, and the mass ratio of the preservative to the antioxidant is 1:1-2; The co-solvent is one of nicotinamide and acetamide.

9. The dinotefuran water dispersible granules according to claim 1, characterized in that: The synergist is one of N-octyl bicycloheptene dicarboximide or piperonyl butoxide; The filler is a mixture of white carbon black and mica powder, wherein the mass ratio of white carbon black to mica powder is 1:1-1.

15.

10. The process for preparing the dinotefuran water dispersible granules according to any one of claims 1 to 9, characterized in that: The following steps are involved: A. Add dinotefuran technical, dispersant, wetting agent, adjuvant, cosolvent, synergist, binder and filler into a mixer in proportion and mix them evenly to obtain a premix, wherein the mixing motor frequency of the three-dimensional mixer in step A is 30-45 Hz and the mixing time is 10-30 min; B. Add the premix into a jet mill for pulverization to make the particle size reach 30-50 μm; C. Transfer the crushed material to a kneader, add purified water and knead for 15-30 min at a kneading temperature of 30-40°C and a rotation speed of 80-120 rpm; D. The kneaded material is granulated by an extrusion granulator to form granules, wherein the die temperature of the extrusion granulator is 80-100° C., the extrusion pressure is 2-10 MPa, the screw speed is 20-80 rpm, and the cutter speed is 180-200 rpm; E. Dry the particles in a fluidized bed dryer for 1-3 hours to reduce the moisture content to less than 3%, wherein the inlet air temperature of the fluidized bed dryer is 100-150°C, the outlet air temperature is 70-140°C, the fluidizing wind speed is 0.5-5m / s, and the drying time is 10-60min; F. The dried particles are sieved to remove unqualified large particles and fine powder to obtain the finished product dinotefuran water-dispersible granules with a particle size of 40-50 μm.

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