Pesticide preparation containing chlorantraniliprole and clothianidin, preparation method and application

Abstract

The invention relates to the field of pesticide preparation, and particularly discloses a pesticide preparation containing chlorantraniliprole and clothianidin and a preparation method and application thereof.The pesticide preparation containing chlorantraniliprole and clothianidin comprises a spherical carrier, an effective component mother solution and an isolation layer; the effective component mother liquor comprises chlorantraniliprole, clothianidin, an auxiliary agent and the balance of water; the preparation method comprises the following steps: preparing the spherical carrier; preparing an isolating layer solution; the preparation method comprises the following steps: uniformly mixing chlorantraniliprole, clothianidin, an auxiliary agent and water to obtain an effective component mother solution; rolling and stirring the spherical carrier in a granulator, then adding the active ingredient mother liquor, and uniformly mixing to obtain a cladding carrier; uniformly mixing the isolation layer solution and the color paste to obtain a compound solution; spraying the composite liquid on the surface of the cladding carrier, drying to obtain a layer of preparation, uniformly spraying the active ingredient mother liquor on the surface, drying, spraying the composite liquid again, drying, repeating the operation, and curing to obtain a finished product. The composition has the advantages of low toxicity, no drift diffusion risk, good control effect and high environmental compatibility.

Description

Technical Field

[0001] The present application relates to the field of pesticide preparation, and more specifically, to a pesticide preparation containing chlorantraniliprole and clothianidin, a preparation method and application thereof. Background Art

[0002] Pesticides play an important role in agricultural production. However, traditional pesticide formulations and their application methods pose potential risks to human and animal health and the environment.

[0003] In the prior art, a Chinese patent document with publication number CN1015541690A discloses an insecticide composition containing chlorantraniliprole for use on crops, which discloses a composition of chlorantraniliprole with thiamethoxam or nitenpyram, and discloses a formulation and preparation method of a water-dispersible granule or a suspension. During the spraying process of liquid pesticides, they are easily inhaled by the human body with the wind, and the wind easily reduces the amount of liquid pesticide attached to the surface of the plant, so granular pesticides are gradually being valued by people.

[0004] In the prior art, a Chinese patent document with publication number CN106417280A, a high-content pesticide coated granule and its preparation method, discloses a preparation process of a coating granule, wherein the mother liquor of the active ingredient is the highly toxic pesticide product carbofuran that has been legally banned by the state, and the front stage of the coating process requires the use of air flow milling to prepare the mother powder. This process not only causes great dust pollution, but also the use of air flow milling to prepare the mother powder of such a highly toxic variety as carbofuran has a very high risk of poisoning for workers in the production process. Therefore, low-toxic pesticides and concealed application methods are the current mainstream direction of pesticide development.

[0005] Existing pesticide granules are generally produced by the dipping method or the paraffin coating method. The dipping method requires the use of a large amount of organic solvents, which poses a risk of environmental pollution, while the paraffin coating has the problem of being difficult to degrade naturally. In addition, the particle size of existing pesticide granules is mostly between 200-2000μm, making it difficult to produce granule products with an active ingredient mother liquor content higher than 15%, and it is difficult to meet the control needs of special plants or special pests.

[0006] Therefore, how to prepare a new pesticide formulation that has the advantages of low toxicity, no risk of drift and diffusion, good pest control effect, and high environmental compatibility is a problem to be solved. Summary of the invention

[0007] In order to prepare a new pesticide preparation which has the advantages of low toxicity, no risk of drift and diffusion, good pest control effect and high environmental compatibility, the present application provides a pesticide preparation containing chlorantraniliprole and clothianidin, a preparation method and application.

[0008] In a first aspect, the present application provides a pesticide preparation containing chlorantraniliprole and clothianidin, using the following technical solution: A pesticide preparation containing chlorantraniliprole and clothianidin, the pesticide preparation comprising a spherical carrier and an active ingredient mother solution and an isolation layer coated layer by layer on the surface of the spherical carrier; The active ingredient mother solution contains the following raw materials in percentage by weight: 35-40% chlorantraniliprole, 12-14% clothianidin, 4.8-5.4% adjuvant, and water is added to 100%; The isolation layer is prepared from an isolation layer solution.

[0009] By adopting the above technical scheme, a spherical carrier is used to load the mother solution of the active ingredient, and then the surface is coated with an isolation layer. The isolation layer uses its good isolation effect to ensure the activity of the mother solution of the active ingredient during the application process, and ensure the compatibility of the pesticide preparation with the environment; chlorantraniliprole and clothianidin have low toxicity effects, further ensuring the low toxicity of the pesticide preparation and not easily affecting the growth of plants; and chlorantraniliprole and clothianidin have good control effects on underground pests and boring pests of traditional Chinese medicines, famous trees and ancient trees, and high-pole and densely planted crops; the pesticide preparation can directly reach the diseased part by concealed application buried in the soil, and has the advantages of no drift and diffusion risk and long-term sustained release.

[0010] Preferably, the spherical carrier is one or more of a clay carrier, a slow-release urea carrier, and an inactivated wheat aged grain carrier.

[0011] By adopting the above technical scheme, the clay carrier, the slow-release urea carrier, and the inactivated wheat aged grain carrier all have high porosity and surface roughness, which are convenient for loading the effective ingredient mother liquor. The effective ingredient mother liquor is loaded in the pores and on the rough surface, which ensures the slow-release and long-acting release of the effective ingredient mother liquor, and blocks part of the odor of the effective ingredient mother liquor, so as to avoid pests from avoiding pesticide preparations due to the smell of pesticides, and ensure that pests contact pesticide preparations. Chlorantraniliprole and clothianidin are systemic ingredients and have stomach poison effects. They have stomach-killing effects on large underground pests, such as mole crickets, grubs, wireworms, cutworms, etc. When pests ingest chlorantraniliprole and clothianidin, they can be effectively killed to achieve a control effect.

[0012] Preferably, the clay carrier is prepared by treating clay particles with atomized water and then bonding them to pomace fibers, wherein the mass ratio of clay particles, atomized water, and pomace fibers is 1:0.3-0.6:0.1-0.3; then clay particles, atomized water, and pomace fibers are added again, and the operation is repeated until the particle size reaches 3-6 mesh, and then the mixture is dried.

[0013] By adopting the above technical scheme, after the clay particles are treated with atomized water, the surface has a certain viscosity, which is convenient for adhering to the pomace fiber. Then, clay, atomized water and pomace fiber are added again to form multiple layers of clay particles and pomace fiber. When the required mesh size is reached, the processing is stopped. Both the clay particles and the pomace fiber have high porosity and can adsorb chlorantraniliprole and clothianidin, increase the adsorption amount, and prolong the sustained release time. In addition, the fruity aroma of the pomace fiber can be used to cover up the smell of chlorantraniliprole and clothianidin as much as possible, attracting soil pests to contact with pesticide preparations. The pomace fiber is rich in dietary fiber, vitamins and minerals. When the pests ingest the pomace fiber, they also ingest chlorantraniliprole and clothianidin, which makes it easier to kill and control the pests.

[0014] Preferably, the auxiliary agent in the active ingredient mother solution comprises sodium carboxymethyl cellulose solution and tributyl phosphate in a mass ratio of 1.3-1.6:1.

[0015] By adopting the above technical scheme, sodium carboxymethyl cellulose solution and tributyl phosphate are combined, and the good bonding effect of sodium carboxymethyl cellulose solution is utilized to facilitate the adhesion of chlorantraniliprole and clothianidin to the surface of the spherical carrier, and tributyl phosphate facilitates the uniform dispersion of chlorantraniliprole and clothianidin, thereby facilitating the uniform loading of chlorantraniliprole and clothianidin on the spherical carrier, thereby achieving the advantages of efficient pest control and low toxicity of the pesticide formulation.

[0016] Preferably, the isolation layer solution comprises the following raw materials in parts by weight: 1-5 parts of acrylic resin, 10-15 parts of polyvinyl alcohol, 1-2 parts of polyacrylate, 1-2 parts of cellulose derivative, 10-20 parts of sucrose, 1-5 parts of gum arabic, and 200-300 parts of water.

[0017] By adopting the above technical scheme, the carboxyl groups in the acrylic resin, the hydroxyl groups in the polyvinyl alcohol, the hydroxyl groups in the cellulose derivatives, the hydroxyl groups in the sucrose and the hydroxyl groups in the gum arabic cooperate with each other, and under the action of their own bonding effect, the cross-linking effect and the bonding effect of the isolation layer solution are further improved, ensuring that the isolation layer solution stably adheres the mother solution of the active ingredient to the surface of the spherical carrier, thereby making the pesticide preparation have a sustained-release and low-toxic effect.

[0018] Acrylic resin, polyvinyl alcohol and polyacrylate can be cross-linked to produce a porous and breathable isolation layer, which ensures the breathability. At the same time, the sugar in sucrose and the high molecular polysaccharide of gum arabic can attract pests. The cellulose derivatives have a loading effect on pests, ensuring that the pests in the soil are bound near the pesticide preparation after contacting the pesticide preparation. The insecticidal effect of the mother solution of the active ingredient can further prevent and control pests in the soil.

[0019] Preferably, the isolation layer solution further comprises 1-3 parts of soybean fiber modified with n-propyl lactate; the soybean fiber modified with n-propyl lactate is prepared from soybean fiber and n-propyl lactate in a mass ratio of 1:0.1-0.25.

[0020] By adopting the above technical scheme, the soybean fiber modified by n-propyl lactate contains rich protein, which can not only attract pests in the soil, but also increase the nutrient content in the soil. The n-propyl lactate has a lipophilic effect and cooperates with the lipophilic effect of tributyl phosphate to ensure the close adhesion between the isolation layer solution and the active ingredient mother solution. The n-propyl lactate contains both hydrophilic groups and lipophilic groups, which is convenient for bonding with acrylic resin, polyvinyl alcohol, sucrose and other hydrophilic substances, and can be attracted and connected with the lipophilic groups of polyacrylates, thereby improving the cross-linking density of the isolation layer and ensuring the sustained-release effect of the pesticide preparation.

[0021] The fiber structure of soybean fiber is convenient for loading the mother liquor of effective ingredients and can easily attract pests to the surface of pesticide preparations. Soybean fiber is rich in fiber and protein, which is convenient for attracting and ingesting soybean fiber, further ensuring that pests will experience stomach poisoning and contact killing effects when they come into contact with pesticide preparations. Propyl lactate also has killing and inhibitory effects on pests, and combined with chlorantraniliprole and clothianidin, it can further improve the control effect of pesticide preparations on pests.

[0022] Preferably, the cellulose derivative consists of sodium carboxymethyl cellulose and cellulose acetate in a mass ratio of 1:0.1-0.35.

[0023] By adopting the above technical solution, sodium carboxymethyl cellulose and cellulose acetate are combined. Sodium carboxymethyl cellulose can absorb and fix moisture and nutrients in the soil, and has a neutralizing effect on acidic substances produced by pest metabolism. Combined with cellulose acetate, it helps to reduce the impact of pesticides on the environment and improve environmental compatibility while preventing and controlling pests.

[0024] In a second aspect, the present application provides a method for preparing a pesticide preparation containing chlorantraniliprole and clothianidin, using the following technical solution: A method for preparing a pesticide preparation containing chlorantraniliprole and clothianidin comprises the following steps: S1, preparing a spherical carrier; preparing an isolation layer solution; S2, mixing chlorantraniliprole, clothianidin, adjuvant and water to obtain a mother solution of active ingredients; S3, rolling and stirring 950-970 parts by weight of the spherical carrier in a granulator, and then adding 30-35 parts of the active ingredient mother solution, mixing evenly, to obtain a coating carrier; S4, mixing the isolation layer solution and the color paste at a mass ratio of 2.5-3.2:1 to obtain a composite solution; S5, spraying the composite liquid uniformly on the surface of the cladding carrier at a mass ratio of 1:24.5-25, and drying to obtain a layer of preparation; S6. Spray the active ingredient mother liquid evenly on the surface of a layer of the preparation. After drying, spray the composite liquid evenly again, dry, repeat the operations of S3 and S5, and obtain the finished product after solidification and dispersion. The finished product has a size of 2-6 mesh.

[0025] By adopting the above technical scheme, a layer-coated pesticide formulation is prepared. After being added to the soil surface, it not only has a slow-release effect, but also has the advantages of multi-layer coating, which can prolong the time of pest control and ensure environmental compatibility and low toxicity.

[0026] Preferably, the spherical carrier is an inactivated wheat aged grain carrier, and the inactivated wheat aged grain carrier is prepared by the following method: The aged wheat grain particles are placed in a hydrogen peroxide solution at a mass ratio of 1:2-5 for soaking and dispersion for 2-4 minutes, the aged wheat grains are filtered out, and dry steam inactivation treatment is performed at 130-140° C. for 25-35 minutes to obtain inactivated aged grains; The inactivated aged grain is cooled to 60-80°C, and is soaked and dispersed in a sucrose solution for 5-10 minutes, wherein the mass ratio of the inactivated aged grain to the sucrose solution is 1:2-5, and the aged wheat grain is filtered out and cooled to room temperature to obtain the loaded aged grain; Sodium alginate solution is evenly sprayed on the surface of the aged grain carrier, and finally pomace fiber is evenly added. The mass ratio of the aged grain carrier to the sodium alginate solution and the pomace fiber is 1:0.1-0.2:0.2-0.4. After drying, the aged grain carrier, sodium alginate solution and pomace fiber are repeatedly sprayed on the surface in sequence until the particle size is 2-3 meshes, thereby obtaining an inactivated wheat aged grain carrier.

[0027] By adopting the above technical scheme, the aged wheat grains are immersed and dispersed in a hydrogen peroxide solution, and the porous effect of the aged wheat grains is utilized to absorb the hydrogen peroxide solution. After being inactivated by high-temperature dry steam, the Aspergillus flavus in the aged wheat grains is killed while the thermal decomposition of the hydrogen peroxide solution is promoted, and the porosity and surface roughness of the aged wheat grains are increased, while the killing effect of Aspergillus flavus is further improved; then, the aged wheat grains are immersed and dispersed in a sucrose solution, and the good flow effect of the sucrose solution at a higher temperature is utilized to facilitate uniform penetration into the internal pores. As the temperature gradually decreases, the viscosity of the sucrose solution increases, and the sodium alginate solution is used to further adhere the pomace fiber to the surface of the aged wheat grain particles. The addition of the pomace fiber facilitates the loading of a higher content of chlorfenapyr and clothianidin, and the aroma of the sucrose solution is used to cover the smell of the pesticide and attract pests in the soil to approach the pesticide preparation. In addition, the nutrients contained in the sucrose and pomace fiber facilitate the attraction of pests to ingest the aged wheat grain particle carrier, thereby causing the pests to be poisoned by the stomach, thereby ensuring the control effect of pests in the soil.

[0028] In a third aspect, the present application provides an application of a pesticide preparation containing chlorantraniliprole and clothianidin, using the following technical solution: The invention discloses an application of a pesticide preparation containing chlorantraniliprole and clothianidin, wherein the pesticide preparation is buried in the soil for concealed application.

[0029] By adopting the above technical solution, it is ensured that there is no risk of drift and diffusion of pesticide preparations during the application process, and the pest control effect is good and the environmental compatibility is high.

[0030] In summary, this application has the following beneficial effects: 1. The product made of slow-release urea granules as carriers is used for sowing with urea, organic fertilizer, and compound fertilizer products. There will be no difference in bulk density and particle size. There is no need to worry about the difference in density of the stratification of medicine and fertilizer caused by the vibration of the seeder during machine sowing. It can effectively avoid uneven fertilization and application of medicine, which is conducive to saving labor and time. Moreover, according to the fertilizer requirements of different crops and the occurrence of pests and diseases, the mixing ratio of pesticide granules and fertilizers can be flexibly adjusted according to local conditions to meet the prevention and control and nutrition needs of more crops and more soil fertilizer types.

[0031] 2. The product prepared by using inactivated wheat seeds as carriers can be sown together with wheat seeds as medicine seeds. There will be no difference in bulk density. There is no need to worry about the difference in medicine and seed stratification density caused by the vibration of the seeder during machine sowing, which can effectively avoid uneven sowing and application of medicine.

[0032] 3. The granule products prepared with homemade carriers are similar to the use scenarios of traditional granules, but the particles are smoother, the particle size is more uniform, the product appearance is more regular, the drug shedding rate and dust are lower, which is beneficial to protecting the health of the applicators.

[0033] 4. In the process of preparing the medicine using the inactivated wheat aged grain carrier, during the layer-by-layer loading, repeated layer-by-layer coating and gradual cooling operations, white oil is used as an anti-caking agent for layer-by-layer coating. While the viscosity of the sucrose solution gradually increases, the stability of the layer-by-layer coating is improved, and it is not easy to cause adhesion between particles. While ensuring the finished product preparation effect, it can also prevent the medicine product from sticking and agglomerating after experiencing a high temperature environment during the shelf life. BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 It is a sustained-release effect curve diagram of Example 1 and Comparative Examples 1 and 2 of the present application. DETAILED DESCRIPTION

[0034] The present application is further described in detail below with reference to the embodiments.

[0035] Preparation example of clay carrier The following raw materials are all commercially available.

[0036] Preparation Example 1: The clay carrier is prepared by the following method: The clay particles are placed in a drum granulator, and then atomized water is sprayed into the drum granulator, the mass ratio of the clay particles to the atomized water is 1:0.5, and the drum granulator is continuously stirred during the water spraying period, and then pomace fiber is added, the average length of the pomace fiber is 40 μm, the pomace fiber is the fiber after apple juice is squeezed, the mass ratio of the clay particles to the pomace fiber is 1:0.2, and the adding speed of the pomace fiber is 60 g / min. During the adding process, the drum granulator is still stirred at a speed of 200 r / min to obtain spherical particles; clay particles, atomized water, and pomace fiber are added to the surface of the spherical particles in sequence, and the ratios of clay particles, atomized water, and pomace fiber are as above, and the operation of adding clay particles, atomized water, and pomace fiber is repeated until the particle size is 4 mesh, and the clay carrier is obtained by drying.

[0037] Preparation Example 2: This preparation example differs from Preparation Example 1 in that: The clay particles were placed in a drum granulator, and then atomized water was sprayed in, the mass ratio of the clay particles to the atomized water was 1:0.3, and the mixture was continuously stirred in the drum granulator during the water spraying period, and then pomace fiber was added, the mass ratio of the clay particles to the pomace fiber was 1:0.1, and the adding speed of the pomace fiber was 60 g / min. During the adding process, the drum granulator was still stirred at a speed of 200 r / min to obtain spherical particles; clay particles, atomized water, and pomace fiber were added to the surface of the spherical particles in sequence, and the ratios of clay particles, atomized water, and pomace fiber were the same as above, and the operation of adding clay particles, atomized water, and pomace fiber was repeated until the particle size was 3 mesh, and the mixture was dried to obtain a clay carrier.

[0038] Preparation Example 3: This preparation example differs from Preparation Example 1 in that: The clay particles were placed in a drum granulator, and then atomized water was sprayed in, the mass ratio of the clay particles to the atomized water was 1:0.6, and the mixture was continuously stirred in the drum granulator during the water spraying period, and then pomace fiber was added, the mass ratio of the clay particles to the pomace fiber was 1:0.3, and the adding speed of the pomace fiber was 60 g / min. During the adding process, the drum granulator was still stirred at a speed of 200 r / min to obtain spherical particles; clay particles, atomized water, and pomace fiber were added to the surface of the spherical particles in sequence, and the ratios of clay particles, atomized water, and pomace fiber were the same as above, and the operation of adding clay particles, atomized water, and pomace fiber was repeated until the particle size was 6 mesh, and the mixture was dried to obtain a clay carrier.

[0039] Example of preparation of inactivated wheat aged grain carrier The following raw materials are all commercially available.

[0040] Preparation Example 4: The inactivated wheat aged grain carrier was prepared by the following method: 1 kg of aged wheat grain particles were placed in 3.5 kg of hydrogen peroxide solution for immersion and dispersion for 3 minutes, the particle size of the aged wheat grain particles was 80 meshes, the concentration of the hydrogen peroxide solution was 3%, the aged wheat grain was filtered out, and dry steam inactivation treatment was performed at 135° C. for 30 minutes to obtain inactivated aged grain; The inactivated aged grain was cooled to 70°C, and immersed in a sucrose solution for 8 minutes, wherein the sucrose solution was a sucrose aqueous solution with a mass fraction of 2%, and the mass ratio of the inactivated aged grain to the sucrose solution was 1:3.5, and the aged wheat grain was filtered out and cooled to room temperature of 25°C to obtain the loaded aged grain; 0.15 kg of sodium alginate solution is evenly sprayed on the surface of 1 kg of loaded aged grain, and finally 0.3 kg of pomace fiber is evenly added, the sodium alginate solution is a sodium alginate aqueous solution with a mass fraction of 1%, the average length of the pomace fiber is 40 μm, the pomace fiber is the fiber after apple juice is squeezed, and the adding speed of the pomace fiber is 60 g / min. During the adding process, the loaded aged grain is continuously stirred at a speed of 200 r / min. After drying, the loaded aged grain, sodium alginate solution and pomace fiber are added to the surface again according to the above-mentioned weight ratio and method, and the loaded aged grain, sodium alginate solution and pomace fiber are repeatedly sprayed in turn until the particle size is 2 mesh to obtain an inactivated wheat aged grain carrier.

[0041] Preparation Example 5: This preparation example differs from Preparation Example 4 in that: 1 kg of aged wheat grain particles were placed in 2 kg of hydrogen peroxide solution for soaking and dispersion for 2 minutes, the aged wheat grains were filtered out, and dry steam inactivation treatment was performed at 130° C. for 35 minutes to obtain inactivated aged grains; The inactivated aged grain was cooled to 60°C, and immersed in a sucrose solution for 10 minutes, the mass ratio of the inactivated aged grain to the sucrose solution being 1:2, the aged wheat grain was filtered out, and after cooling to room temperature of 25°C, the loaded aged grain was obtained; 0.1 kg of sodium alginate solution is evenly sprayed on the surface of 1 kg of aged grain, and finally 0.2 kg of pomace fiber is evenly added. The adding rate of pomace fiber is 60 g / min. During the adding process, the aged grain is continuously stirred at a speed of 200 r / min. After drying, the aged grain, sodium alginate solution and pomace fiber are added to the surface again according to the above-mentioned weight ratio and method. The aged grain, sodium alginate solution and pomace fiber are sprayed repeatedly in sequence until the particle size is 2 mesh to obtain an inactivated wheat aged grain carrier.

[0042] Preparation Example 6: This preparation example differs from Preparation Example 4 in that: 1 kg of aged wheat grain particles were placed in 5 kg of hydrogen peroxide solution for immersion and dispersion for 4 minutes, the aged wheat grains were filtered out, and dry steam inactivation treatment was performed at 140°C for 25 minutes to obtain inactivated aged grains; The inactivated aged grain was cooled to 80°C, and immersed in a sucrose solution for 5 minutes, the mass ratio of the inactivated aged grain to the sucrose solution being 1:5, the aged wheat grain was filtered out, and after cooling to room temperature of 25°C, the loaded aged grain was obtained; 0.2kg of sodium alginate solution is evenly sprayed on the surface of 1kg of aged grain, and finally 0.4kg of pomace fiber is evenly added. The adding rate of pomace fiber is 60g / min. During the adding process, the aged grain is continuously stirred at a speed of 200r / min. After drying, the aged grain, sodium alginate solution and pomace fiber are added to the surface again according to the above-mentioned weight ratio and method. The aged grain, sodium alginate solution and pomace fiber are sprayed repeatedly in turn until the particle size is 3 mesh to obtain an inactivated wheat aged grain carrier.

[0043] Preparation Example of Isolation Layer Solution The following raw materials are all commercially available.

[0044] Preparation Example 7: The isolation layer solution is prepared by the following method: 1kg acrylic resin, 10kg polyvinyl alcohol, 1kg polyacrylate, 1kg cellulose derivative, 10kg sucrose, 1kg gum arabic, 200kg water; the cellulose derivative is sodium carboxymethyl cellulose; The preparation method is as follows: Acrylic resin, polyvinyl alcohol, polyacrylate, cellulose derivative, sucrose, gum arabic and water are mixed and stirred uniformly to obtain an isolation layer solution.

[0045] Preparation Example 8: This preparation example differs from Preparation Example 7 in that: 3kg of acrylic resin, 12kg of polyvinyl alcohol, 1.5kg of polyacrylate, 1.5kg of cellulose derivative, 15kg of sucrose, 3kg of gum arabic, 250kg of water, and 2kg of n-propyl lactate-modified soybean fiber; the cellulose derivative is composed of sodium carboxymethyl cellulose and cellulose acetate in a mass ratio of 1:0.25; the n-propyl lactate-modified soybean fiber is prepared by uniformly spraying 0.25kg of n-propyl lactate on the surface of 1kg of soybean fiber, and the average length of the soybean fiber is 80μm; The preparation method is as follows: Acrylic resin, polyvinyl alcohol, polyacrylate, cellulose derivative, sucrose, gum arabic, water and n-propyl lactate modified soybean fiber are mixed and stirred uniformly to obtain an isolation layer solution.

[0046] Preparation Example 9: This preparation example differs from Preparation Example 8 in that: 5kg of acrylic resin, 15kg of polyvinyl alcohol, 2kg of polyacrylate, 2kg of cellulose derivative, 20kg of sucrose, 5kg of gum arabic, 300kg of water and 3kg of n-propyl lactate-modified soybean fiber; the cellulose derivative is composed of sodium carboxymethyl cellulose and cellulose acetate in a mass ratio of 1:0.35; the n-propyl lactate-modified soybean fiber is prepared by uniformly spraying 0.1kg of n-propyl lactate on the surface of 1kg of soybean fiber. Example

[0047] The following raw materials are all commercially available.

[0048] Example 1: A pesticide preparation containing chlorantraniliprole and clothianidin: It comprises a spherical carrier and an effective component mother solution and an isolation layer coated layer by layer on the surface of the spherical carrier; The active ingredient mother solution contains the following raw materials: 37.5% chlorantraniliprole, 12.5% ​​clothianidin, 5% adjuvant, and 45% water; The isolation layer is prepared from an isolation layer solution; The preparation method is as follows: S1, selecting the clay carrier prepared in Preparation Example 1; selecting the isolation layer solution prepared in Preparation Example 7; S2, 37.5kg of chlorfenapyr and 12.5kg of clothianidin were mixed and subjected to air flow pulverization to obtain a mother powder; 5kg of auxiliary agent and 45kg of water were added to the mother powder and mixed and stirred evenly to obtain an effective ingredient mother solution; the auxiliary agent was composed of 3kg of sodium carboxymethyl cellulose solution and 2kg of tributyl phosphate; S3, rolling and stirring 960 kg of the spherical carrier in a drum granulator, then adding 32 kg of the active ingredient mother solution, continuing to stir, and mixing evenly to obtain a coating carrier; S4, 30kg of the isolation layer solution and 10kg of the color paste were mixed and stirred to obtain a composite solution; S5, spraying 40 kg of the composite liquid evenly on the surface of 992 kg of the cladding carrier, and drying to obtain a layer of preparation; S6. Spray 32 kg of active ingredient mother solution evenly on the surface of a layer of preparation. After drying, spray 40 kg of composite layer solution evenly again. Dry, repeat the operations of S3 and S5. After solidification and dispersion, a finished product is obtained. The finished product has a size of 4 mesh.

[0049] Embodiment 2: This embodiment differs from Embodiment 1 in that: The active ingredient mother solution contains the following raw materials: 35% chlorantraniliprole, 14% clothianidin, 4.6% adjuvant, and 46.4% water; During the preparation process: S1, selecting the clay carrier prepared in Preparation Example 2; selecting the isolation layer solution prepared in Preparation Example 7; S2, 35kg of chlorfenapyr and 14kg of clothianidin were mixed and subjected to air flow pulverization to obtain a mother powder; 4.6kg of auxiliary agent and 46.4kg of water were added to the mother powder and mixed and stirred evenly to obtain an effective ingredient mother solution; the auxiliary agent was composed of 2.6kg of sodium carboxymethyl cellulose solution and 2kg of tributyl phosphate; S3, rolling and stirring 950 kg of the spherical carrier in a drum granulator, then adding 30 kg of the active ingredient mother solution, continuing to stir, and mixing evenly to obtain a coating carrier; S4, 25kg of the isolation layer solution and 10kg of the color paste were mixed and stirred to obtain a composite solution; S5, spraying 40 kg of the composite liquid evenly on the surface of 980 kg of the cladding carrier, and drying to obtain a layer of preparation; S6. Spray 30 kg of active ingredient mother solution evenly on the surface of a layer of preparation. After drying, spray 40 kg of composite layer solution evenly again. Dry, repeat the operations of S3 and S5. After solidification and dispersion, a finished product is obtained. The finished product is 2 mesh.

[0050] Embodiment 3: This embodiment differs from Embodiment 1 in that: The active ingredient mother solution contains the following raw materials: 40% chlorantraniliprole, 12% clothianidin, 5.4% adjuvant, and 42.6% water; During the preparation process: S1, selecting the clay carrier prepared in Preparation Example 3; selecting the isolation layer solution prepared in Preparation Example 7; S2, 40kg of chlorfenapyr and 12kg of clothianidin were mixed and subjected to air flow milling to obtain a mother powder; 5.4kg of auxiliary agent and 42.6kg of water were added to the mother powder and mixed and stirred evenly to obtain an effective ingredient mother solution; the auxiliary agent was composed of 3.2kg of sodium carboxymethyl cellulose solution and 2kg of tributyl phosphate; S3, rolling and stirring 970 kg of the spherical carrier in a drum granulator, then adding 35 kg of the active ingredient mother solution, continuing to stir, and mixing evenly to obtain a coating carrier; S4, 32kg of the isolation layer solution and 10kg of the color paste were mixed and stirred to obtain a composite solution; S5, spraying 40.2 kg of the composite liquid evenly on the surface of 1005 kg of the cladding carrier, and drying to obtain a layer of preparation; S6. Spray 35 kg of active ingredient mother solution evenly on the surface of a layer of preparation. After drying, spray 40.2 kg of composite layer solution evenly again. Dry. Repeat the operations of S3 and S5. After solidification and dispersion, a finished product is obtained. The finished product has a size of 6 mesh.

[0051] Embodiment 4: This embodiment differs from Embodiment 1 in that: During the preparation process: S1. Select the inactivated aged wheat grain carrier prepared in Preparation Example 4; and select the isolation layer solution prepared in Preparation Example 8.

[0052] S6. Spray 32 kg of active ingredient mother solution evenly on the surface of a layer of preparation. After drying, spray 40 kg of composite layer solution evenly again and dry to obtain a semi-finished product. Repeat the operations of S3 and S5. Add white oil during the repeated operations. The mass ratio of the semi-finished product to the white oil is 100:2. During the repeated loading process, coat layer by layer and cool down layer by layer. Finally, the coated liquid is solidified and dispersed to obtain a finished product. The finished product is 4 mesh.

[0053] Embodiment 5: This embodiment differs from Embodiment 4 in that: During the preparation process: S1, the inactivated aged wheat grain carrier prepared in Preparation Example 5 is selected; the isolation layer solution prepared in Preparation Example 9 is selected.

[0054] Embodiment 6: This embodiment differs from Embodiment 4 in that: During the preparation process: S1, the inactivated aged wheat grain carrier prepared in Preparation Example 6 is selected; the isolation layer solution prepared in Preparation Example 8 is selected.

[0055] Embodiment 7: This embodiment differs from Embodiment 1 in that: During the preparation process, a slow-release urea carrier is selected.

[0056] Embodiment 8: This embodiment differs from Embodiment 1 in that: No pomace fiber was added during the preparation of the clay carrier.

[0057] Embodiment 9: This embodiment differs from Embodiment 4 in that: No hydrogen peroxide solution was added during the preparation of aged wheat grain pellets.

[0058] Embodiment 10: This embodiment differs from Embodiment 4 in that: The aged wheat grain particles are commercially available aged wheat grain particles without any processing.

[0059] Embodiment 11: This embodiment differs from Embodiment 4 in that: In the isolation layer solution, the n-propyl lactate-modified soybean fiber was replaced by soybean fiber of equal mass.

[0060] Comparative Example Comparative Example 1: The pesticide preparation was 0.16% chlorantraniliprole·thiamethoxam GR, purchased from Zhongcheng Guolian (Henan) Biotechnology Co., Ltd.

[0061] Comparative Example 2: The pesticide preparation was 40% chlorantraniliprole·thiamethoxam WDG, purchased from Dongguan Redefeng Biotechnology Co., Ltd.

[0062] Performance testing 1. Co-toxicity test The eggs of Chilo suppressalis collected from the field were artificially hatched and raised indoors with rice seedlings; the second-instar larvae of Chilo suppressalis were tested; the Chilo suppressalis was tested by the insect and seedling immersion method; the rice seedlings of about 30 days old were cut into rice stalks of about 18 cm, leaving a little rice root, washed and dried, soaked in a drug for 10 seconds and then taken out, the drug was selected from any one of Example 1 and Comparative Examples 1 and 2, dried, and put into a test tube with a little water left at the bottom of the tube; the reared second-instar Chilo suppressalis larvae were soaked in the drug for 10 seconds and then taken out, the drug on the surface of the insect body was sucked dry, and carefully moved into a test tube with rice seedlings treated with corresponding concentrations, and sealed with black cloth; after the treatment, the larvae were transferred to the insect breeding room for breeding and observation; the co-toxicity test data for the drug ratio are as follows.

[0063] Table 1 It can be seen from Example 1 and Comparative Examples 1 and 2 and Table 1 that the combination of chlorantraniliprole and clothianidin in a ratio of 1:3 has the best co-toxic effect.

[0064] 2. Particle index detection test The indicators of Example 1, Example 4, Example 7 and Comparative Example 1 were tested respectively.

[0065] Table 2 By comparing the test results of the relevant CIPAC standard methods, it can be clearly seen that the finished pesticide preparation prepared in the present application is superior to the commercially available pesticide preparations.

[0066] The product prepared using inactivated wheat seeds as carriers is used for sowing together with wheat seeds as medicine seeds. There will be no difference in bulk density, and there is no need to worry about the difference in medicine seed stratification density caused by the vibration of the seeder during machine sowing. This can effectively avoid uneven sowing and application of medicine.

[0067] 3. Sustained release test A plot test was carried out in the small trumpet stage of corn, and a pesticide application test with the same 100% effective dose was performed. The pesticide of Example 1 (referred to as Sadokin) was selected, and compared with Comparative Examples 1 and 2. Based on the data of chlorfenapyr pesticide residues in corn leaves measured by ZYD-NP6 pesticide residue detector every other day, a release curve was obtained to characterize the sustained-release effect of the granule product.

[0068] Combination Figure 1The results showed that the dosage concentration of the conventional 0.16% chlorfenapyr·thianidin GR product in plant leaves was higher than the minimum effective dose on the 9th day after application, and was lower than the effective dose on the 15th day after application, and decayed linearly until the 45th day after application, when it could still be detected in the leaves and was higher than the minimum limit of pesticide residues. This indicates that the product has poor quick-acting property after application, short effective period, and high risk of pesticide residues; the 40% chloranil·thianidin WDG product is applied by foliar spraying, and the dosage concentration on the first day after application and in the plant leaves is much higher than the minimum effective dose, and it is not lower than the minimum effective dose until the 9th day after application, and it is difficult to detect in the leaves 15 days after application, indicating that the agent has good quick-acting property and no residual risk, but the effective period is short, and multiple applications are required to achieve a better prevention and control effect; after using the product of Example 1, the minimum effective dose is reached on the 5th day after application, and it is lower than the minimum effective dose until the 25th day after application, and then it decays rapidly, and it is difficult to detect in the leaves on the 35th day after application, indicating that the product is quick to show effect, has a long effective period, and has a low risk of pesticide residues, and has obvious advantages of saving labor and time.

[0069] 4. Test on the effectiveness of preventing sugarcane borer The pesticide formulations were prepared by the methods of Example 1, Comparative Examples 1 and 2, respectively. Example 1 adopted the method of drone sowing, 2 kg / mu; Comparative Example 1 adopted the method of broadcasting, 20 kg / mu; Comparative Example 2 adopted the method of spraying, 0.02 kg / mu; the control effect (i.e., relative control effect) was detected with reference to GB / T17980.6-2000, and the data was recorded.

[0070] Table 3 The field efficacy data show that the product of Example 1 has a longer lasting effect, and even as a preventive drug, it can effectively control the occurrence of pests during the peak period of pests; the product of Comparative Example 1 has poor initial prevention effect and a shorter lasting effect, and fails to effectively control the development of pests in the later period; the product of Comparative Example 2 has good rapid effect and is suitable for application during the peak period of pests, but a single use cannot effectively control the development of pests, and during the peak period of sugarcane borer, the plants are tall and the leaf coverage is high, making manual spraying difficult, and it is difficult for flying spray droplets to effectively settle to the middle and lower parts of the plants, making application difficult.

[0071] 5. Wheat field prevention test In the wheat test field of Jiazhuang Township, Shanghe County, Jinan City, Shandong Province, 20 kg / mu of wheat seeds were used, and 2 kg / mu of the products of Examples 1-6 and 8-11 were sown together with the medicine seeds; 20 kg / mu of wheat seeds were used, and 2 kg / mu of the product of Example 7 was used for fertilization 15 days after sowing; 20 kg / mu of wheat seeds were used, and 20 kg / mu of the product of Comparative Example 1 was used for fertilization 15 days after sowing; 20 kg / mu of wheat seeds were used, and 0.02 kg / mu of the product of comparative example 2 was used for spraying and fertilization 20 days after sowing; The control effect of aphids in the seedling stage was investigated at 25 days and 40 days after sowing, and the control effect (recorded as relative control effect) data was tested with reference to GB / T17980.6-2000.

[0072] Table 4 Performance test table It can be seen from Examples 1-6 and Table 4 that the pesticide preparation can achieve simultaneous sowing of pesticide and seeds, can be fully mechanized, and can adapt to the differences in sowing amounts in different regions. The prevention effect data shows that it has a long lasting effect. Even as a preventive drug, it can effectively control the occurrence of pests during the peak period of pests. It can be seen from Example 7 and Table 4 that the prepared pesticide preparation can be applied together with the topdressing formula fertilizer and can adapt to the differences in fertilizer requirements under different fertility conditions. The control effect data shows that it has a long lasting effect and can ensure the high-standard control requirements of aphids throughout the pre-winter period.

[0073] It can be seen from Example 1 and Example 8 and Table 4 that pomace fiber is rich in dietary fiber, vitamins and minerals, and the surface of the pomace fiber is loaded with some chlorantraniliprole and clothianidin. When pests ingest the nutrients of the pomace fiber, they also ingest chlorantraniliprole and clothianidin, thereby facilitating the killing and control of pests. At the same time, the pomace fiber provides crops with signal substances for the direction of root growth, promotes the roots to absorb more agents, and further improves the control effect.

[0074] Combining Example 4 and Examples 9-11 and Table 4, it can be seen that in the preparation process of the aged wheat grain particles in Example 9, no hydrogen peroxide solution was added, and the aged wheat grain particles in Example 10 were commercially available aged wheat grain particles without any treatment. Compared with Example 4, the control effects of Examples 9 and 10 were worse than that of Example 4, indicating that the aged wheat grain was soaked and dispersed in a hydrogen peroxide solution, which killed the Aspergillus flavus in the aged wheat grain while promoting the thermal decomposition of the hydrogen peroxide solution, increasing the porosity of the aged wheat grain and further improving the killing effect of the Aspergillus flavus; utilizing the better flow effect of the sucrose solution at a higher temperature, the pomace fiber was further adhered to the surface of the aged wheat grain particles, and the nutrients contained in the sucrose and pomace fiber could provide signal substances for the direction of root growth for crops, promote the root system to absorb more agents, and thus achieve better control effects.

[0075] In Example 11, the soybean fiber modified with n-propyl lactate was replaced with soybean fiber of equal mass in the isolation layer solution. Compared with Example 4, the control effect of Example 11 was worse than that of Example 4, indicating that n-propyl lactate contains both hydrophilic groups and lipophilic groups, which facilitates adhesion with hydrophilic substances such as acrylic resin, polyvinyl alcohol, and sucrose, and can also attract and connect with the lipophilic groups of polyacrylates, thereby improving the cross-linking density of the isolation layer and ensuring the sustained-release control effect of the pesticide preparation.

[0076] Combining Example 1 with Comparative Examples 1 and 2 and Table 4, it can be seen that the carrier material used in the pesticide preparation prepared in Comparative Example 1 is an organic fertilizer granule containing a large amount of elements, which is easy to cause a high risk of fertilizer damage. If the dosage is reduced, the mother liquor of the active ingredient of the insecticide is insufficient, and the prevention effect is worrying. When used with finished fertilizers, the amount of fertilization operation is greatly increased, and the operation efficiency is reduced; and the initial prevention effect of the pesticide preparation is poor, the effective period is short, and the efficacy is not effectively exerted during the high incidence period of pests before winter. As the temperature before winter gradually decreases, the prevention effect decreases.

[0077] The pesticide preparation of Comparative Example 2 is an extrusion granulation product. The bulk density of the product is very different from that of fertilizer particles, so they cannot be sown together and can only be applied by spraying. Since its application period can be combined with pre-winter chemical control products, it can be mixed with pre-winter chemical control plant adjustment products in tanks. However, the current wheat application mode is mostly carried out by aerial spraying. The high-concentration tank mix of Comparative Example 2 has poor compatibility and is prone to flocculation and precipitation of the tank-mixed agents, which brings a greater risk of pesticide damage. At the same time, the pesticide preparation of Comparative Example 2 has good rapidity and good prevention and control effects. It is suitable for application during the peak period of pests. However, in order to ensure the efficacy, it must be applied alone and is not suitable for tank mixing with other types of products for pre-winter application, which increases the number of aerial spraying flights and the cost of aerial spraying operations.

[0078] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make modifications to the present embodiment without any creative contribution as needed, but such modifications are protected by the patent law as long as they are within the scope of the claims of the present application.

Claims

1. A pesticide preparation containing chlorantraniliprole and clothianidin, characterized in that: The pesticide preparation comprises a spherical carrier and an active ingredient mother solution and an isolation layer coated layer by layer on the surface of the spherical carrier; The active ingredient mother solution contains the following raw materials in percentage by weight: 35-40% chlorantraniliprole, 12-14% clothianidin, 4.8-5.4% adjuvant, and water is added to 100%; The isolation layer is prepared from an isolation layer solution.

2. A pesticide preparation containing chlorantraniliprole and clothianidin according to claim 1, characterized in that: The spherical carrier is one or more of a clay carrier, a slow-release urea carrier, and an inactivated wheat aged grain carrier.

3. A pesticide preparation containing chlorantraniliprole and clothianidin according to claim 2, characterized in that: The clay carrier is prepared by treating clay particles with atomized water and then bonding them with pomace fibers, wherein the mass ratio of clay particles, atomized water and pomace fibers is 1:0.3-0.6:0.1-0.3; then clay particles, atomized water and pomace fibers are added again, and the operation is repeated until the particle size reaches 3-6 meshes, and then drying is performed.

4. A pesticide preparation containing chlorantraniliprole and clothianidin according to claim 1, characterized in that: The auxiliary agent in the active ingredient mother solution comprises sodium carboxymethyl cellulose solution and tributyl phosphate in a mass ratio of 1.3-1.6:

1.

5. A pesticide preparation containing chlorantraniliprole and clothianidin according to claim 1, characterized in that: The isolation layer solution comprises the following raw materials in parts by weight: 1-5 parts of acrylic resin, 10-15 parts of polyvinyl alcohol, 1-2 parts of polyacrylate, 1-2 parts of cellulose derivative, 10-20 parts of sucrose, 1-5 parts of gum arabic, and 200-300 parts of water.

6. A pesticide preparation containing chlorantraniliprole and clothianidin according to claim 5, characterized in that: The isolation layer solution also includes 1-3 parts of n-propyl lactate modified soybean fiber; the n-propyl lactate modified soybean fiber is prepared from soybean fiber and n-propyl lactate in a mass ratio of 1:0.1-0.

25.

7. A pesticide preparation containing chlorantraniliprole and clothianidin according to claim 5, characterized in that: The cellulose derivative consists of sodium carboxymethyl cellulose and cellulose acetate in a mass ratio of 1:0.1-0.

35.

8. A method for preparing a pesticide preparation containing chlorantraniliprole and clothianidin according to any one of claims 1 to 7, characterized in that: The following steps are involved: S1, preparing a spherical carrier; preparing a spacer layer solution; S2, mixing chlorantraniliprole, clothianidin, adjuvant and water to obtain a mother solution of active ingredients; S3, rolling and stirring 950-970 parts by weight of the spherical carrier in a granulator, and then adding 30-35 parts of the active ingredient mother solution, mixing evenly, to obtain a coating carrier; S4, mixing the isolation layer solution and the color paste at a mass ratio of 2.5-3.2:1 to obtain a composite solution; S5, spraying the composite liquid uniformly on the surface of the cladding carrier at a mass ratio of 1:24.5-25, and drying to obtain a layer of preparation; S6. Spray the active ingredient mother liquid evenly on the surface of a layer of the preparation. After drying, spray the composite liquid evenly again, dry, repeat the operations of S3 and S5, and obtain the finished product after solidification and dispersion. The finished product has a size of 2-6 mesh.

9. The method for preparing a pesticide preparation containing chlorantraniliprole and clothianidin according to claim 8, characterized in that: The spherical carrier is an inactivated wheat aged grain carrier, and the inactivated wheat aged grain carrier is prepared by the following method: The aged wheat grain particles are placed in a hydrogen peroxide solution at a mass ratio of 1:2-5 for soaking and dispersion for 2-4 minutes, the aged wheat grains are filtered out, and dry steam inactivation treatment is performed at 130-140° C. for 25-35 minutes to obtain inactivated aged grains; The inactivated aged grain is cooled to 60-80°C, and is soaked and dispersed in a sucrose solution for 5-10 minutes, wherein the mass ratio of the inactivated aged grain to the sucrose solution is 1:2-5, and the aged wheat grain is filtered out and cooled to room temperature to obtain the loaded aged grain; Sodium alginate solution is evenly sprayed on the surface of the aged grain carrier, and finally pomace fiber is evenly added. The mass ratio of the aged grain carrier to the sodium alginate solution and the pomace fiber is 1:0.1-0.2:0.2-0.

4. After drying, the aged grain carrier, sodium alginate solution and pomace fiber are repeatedly sprayed on the surface in sequence until the particle size is 2-3 meshes, thereby obtaining an inactivated wheat aged grain carrier.

10. An application of a pesticide preparation containing chlorantraniliprole and clothianidin, characterized in that: The pesticide preparation prepared according to any one of claims 1 to 7 or the pesticide preparation prepared by the preparation method according to any one of claims 8 to 9 is buried in the soil for concealed application.

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