Fluopyram powder, preparation method and application thereof

Abstract

The application provides a fluopicolide powder, which comprises 0.1-2% fluopicolide, 5-55% rice husk charcoal, 10-85% filler, 1-5% yellow gelatin and 10-30% light calcium powder in percentage by mass. The powder has good diffusion, adsorption and anti-caking properties, thereby having good control effect on pine wood nematode disease.

Description

Technical Field

[0001] The present invention relates to fluopyram powder, a preparation method and application thereof, and belongs to the technical field of fluopyram powder preparation. Background Art

[0002] Fluopyram is a pyrazole amide broad-spectrum fungicide and nematicide with the chemical formula C 14 H8Cl3F3N2O is used not only to control leaf spot, leaf spot, gray mold, powdery mildew, sclerotinia, and early blight on vegetables and field crops like grapes, pears, bananas, apples, cucumbers, and tomatoes, but can also be used to control various nematodes on a variety of crops. It is a highly effective, environmentally friendly, and low-toxic nematicide. For large-scale crop applications, such as forests, those skilled in the art typically convert fluopyram into a powder and spray it via drone for pest control. Powders suitable for spraying in forests by drones need to meet the following performance conditions: (1) The powder has a qualified diffusibility, which should not be too strong or too weak. If the diffusibility is too strong, most of the powder will diffuse into the air when sprayed by drones, and only a small part will be adsorbed on the wood, resulting in low effective utilization of the powder. If the diffusibility is too weak, it will not be able to be effectively sprayed on the trees; (2) The powder should not have the phenomenon of adhesion and hardening, otherwise some of the powder will clump during the drone spraying operation, thereby affecting the spraying effect of the agent; (3) The powder has a strong leaf adsorption capacity, otherwise even if the powder is sprayed on pine wood, a large part of it will be lost and cannot penetrate into the pine tree body, resulting in a weakened preventive effect on pine wood nematode disease. However, the above three performances of existing fluopyram powders are often contradictory to each other, making it difficult to take them into account, which seriously affects the application efficiency and control effect.

[0003] Therefore, it is crucial to develop a fluopyram powder that combines the above three properties. Summary of the Invention

[0004] The present invention provides a fluopyram powder, a preparation method and an application thereof, which can effectively solve the above problems.

[0005] The present invention is achieved in that:

[0006] A fluopyram powder comprises, by mass percentage, 0.1%-2% fluopyram, 5%-55% rice husk charcoal, 10%-85% filler, 1%-5% xanthocollagen, and 10%-30% light calcium powder.

[0007] As a further improvement, the fluopyram powder comprises, by mass percentage, 1% fluopyram, 30% rice husk charcoal, 48% filler, 1% xanthan gum, and 20% light calcium powder.

[0008] As a further improvement, the fluopyram powder comprises, by mass percentage, 2% fluopyram, 5% rice husk charcoal, 62% filler, 1% xanthan gum, and 30% light calcium powder.

[0009] As a further improvement, the filler is one or more of talc powder and montmorillonite powder.

[0010] As a further improvement, the particle size of the fluopyram, rice husk charcoal, filler, and light calcium powder is 8-12 μm.

[0011] A method for preparing the above-mentioned fluopyram powder comprises coarsely grinding fluopyram, light calcium powder, and a portion of filler, mixing them, and then ultrafinely grinding them again to a particle size of 8-12 μm; then grinding the remaining filler to a particle size of 8-12 μm and mixing it with xanthan gum; and finally fully mixing all the above-mentioned substances to form a finished compound powder.

[0012] A use of the fluopyram powder in preventing and controlling crop diseases and insect pests.

[0013] As a further improvement, the crop pest is pine wood nematode.

[0014] The beneficial effects of the present invention are:

[0015] The fluopyram powder of the present invention has an appropriate content ratio of the three components of xanthocollagen, light calcium powder and rice husk charcoal, so that the diffusibility, adsorption and anti-caking properties of the powder are balanced and taken into account, thereby achieving optimal performance of the powder, making it suitable for drone spraying, and further improving the pest and disease control effect of the fluopyram powder. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for use in the embodiments. It should be understood that the following drawings only illustrate certain embodiments of the present invention and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other relevant drawings can be obtained based on these drawings without paying any creative work.

[0017] Figure 1 This is a graph comparing the adsorption effects of different powder formulations provided in the embodiments of the present invention.

[0018] Figure 2 This is a result diagram comparing the compaction conditions of different powder formulations provided in the embodiments of the present invention.

[0019] Figure 3 This is a statistical area map of dead wood caused by pine wood nematode disease in the application area of ​​the powder spraying in 2019 provided by an embodiment of the present invention.

[0020] Figure 4 The statistical area chart of pine wilt disease dead wood in the control area without spraying powder provided by the embodiment of the present application is shown in the following table.

[0021] Note: In the chart, different lowercase letters represent significant differences at p<0.05, the same marked letters represent no significant difference, and different marked letters represent significant difference. DETAILED DESCRIPTION

[0022] In order to make the purpose, technical scheme and advantages of the embodiments of the present application clearer, the technical scheme in the embodiments of the present application will be described clearly and completely below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application. Therefore, the following detailed description of the embodiments of the present application provided in the drawings is not intended to limit the scope of the claimed present application, but only represents selected embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0023] The embodiment of the present application provides a fluopyram powder, which comprises 0.1-2% fluopyram, 5-55% rice husk charcoal, 10-85% filler, 1-5% yellow collagen and 10-30% light calcium powder in terms of mass percentage. The ingredients of the powder synergize with each other. The rice husk charcoal, which is a waste material, is used as a carrier of the original pesticide after being ground into powder. The filler is matched with the rice husk charcoal, so that the pesticide particles can enter the gaps of fibers, effectively controlling the diffusion of the powder. The yellow collagen wrapped outside maintains the adsorption of the powder. At the same time, the light calcium powder can also play a lubricating role to prevent hardening. After strict proportioning, the functions of each component reach a balanced state, so that the performance of the powder reaches the best, with good diffusion, adsorption and anti-hardening properties, suitable for unmanned aerial vehicle spraying, improving the pesticide application efficiency, and thus better playing the disease and pest control effect of fluopyram.

[0024] Rice husk charcoal, i.e. carbonized rice husk, refers to charcoal material formed by heating rice husk to a temperature below its ignition point so that it does not burn completely. It is light in weight, has good air permeability and moderate moisture absorption. This material can not only control the excessive diffusion of the powder, but also prevent hardening. In addition, the low thermal conductivity of the rice husk charcoal can maintain the ground and water temperature, promote plant growth and reduce cold damage, at the same time, promote the effectiveness of P, K, Ca and Mg, provide nutrients for plants and promote nitrogen fixation. After application in the forest, it will not release new carbon dioxide due to the degradation of cellulose.

[0025] The role of light calcium powder is to provide lubrication for the ingredients and prevent the powder from hardening during the spraying process.

[0026] Collagen prevents drift and reduces excessive spread of the sprayed pesticide, allowing it to adhere well to leaves and improving its long-lasting effectiveness. Collagen exhibits high viscosity, high temperature resistance, water retention, salt tolerance, and shear resistance. It is often used as a stabilizing suspending agent, controlling droplet size and preventing drift during spraying. This increases the amount of active ingredient retained on crops and improves the long-lasting effectiveness of the pesticide.

[0027] Fillers also affect the diffusibility of the powder and, together with rice husk charcoal, regulate the diffusibility of the powder. An appropriate proportion of rice husk charcoal can maintain the diffusibility of the powder within an appropriate range. The filler is preferably one or more of talc powder and montmorillonite powder.

[0028] As a further improvement, the fluopyram powder comprises, by weight, 2% fluopyram, 5% rice husk charcoal, 62% filler, 1% xanthan gum, and 30% light calcium powder. This fluopyram powder has a longer diffusion distance within forests and is suitable for large-scale drone spraying in concentrated, contiguous woodlands.

[0029] As a further improvement, the fluopyram powder comprises, by weight, 1% fluopyram, 30% rice husk charcoal, 48% filler, 1% xanthan gum, and 20% light calcium powder. This fluopyram powder has a shorter diffusion distance within a forest and is suitable for drone spraying in scattered pine forests.

[0030] As a further improvement, the particle size of the fluopyram, rice husk charcoal, filler, and light calcium powder is 8-12 μm.

[0031] A method for preparing the aforementioned fluopyram powder comprises coarsely grinding fluopyram, light calcium powder, and a portion of filler, mixing them, and then ultrafinely grinding them to a particle size of 8-12 μm. The remaining filler is then ground to a particle size of 8-12 μm and mixed with xanthan gum. Finally, all of the above substances are thoroughly mixed to form a finished composite powder. This floating particle size allows for better drifting of the powder, facilitating its diffusion.

[0032] A use of the fluopyram powder in controlling crop diseases and insect pests. The fluopyram powder has good diffusibility, adsorption, and anti-caking properties, and is suitable for drone spraying, thereby better exerting the pest control effect of fluopyram.

[0033] As a further improvement, the crop pest is pine wood nematode. Fluopyram can penetrate into pine trees by spraying, having a preventive and therapeutic effect on pine wood nematode disease. In this application, a flying drone is used for forest spraying. The host plant of pine wood nematode disease is a Pinus host plant, including but not limited to one of the following: Masson pine (Pinus massoniana), Black pine (P. thunbergii), Cedrus deodara, Red pine (P. densiflora), Larch (Larix gmelini), and Yunnan pine (P. yunnanensis). The fluopyram powder is suitable for preventing and controlling pine wood nematode disease in the above-mentioned host plants.

[0034] Example 1

[0035] Preparation of Fluopyram Powder

[0036] Weigh all ingredients according to the recipe, pour into a blender and mix thoroughly to prepare 5 kg of fluopyram powder. The recipe is shown in Table 1.

[0037] Preparation method: Fluopyram, light calcium powder, talc powder and part of montmorillonite powder are coarsely crushed and mixed, and then ultrafinely ground again to a particle size of about 10 μm; then the remaining montmorillonite is finely ground to a particle size of about 10 μm and mixed with xanthan gum; finally, all the above substances are fully mixed to form a finished compound powder.

[0038] Table 1 Different powder formulations

[0039]

[0040] Example 2

[0041] Performance test of fluopyram powder

[0042] The experimental method is as follows:

[0043] 1) Determination of adsorption effect: In a nursery of 3-year-old Masson pine seedlings with a height of 1.1m-1.3m, the prepared powder was sprayed on the branches and leaves using a duster. Three pine seedlings were randomly selected for each formula and the residual concentration of fluopyram on the branches and leaves was measured to determine the adsorption effect of the powder. The results of the comparison of the adsorption effect of different powder formulas are shown in the figure below. Figure 1 and as shown in Table 2.

[0044] Depend on Figure 1Compared to the most effective formulations 1 and 2, the residual concentration of the powder on branches and leaves in formulation 9, which lacked xanthan gum, was significantly lower, indicating poor adsorption. However, when the formulations contained both reduced gum and either light calcium powder (formula 10) or rice husk charcoal (formula 11), the residual concentration of the powder was significantly higher than that of formulation 9. When the xanthan gum content exceeded 5% (formula 8), the powder's adsorption capacity was also reduced. When the light calcium powder content was less than 10% or exceeded 30%, the powder became compacted (formulas 4 and 5), hindering sprayability and impairing its adsorption to leaves. When the rice husk charcoal content was less than 5% or exceeded 55%, the powder's diffusivity was impaired, thus affecting its adsorption to leaves (formulas 6 and 7). Adsorption to branches and leaves was the worst when the ratios of two or more of the three ingredients exceeded the appropriate range (formulas 12-15), or when the formulation contained only one of the three ingredients (formulas 16-18). Among them, the sum of the adsorption capacities of formulas 16, 17, and 18 is less than that of formula 1, indicating that xanthan gum, light calcium powder, and rice husk charcoal have a synergistic effect and jointly improve the adsorption effect of the powder.

[0045] 2) Prevention of compaction: A Masson pine forest stand was selected in Cangshan District, Fuzhou City, Fujian Province (26°4'50.00"N, 119°14'25.23"E). Each test plot was about 15 mu. A battery-powered multi-rotor plant protection drone (powder sprayer) was used to conduct a forest simulation operation experiment. The completion time and flight sorties of a 5kg spraying operation were recorded, and the amount of powder sprayed per unit time was calculated to determine whether the powder formula had compaction. Comparison of compaction of different powder formulas is as follows: Figure 2 and as shown in Table 2.

[0046] Depend on Figure 2 It can be seen that compared with the most effective formulas 1 and 2, when formula 10 does not contain light calcium powder, the spray volume per unit time using the drone is significantly reduced, indicating that the powder has serious compaction. When the formula contains light calcium powder and one of the reducing gum (formula 11) or rice husk charcoal (formula 9), the spray volume per unit time is significantly higher than that of formula 10. When the light calcium powder content is less than 10% or exceeds 30%, the powder will also cause compaction (formulas 4 and 5). When the xanthan gum content is less than 1% or exceeds 5% (formulas 8 and 9) and when the rice husk powder content is less than 5% or exceeds 55% (formulas 6 and 7), although the spray volume per unit time is increased compared to formula 10, compaction still occurs. When the ratio of two or more of the three ingredients exceeds the appropriate range (formulas 12-15), or when the formula contains only one of the three ingredients (formulas 16-18), the powder compaction phenomenon is more serious.

[0047] 3) Diffusion Assessment: New 1m x 1m black non-woven fabrics were laid at 1m, 10m, and 30m distances around each test plot (east, south, west, and north) to observe the powder's diffusion range (test plots within the same forest can be reused). After spraying each formulation listed in Table 1, the powder's diffusion distance was determined by manually inspecting the powder's fall from each non-woven fabric. A diffusion distance of 10-30m indicated good diffusion; a diffusion distance of <10m or >30m indicated unsatisfactory diffusion. Each powder was tested five times, and the pass rate was calculated. The test results are shown in Table 2.

[0048] Table 2 Summary of spraying conditions of different powder formulations

[0049]

[0050]

[0051] Note: Different lowercase letters indicate significant differences at p < 0.05, the same lowercase letters indicate insignificant differences, and different lowercase letters indicate significant differences.

[0052] As shown in Table 2, powder formulations 1 and 2 have the best diffusion properties. When formulation 11 does not contain rice husk charcoal, the qualified rate of the range of the pesticide sprayed by drone is only 20%. When the formulation contains rice husk charcoal and either reduced gum (formulation 10) or light calcium powder (formulation 9), the qualified rate of the pesticide diffusion is higher than that of formulation 11. When the rice husk charcoal content is less than 5% or exceeds 55%, the diffusion properties of the formulation are also low (formulations 6 and 7). When the xanthan gum content exceeds 5% (formulation 8) and when the light calcium powder content is less than 10% or exceeds 30% (formulations 4 and 5), the diffusion properties of the powder are improved compared to formulation 11, but still not high. When the ratios of two or more of the three ingredients exceed the appropriate range (formulations 12-15), or when the formulation contains only one of the three ingredients (formulations 16-18), the diffusion properties of the powder are seriously affected. Among them, the diffusion qualification rate of the powders of formulas 16-18 is zero, and the diffusion qualification rate of formula 1 is 100%, indicating that xanthan gum, light calcium powder and rice husk charcoal have a synergistic effect and jointly improve the diffusion qualification rate of the powders. Their ratio needs to be within a certain range to enable the powder to achieve the best effect.

[0053] Example 3

[0054] Formula 1 (1% xanthan gum, 30% light calcium powder, 5% rice husk charcoal, 2% fluopyram, 31% talc powder and 31% montmorillonite powder) was selected to test the effects of different industrial and agricultural cellulosic wastes on the powder. The rice husk charcoal in the formula was replaced with an equal amount of industrial and agricultural cellulosic waste, such as straw powder and wheat bran powder. The specific formula is shown in Table 3.

[0055] Table 3 Powder formulations for different industrial and agricultural cellulose wastes

[0056]

[0057] The method of Example 2 was used to test powders of different industrial and agricultural cellulose wastes. The test results are shown in Table 4 below:

[0058] Table 4 Effects of different industrial and agricultural cellulose wastes on powders

[0059]

[0060] Note: Different lowercase letters indicate significant differences at p < 0.05, the same lowercase letters indicate insignificant differences, and different lowercase letters indicate significant differences.

[0061] The results in Table 4 show that when the rice husk charcoal in Formulation 1 is replaced with straw powder or wheat bran powder, the powder's diffusion is poor, resulting in compaction and impaired adsorption to foliage in forests. Therefore, rice husk charcoal is a suitable raw material for developing powder formulations, ensuring efficient powder diffusion during forest application while also preventing compaction. Furthermore, its inherent properties, such as soil improvement and insecticide activity, also meet current requirements for environmentally friendly pesticide application.

[0062] Example 4:

[0063] Powder control efficiency in forests

[0064] Powder: Formula 1 (1% xanthan gum, 30% light calcium powder, 5% rice husk charcoal, 2% fluopyram, 31% talc powder and 31% montmorillonite powder).

[0065] Application: Six pure Pinus massoniana stands in the pine wood nematode epidemic area of ​​Jin'an District, Fuzhou City were selected. Each stand is about 15 mu in area and has a canopy density of more than 0.7. Three stands were used as experimental sites (application areas), and the other three stands were left untreated as control areas. UAV photography of the demonstration forest plots was conducted every year. The experimental sites were applied with 1000g / hm2 of pesticide in May 2019. 2The canopy of Pinus massoniana was sprayed with aerial spraying at a dosage of , and no pesticide was applied in the control area. The number of dead trees in Pinus massoniana was subsequently counted in November 2019 and November 2020.

[0066] Statistics: The dead pine trees were counted by drone aerial photography at an altitude of 150-200m over the sprayed and control areas. The small images were stitched together into a regional map, and the images were analyzed using a computer to mark suspected dead trees. Based on the identified dead pine tree distribution images, manual on-site confirmation was conducted in the test area, and the dead pine trees were counted. The application effect was calculated and evaluated according to the following formula:

[0067]

[0068]

[0069] Table 5 Statistics and control of dead wood in the powder spraying sites

[0070]

[0071] The statistical area maps of dead wood caused by pine wilt disease in the sprayed area and the control area without spraying powder in 2019 are as follows: Figure 3 and 4 shown.

[0072] As shown in Table 5, after the powder was applied, the average control efficiency in the first and second years was 78.95% and 85.86%, respectively, indicating that the powder can effectively prevent pine wood nematode disease in the forest, and the control efficiency continued to improve over the two years.

[0073] The foregoing description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Those skilled in the art will readily appreciate that various modifications and variations are possible. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the present invention are intended to be within the scope of protection of the present invention.

Claims

1. A fluopyram powder, characterized in that Calculated by mass percentage, it includes 1% fluopyram, 30% rice husk charcoal, 48% filler, 1% yellow collagen, and 20% light calcium powder; or it includes 2% fluopyram, 5% rice husk charcoal, 62% filler, 1% yellow collagen, and 30% light calcium powder; The filler is one or more of talc powder and montmorillonite powder; the particle size of the fluopyram, rice husk charcoal, filler and light calcium powder is 8-12 μm.

2. A method for preparing the fluopyram powder according to claim 1, characterized in that: Fluopyram, light calcium powder, and part of the filler are coarsely crushed and mixed, and then ultrafinely crushed again to a particle size of 8-12 μm; then the remaining filler is crushed to a particle size of 8-12 μm and mixed with xanthan gum; finally, all of the above substances are fully mixed to form a finished compound powder.

3. Use of the fluopyram powder according to claim 1 in preventing and controlling crop diseases and insect pests.

4. The use according to claim 3, characterized in that The crop pest is pine wood nematode.

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