A fluazamamide-based composite insecticide and a preparation method thereof

Abstract

The present application relates to the technical field of compound pesticide, in particular to a kind of composite insecticide based on fluopyram and a preparation method thereof, the present application is obtained by the combination of fluopyram composition, insecticidal active substance, insecticide adjuvant and dispersant, emulsifier and defoaming agent, a kind of composite insecticide with good stability, high utilization rate, good insecticidal effect;In the present application, polylactic acid with high thermal stability and biodegradability and cellulose nanocrystal with emulsifying capacity are used to load fluopyram, obtaining fluopyram microspheres with high photothermal stability, high utilization rate and slow-release performance, and the fluopyram microspheres are mixed with fluopyram, so that the fluopyram composition can rapidly kill insects and continuously exert insecticidal effect;Insecticide adjuvant prevents and controls nematode from multiple dimensions, and has wide application prospect.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of compound pesticides, and particularly relates to a fluopyram-based composite insecticide and a preparation method thereof. BACKGROUND

[0002] The grubs, larvae of scarab beetles, feed on the tender stems of peanut seedlings, and when the plants wither and die, they move to other plants to continue the damage. In addition, the wounds caused by grubs can also induce diseases. Among them, the phytophagous grubs have a wide range of food and can harm many crops, economic crops and flower seedlings. They prefer to eat newly sown seeds, roots, tubers and seedlings, causing great damage.

[0003] Peanut root-knot nematode is a pathogenic nematode that has a serious impact on peanut crops, belonging to the genus Meloidogyne. Peanut root-knot nematode disease is a global disease that occurs in almost all areas where peanuts are grown, especially in various peanut production areas in China. Peanut root-knot nematode can reduce peanut yield, cause poor fruit development, and may cause small white bumps on the shell, which may turn brown and scabby in the later stage.

[0004] Peanut root-knot nematode and grubs are common underground pests of peanuts and other crops, each of which damages the roots of plants in different ways, leading to impaired crop growth and reduced yield. Fluopyram is a highly effective fungicide belonging to the succinate dehydrogenase inhibitor class of compounds. It mainly inhibits the activity of succinate dehydrogenase in fungal cells, thereby preventing fungal energy metabolism and achieving fungicidal effects.

[0005] In the prior art, insecticides containing fluopyram usually use multiple insecticides with insecticidal effects to compound, thereby improving the insecticidal effect. However, fluopyram is unstable under light and heat conditions, and simple compounding leads to low utilization rate of fluopyram, reduced insecticidal efficiency, and increased insecticide usage, which not only loses economic benefits but also causes drug resistance.

[0006] Therefore, according to the related technology in the above, it is urgent to develop a fluopyram-based composite insecticide and a preparation method thereof. SUMMARY

[0007] Therefore, according to the related technology in the above, it is urgent to develop a fluopyram-based composite insecticide and a preparation method thereof.

[0008] To achieve the above purpose, the present application provides a fluopyram-based composite insecticide and a preparation method thereof.

[0009] A fluopyram-based composite insecticide comprises the following raw materials by mass:

[0010] Fluopicolide composition 37.2-49 parts; insecticidal active 15.5-26.7 parts; antifoaming agent 1-2 parts; dispersing agent 8-11.3 parts; emulsifying agent 13.5-17 parts; insecticidal adjuvant 4.5-8.2 parts; deionized water 480-650 parts;

[0011] The insecticidal adjuvant is prepared from insecticidal adjuvant A, insecticidal adjuvant B and insecticidal adjuvant C;

[0012] The fluopicolide composition is obtained by mixing fluopicolide, fluopicolide microspheres in a mass ratio of 6-9:13-17;

[0013] The fluopicolide microspheres are prepared from fluopicolide, cellulose nanocrystals and polylactic acid.

[0014] Preferably, the insecticidal adjuvant A is obtained by mixing limonene, garlicin and humic acid in a mass ratio of 4-7:4-7:13-19;

[0015] The insecticidal adjuvant B is silicon carbide nanoparticles;

[0016] The insecticidal adjuvant C is prepared from Bacillus subtilis and Bacillus megaterium;

[0017] The particle size of the silicon carbide nanoparticles is 50-60 nm.

[0018] Preferably, the mass ratio of insecticidal adjuvant A, insecticidal adjuvant B and insecticidal adjuvant C in the insecticidal adjuvant is 11.5-15:0.2-0.5:4-6.

[0019] Preferably, the preparation method of the fluopicolide microspheres is as follows:

[0020] Step A1. Disperse cellulose nanocrystals in deionized water, and add sodium chloride to mix uniformly to obtain an aqueous phase suspension;

[0021] Step A2. Add fluopicolide and polylactic acid to dichloromethane, mix uniformly to obtain an oil phase, then add the oil phase to the aqueous phase suspension, ultrasonically treat at 0-4℃ for 10-15 min, then place in a fume hood and stir at a rotation speed of 400-550 rpm for 22-24 h, centrifuge, wash with deionized water, freeze-dry to obtain fluopicolide microspheres.

[0022] Preferably, the amount ratio of cellulose nanocrystals, deionized water and sodium chloride in step A1 is 0.04-0.08 g:20-40 mL:0.04-0.08 g.

[0023] Preferably, the amount ratio of the fluopicolide, polylactic acid and dichloromethane in step A2 is 8-13mg:0.18-0.25g:9-15mL.

[0024] Preferably, the insecticidal active substance is mixed by imidacloprid, abamectin and thiamethoxam in the mass ratio of 18.6-24:7-11.3:5.3-8.5.

[0025] Preferably, the defoaming agent is silicone defoaming agent HY1572.

[0026] The dispersant is at least one of phosphate ester dispersant 1015, sodium dodecyl benzene sulfonate and sodium dodecyl sulfate.

[0027] The emulsifier is at least one of Tween 60, calcium dodecyl benzene sulfonate and pesticide emulsifier 2201.

[0028] Preferably, the bacillus subtilis and bacillus megaterium in the insecticide adjuvant C are in the form of bacillus subtilis bacterial suspension and bacillus megaterium bacterial suspension.

[0029] The mass ratio of the bacillus subtilis bacterial suspension and the bacillus megaterium bacterial suspension is 3-7:2-5.

[0030] The viable bacterial count of bacillus subtilis in the insecticide adjuvant C is 4×10 8 CFU / mL, and the viable bacterial count of bacillus megaterium is 2×10 10 CFU / mL. 7 9 CFU / mL.

[0031] A preparation method of a fluopicolide-based composite insecticide, comprising the following steps:

[0032] Step S1. Sodium carboxymethyl cellulose is added in deionized water, after stirring uniformly, silicon carbide nanoparticles are added, to obtain a silicon carbide nanoparticle suspension, which is mixed with insecticide adjuvant A and insecticide adjuvant C to obtain an insecticide adjuvant.

[0033] Step S2. The dispersant and the emulsifier are added in deionized water, stirring at a speed of 300-400rpm for 10-15min, then the fluopicolide composition and the insecticidal active substance are added and stirred for 30-50min, and then the insecticide adjuvant and the defoaming agent are added and mixed uniformly, to obtain the fluopicolide-based composite insecticide.

[0034] The amount ratio of the deionized water, sodium carboxymethyl cellulose and silicon carbide nanoparticles in step S1 is 40-60mL:0.01-0.02mg:0.75-1mg.

[0035] The beneficial effects of the present application:​

[0036] The application provides a fluopicolide-based composite insecticide and a preparation method thereof. The application is prepared by compounding a fluopicolide composition, an insecticidal active substance, an insecticidal adjuvant, a dispersant, an emulsifier and an antifoaming agent, and has good stability, high utilization rate and good insecticidal effect. In the application, polylactic acid with high thermal stability and biodegradability and cellulose nanocrystals with emulsifying capacity are used to load fluopicolide, and fluopicolide microspheres with high photothermal stability, high utilization rate and slow-release performance are obtained. The fluopicolide microspheres are mixed with fluopicolide, so that the fluopicolide composition can rapidly kill insects and continuously exert insecticidal effect. In the insecticidal adjuvant, the insecticidal adjuvant A can enhance soil organic matter, promote the reproduction of nematode antagonistic microorganisms, has a small amount of irritating odor, accelerates the death of nematodes and inhibits the hatching of nematode eggs. The insecticidal adjuvant B is absorbed into the body of nematodes, and then affects the survival of nematode larvae. The insecticidal adjuvant C has a remarkable control effect on nematodes, and is mixed with the insecticidal adjuvant A and the insecticidal adjuvant B to control nematodes from multiple dimensions. Compared with the prior art, the application has a wide application prospect. DETAILED DESCRIPTION

[0037] In order to make the purpose, technical scheme and advantages of the application clearer, the application is further described in detail below with reference to specific examples.

[0038] The sources and properties of some raw materials used in the application are as follows:

[0039] The Bacillus subtilis used in the application is Bacillus subtilis 2JQ3, which is disclosed in the invention patent with the authorized publication number “CN114507626B” and the name “Bacillus subtilis 2JQ3 with toxic and killing activity on root-knot nematodes and application thereof”, and the preservation number is CGMCC No. 23580.

[0040] The Bacillus megaterium used in the application is Bacillus megaterium BCCX15, which is disclosed in the invention patent with the authorized publication number “CN110669691B” and the name “Bacillus megaterium for preventing and treating plant nematode diseases and application thereof”, and the preservation number is CGMCC NO. 18007.

[0041] Example 1: A preparation method of a fluopicolide-based composite insecticide, comprising the following steps:

[0042] S1. Take beef extract 3 g, proteose peptone 10 g, NaCl 5 g, add 1000 mL of distilled water, heat to complete dissolution at 40°C, adjust pH to 7, filter, and sterilize at 121°C for 15 min to obtain a NA liquid medium; take beef extract 10 g, proteose peptone 20 g, NaCl 5 g, add 1000 mL of distilled water, heat to complete dissolution at 40°C, and sterilize at 121°C for 20 min to obtain a beef extract proteose peptone medium;

[0043] S2. The activated Bacillus megaterium is inoculated into the beef extract proteose peptone liquid medium, and cultured at 28°C and 140 rpm for 3 days. After centrifugation of the fermentation broth at 8000 rpm for 10 min, the bacterial cells are collected and suspended in sterile water to obtain a Bacillus megaterium bacterial suspension. The Bacillus subtilis is inoculated into the NA liquid medium, and cultured at 28°C and 180 rpm for 1 day. After centrifugation of the bacterial liquid, the supernatant is removed, the bacterial cells are collected, and suspended in sterile water to obtain a Bacillus subtilis bacterial suspension. Then, 3 g of the Bacillus subtilis bacterial suspension and 2 g of the Bacillus megaterium bacterial suspension are mixed to obtain an insecticidal adjuvant C;

[0044] S3. 4 g of limonene, 4 g of garlicin, and 13 g of humic acid are mixed to obtain an insecticidal adjuvant A. 0.01 mg of sodium carboxymethyl cellulose is added to 40 mL of deionized water, stirred uniformly, and then 0.75 mg of silicon carbide nanoparticles is added to obtain an insecticidal adjuvant B;

[0045] S4. 0.04 g of cellulose nanocrystals is dispersed in 20 mL of deionized water, and 0.04 g of sodium chloride is added and mixed uniformly to obtain an aqueous phase suspension;

[0046] S5. 8 mg of fluopyram and 0.18 g of polylactic acid are added to 9 mL of dichloromethane, mixed uniformly to obtain an oil phase, which is then added to the aqueous phase suspension, ultrasonically treated at 0°C for 10 min, and then stirred at a speed of 400 rpm in a fume hood for 22 h, centrifuged, washed with deionized water, and freeze-dried to obtain fluopyram microspheres. 6 g of fluopyram and 13 g of fluopyram microspheres are mixed to obtain a fluopyram composition;

[0047] S6. 11.5 g of the insecticidal adjuvant A, 0.2 g of the insecticidal adjuvant B, and 4 g of the insecticidal adjuvant C are mixed to obtain an insecticidal adjuvant. 18.6 g of imidacloprid, 7 g of abamectin, and 5.3 g of thiamethoxam are mixed uniformly to obtain an insecticidal active substance;

[0048] S7. Add 8 g of phosphate ester dispersant 1015 and 13.5 g of calcium dodecylbenzenesulfonate into 480 g of deionized water, stir for 10 min at a rotation speed of 300 rpm, then add 37.2 g of fluopyram composition and 15.5 g of insecticidal active substance, stir for 30 min, and then add 4.5 g of insecticidal adjuvant and 1 g of silicone antifoaming agent HY1572, and mix uniformly to obtain a fluopyram-based composite insecticide.

[0049] Example 2: A preparation method of a fluopyram-based composite insecticide, comprising the following steps:

[0050] S1. Weigh 3 g of beef extract, 10 g of proteose peptone, and 5 g of NaCl, add 1000 mL of distilled water, heat to complete dissolution at 43°C, adjust the pH to 7, filter, and then sterilize at 121°C for 15 min to obtain a NA liquid medium; weigh 10 g of beef extract, 20 g of proteose peptone, and 5 g of NaCl, add 1000 mL of distilled water, heat to complete dissolution at 43°C, and sterilize at 121°C for 20 min to obtain a rich beef extract proteose peptone medium;

[0051] S2. Inoculate the activated Bacillus megaterium into the beef extract proteose peptone liquid medium, and shake culture at 28°C and 140 rpm for 3 d; centrifuge the fermentation broth at 8000 rpm for 10 min, collect the bacterial cells, and configure a bacterial suspension with sterile water to obtain a Bacillus megaterium bacterial suspension; inoculate the Bacillus subtilis into the NA liquid medium, and shake culture at 28°C and 180 rpm for 1 d; centrifuge the bacterial liquid, remove the supernatant, collect the bacterial cells, and configure a bacterial suspension with sterile water to obtain a Bacillus subtilis bacterial suspension; mix 4 g of the Bacillus subtilis bacterial suspension and 2.5 g of the Bacillus megaterium bacterial suspension to obtain an insecticidal adjuvant C;

[0052] S3. Mix 5 g of limonene, 5 g of garlicin, and 14 g of humic acid to obtain an insecticidal adjuvant A, add 0.013 mg of sodium carboxymethyl cellulose to 45 mL of deionized water, stir uniformly, and then add 0.8 mg of silicon carbide nanoparticles to obtain an insecticidal adjuvant B;

[0053] S4. Disperse 0.05 g of cellulose nanocrystals in 25 mL of deionized water, and add 0.05 g of sodium chloride to mix uniformly to obtain an aqueous suspension;

[0054] S5. 9 mg fluopicolide and 0.2 g polylactic acid were added into 10 mL dichloromethane, mixed uniformly, and then the oil phase was added into the water phase suspension, and ultrasonic treatment was performed at 2 °C for 12 min, and then the mixture was placed in a fume hood and stirred at a speed of 430 rpm for 23 h, centrifuged, washed with deionized water, and freeze-dried to obtain fluopicolide microspheres, and 6.5 g fluopicolide and 14 g fluopicolide microspheres were mixed to obtain a fluopicolide composition;

[0055] S6. 12.5 g of the insecticidal adjuvant A, 0.3 g of the insecticidal adjuvant B, and 4.5 g of the insecticidal adjuvant C were mixed to obtain an insecticidal adjuvant, and 20 g of imidacloprid, 8 g of abamectin, and 6.3 g of thiamethoxam were mixed uniformly to obtain an insecticidal active substance;

[0056] S7. 9 g of the phosphate ester dispersant 1015 and 14.5 g of calcium dodecylbenzenesulfonate were added into 520 g of deionized water, stirred at a speed of 330 rpm for 12 min, and then 40.2 g of the fluopicolide composition and 17.7 g of the insecticidal active substance were added and stirred for 35 min, and then 5.5 g of the insecticidal adjuvant and 1.3 g of the silicone defoamer HY1572 were added and mixed uniformly to obtain a fluopicolide-based composite insecticide.

[0057] Example 3: A preparation method of a fluopicolide-based composite insecticide, comprising the following steps:

[0058] S1. 3 g of beef extract, 10 g of peptone, and 5 g of NaCl were added into 1000 mL of distilled water, heated at 45 °C until completely dissolved, the pH was adjusted to 7, and then filtered and autoclaved at 121 °C for 15 min to obtain a NA liquid medium; 10 g of beef extract, 20 g of peptone, and 5 g of NaCl were added into 1000 mL of distilled water, heated at 45 °C until completely dissolved, and then autoclaved at 121 °C for 20 min to obtain a beef extract peptone medium;

[0059] S2. The activated Bacillus megaterium was inoculated into the beef extract peptone liquid medium, and cultured at 28 °C and 140 rpm for 3 d, and then the fermentation broth was centrifuged at 8000 rpm for 10 min, the bacterial cells were collected, and then a bacterial suspension was prepared with sterile water to obtain a Bacillus megaterium bacterial suspension; the Bacillus subtilis was inoculated into the NA liquid medium, and cultured at 28 °C and 180 rpm for 1 d, and then the bacterial liquid was centrifuged, the supernatant was removed, the bacterial cells were collected, and then a bacterial suspension was prepared with sterile water to obtain a Bacillus subtilis bacterial suspension, and then 5 g of the Bacillus subtilis bacterial suspension and 3 g of the Bacillus megaterium bacterial suspension were mixed to obtain the insecticidal adjuvant C;

[0060] S3. Mix 6 g of limonene, 6 g of allicin and 15 g of humic acid to obtain an insecticide adjuvant A, and add 0.015 mg of sodium carboxymethyl cellulose in 50 mL of deionized water, stir uniformly, then add 0.85 mg of silicon carbide nanoparticles to obtain an insecticide adjuvant B;

[0061] S4. Disperse 0.06 g of cellulose nanocrystals in 30 mL of deionized water, and add 0.06 g of sodium chloride and mix uniformly to obtain an aqueous phase suspension;

[0062] S5. Add 10 mg of fluopyram and 0.22 g of polylactic acid to 11 mL of dichloromethane, mix uniformly to obtain an oil phase, then add the oil phase to the aqueous phase suspension, ultrasonic treatment for 12 min at 2℃, then place in a fume hood and stir at a speed of 460 rpm for 23 h, centrifugation, deionized water washing, freeze-drying to obtain fluopyram microspheres, and mix 8 g of fluopyram and 15 g of fluopyram microspheres to obtain a fluopyram composition;

[0063] S6. Mix 13.5 g of insecticide adjuvant A, 0.3 g of insecticide adjuvant B and 5 g of insecticide adjuvant C to obtain an insecticide adjuvant, and mix 21.5 g of imidacloprid, 9.4 g of abamectin and 7.1 g of thiamethoxam uniformly to obtain an insecticide active substance;

[0064] S7. Add 10.4 g of sodium dodecyl sulfate and 15.4 g of Tween 60 to 580 g of deionized water, stir at a speed of 350 rpm for 12 min, then add 44.2 g of fluopyram composition and 19.8 g of insecticide active substance and stir for 40 min, then add 6.5 g of insecticide adjuvant and 1.5 g of silicone defoamer HY1572, and mix uniformly to obtain a fluopyram-based composite insecticide.

[0065] Example 4: A preparation method of a fluopyram-based composite insecticide, comprising the following steps:

[0066] S1. Weigh 3 g of beef extract, 10 g of peptone and 5 g of NaCl, add 1000 mL of distilled water and heat to complete dissolution at 47℃, adjust the pH to 7, filter and sterilize at 121℃ for 15 min to obtain a NA liquid medium; weigh 10 g of beef extract, 20 g of peptone and 5 g of NaCl, add 1000 mL of distilled water and heat to complete dissolution at 47℃, and sterilize at 121℃ for 20 min to obtain a rich beef extract peptone culture medium;

[0067] S2. The activated Bacillus megaterium is inoculated into beef extract proteose peptone liquid medium and cultured at 28°C with 140 rpm shaking for 3 days. After centrifugation of the fermentation broth at 8000 rpm for 10 min, the bacterial cells are collected and suspended in sterile water to obtain a Bacillus megaterium bacterial suspension. The Bacillus subtilis is inoculated into NA liquid medium and cultured at 28°C with 180 rpm shaking for 1 day. After centrifugation of the bacterial broth, the supernatant is removed, the bacterial cells are collected, and suspended in sterile water to obtain a Bacillus subtilis bacterial suspension. Then 6 g of the Bacillus subtilis bacterial suspension and 4 g of the Bacillus megaterium bacterial suspension are mixed to obtain the insecticidal adjuvant C;

[0068] S3. 6 g of limonene, 6 g of garlicin, and 17 g of humic acid are mixed to obtain the insecticidal adjuvant A. 0.017 mg of sodium carboxymethyl cellulose is added to 55 mL of deionized water, stirred uniformly, and then 0.9 mg of silicon carbide nanoparticles is added to obtain the insecticidal adjuvant B.

[0069] S4. 0.07 g of cellulose nanocrystals is dispersed in 35 mL of deionized water, and 0.07 g of sodium chloride is added and mixed uniformly to obtain an aqueous phase suspension.

[0070] S5. 12 mg of fluopyram and 0.24 g of polylactic acid are added to 13 mL of dichloromethane, mixed uniformly to obtain an oil phase, which is then added to the aqueous phase suspension, ultrasonically treated at 4°C for 13 min, and then stirred at a speed of 520 rpm in a fume hood for 24 h, centrifuged, washed with deionized water, and freeze-dried to obtain fluopyram microspheres. Then 8.5 g of fluopyram and 16 g of fluopyram microspheres are mixed to obtain a fluopyram composition.

[0071] S6. 14.3 g of the insecticidal adjuvant A, 0.4 g of the insecticidal adjuvant B, and 5.5 g of the insecticidal adjuvant C are mixed to obtain an insecticidal adjuvant. 22.8 g of imidacloprid, 10.5 g of abamectin, and 7.5 g of thiamethoxam are mixed uniformly to obtain an insecticidal active substance.

[0072] S7. 10.3 g of phosphate ester dispersant 1015 and 16.3 g of pesticide emulsifier 2201 are added to 610 g of deionized water, stirred at a speed of 370 rpm for 15 min, and then 44.8 g of the fluopyram composition and 24.1 g of the insecticidal active substance are added and stirred for 45 min. Then 7.5 g of the insecticidal adjuvant and 1.7 g of the silicone defoamer HY1572 are added and mixed uniformly to obtain a fluopyram-based composite insecticide.

[0073] Example 5: A preparation method of a fluopyram-based composite insecticide, comprising the following steps:

[0074] S1. Take beef extract 3 g, proteose peptone 10 g, NaCl 5 g, add 1000 mL of distilled water, heat to complete dissolution at 50°C, adjust pH to 7, filter, and sterilize at 121°C for 15 min to obtain a NA liquid medium; take beef extract 10 g, proteose peptone 20 g, NaCl 5 g, add 1000 mL of distilled water, heat to complete dissolution at 50°C, and sterilize at 121°C for 20 min to obtain a beef extract proteose peptone medium;

[0075] S2. The activated Bacillus megaterium is inoculated into the beef extract proteose peptone liquid medium, and cultured at 28°C and 140 rpm for 3 days. After centrifugation of the fermentation broth at 8000 rpm for 10 min, the bacterial cells are collected and suspended in sterile water to obtain a Bacillus megaterium bacterial suspension. The Bacillus subtilis is inoculated into the NA liquid medium, and cultured at 28°C and 180 rpm for 1 day. After centrifugation of the bacterial liquid, the supernatant is removed, the bacterial cells are collected, and suspended in sterile water to obtain a Bacillus subtilis bacterial suspension. Then 7 g of the Bacillus subtilis bacterial suspension and 5 g of the Bacillus megaterium bacterial suspension are mixed to obtain an insecticidal adjuvant C;

[0076] S3. 7 g of limonene, 7 g of garlicin, and 19 g of humic acid are mixed to obtain an insecticidal adjuvant A. 0.02 mg of sodium carboxymethyl cellulose is added to 60 mL of deionized water, stirred uniformly, and then 1 mg of silicon carbide nanoparticles is added to obtain an insecticidal adjuvant B;

[0077] S4. 0.08 g of cellulose nanocrystals is dispersed in 40 mL of deionized water, and 0.08 g of sodium chloride is added and mixed uniformly to obtain an aqueous phase suspension;

[0078] S5. 13 mg of fluopyram and 0.25 g of polylactic acid are added to 15 mL of dichloromethane, mixed uniformly to obtain an oil phase, which is then added to the aqueous phase suspension, ultrasonically treated at 4°C for 15 min, stirred in a fume hood at a speed of 550 rpm for 24 h, centrifuged, washed with deionized water, and freeze-dried to obtain fluopyram microspheres. Then 9 g of fluopyram and 17 g of fluopyram microspheres are mixed to obtain a fluopyram composition;

[0079] S6. 15 g of the insecticidal adjuvant A, 0.5 g of the insecticidal adjuvant B, and 6 g of the insecticidal adjuvant C are mixed to obtain an insecticidal adjuvant. 24 g of imidacloprid, 11.3 g of abamectin, and 8.5 g of thiamethoxam are mixed uniformly to obtain an insecticidal active substance;

[0080] S7. To 650 g of deionized water, 11.3 g of sodium dodecyl benzene sulfonate and 17 g of pesticide emulsifier 2201 were added, stirred at 400 rpm for 15 min, then 49 g of fluopyram composition and 26.7 g of insecticidal active were added and stirred for 50 min, then 8.2 g of insecticidal adjuvant and 2 g of silicone defoamer 1572 were added, and mixed uniformly to obtain a fluopyram-based composite insecticide.

[0081] Comparative Example 1:

[0082] This comparative example is compared with Example 1 without adding fluopyram microspheres in the preparation process of fluopyram composition, and the rest of the steps and parameters are the same. This comparative example will not be repeated here. Finally, a composite insecticide is obtained.

[0083] Comparative Example 2:

[0084] This comparative example is compared with Example 1 without adding fluopyram in the preparation process of fluopyram composition, and the rest of the steps and parameters are the same. This comparative example will not be repeated here. Finally, a composite insecticide is obtained.

[0085] Comparative Example 3:

[0086] This comparative example is compared with Example 1 without adding insecticidal active in the preparation process of composite insecticide, and the rest of the steps and parameters are the same. This comparative example will not be repeated here. Finally, a composite insecticide is obtained.

[0087] Comparative Example 4:

[0088] This comparative example is compared with Example 1 without adding insecticidal adjuvant in the preparation process of composite insecticide, and the rest of the steps and parameters are the same. This comparative example will not be repeated here. Finally, a composite insecticide is obtained.

[0089] Comparative Example 5:

[0090] This comparative example is compared with Example 1 only by replacing "insecticidal adjuvant" with "insecticidal adjuvant A", and the rest of the steps and parameters are the same. This comparative example will not be repeated here. Finally, a composite insecticide is obtained.

[0091] Comparative Example 6:

[0092] This comparative example is compared with Example 1 only by replacing "insecticidal adjuvant" with "insecticidal adjuvant B", and the rest of the steps and parameters are the same. This comparative example will not be repeated here. Finally, a composite insecticide is obtained.

[0093] Comparative Example 7:

[0094] This comparative example is compared with Example 1 only by replacing "insecticidal adjuvant" with "insecticidal adjuvant C", and the rest of the steps and parameters are the same. This comparative example will not be repeated here. Finally, a composite insecticide is obtained.

[0095] Comparative Example 8

[0096] S1. Take beef extract 3 g, proteose peptone 10 g, NaCl 5 g, add 1000 mL of distilled water, heat to complete dissolution at 40°C, adjust pH to 7, filter, and sterilize at 121°C for 15 min to obtain a NA liquid medium; take beef extract 10 g, proteose peptone 20 g, NaCl 5 g, add 1000 mL of distilled water, heat to complete dissolution at 40°C, and sterilize at 121°C for 20 min to obtain a beef extract proteose peptone medium;

[0097] S2. Inoculate the activated Bacillus megaterium into the beef extract proteose peptone liquid medium, and shake culture at 28°C and 140 rpm for 3 d; centrifuge the fermentation broth at 8000 rpm for 10 min, collect the bacterial cells, and configure a bacterial suspension with sterile water to obtain a Bacillus megaterium bacterial suspension; inoculate Bacillus subtilis into the NA liquid medium, shake culture at 28°C and 180 rpm for 1 d, centrifuge the bacterial liquid, remove the supernatant, collect the bacterial cells, and configure a bacterial suspension with sterile water to obtain a Bacillus subtilis bacterial suspension; mix 3 g of the Bacillus subtilis bacterial suspension and 2 g of the Bacillus megaterium bacterial suspension to obtain an insecticidal adjuvant C;

[0098] S3. Mix 4 g of limonene, 4 g of garlicin, and 13 g of humic acid to obtain an insecticidal adjuvant A, add 0.01 mg of sodium carboxymethyl cellulose to 40 mL of deionized water, stir uniformly, and add 0.75 mg of silicon carbide nanoparticles to obtain an insecticidal adjuvant B;

[0099] S4. Disperse 0.04 g of cellulose nanocrystals in 20 mL of deionized water, and add 0.04 g of sodium chloride to mix uniformly to obtain an aqueous phase suspension;

[0100] S5. Add 8 mg of fluopyram and 0.18 g of polylactic acid to 9 mL of dichloromethane, mix uniformly to obtain an oil phase, add the oil phase to the aqueous phase suspension, and spray dry to obtain fluopyram microspheres; mix 6 g of fluopyram and 13 g of fluopyram microspheres to obtain a fluopyram composition;

[0101] S6. Mix 11.5 g of the insecticidal adjuvant A, 0.2 g of the insecticidal adjuvant B, and 4 g of the insecticidal adjuvant C to obtain an insecticidal adjuvant; mix 18.6 g of imidacloprid, 7 g of abamectin, and 5.3 g of thiamethoxam uniformly to obtain an insecticidal active substance;

[0102] S7. To 480 g of deionized water, 8 g of phosphate ester dispersant 1015 and 13.5 g of calcium dodecylbenzenesulfonate were added, stirred at 300 rpm for 10 min, then 37.2 g of fluopyram composition and 15.5 g of insecticidal active were added and stirred for 30 min, then 4.5 g of insecticidal adjuvant and 1 g of silicone antifoaming agent HY1572 were added, and mixed uniformly to obtain a fluopyram-based composite insecticide.

[0103] Comparative Example 9:

[0104] This comparative example is compared with Example 1 only by replacing "6 g of fluopyram and 13 g of fluopyram microspheres" with "6 g of fluopyram and 30 g of fluopyram microspheres", and the rest of the steps and parameters are the same. This comparative example will not be repeated here. Finally, a composite insecticide is obtained.

[0105] Comparative Example 10:

[0106] This comparative example is compared with Example 1 only by replacing "6 g of fluopyram and 13 g of fluopyram microspheres" with "15 g of fluopyram and 3 g of fluopyram microspheres", and the rest of the steps and parameters are the same. This comparative example will not be repeated here. Finally, a composite insecticide is obtained.

[0107] Comparative Example 11:

[0108] This comparative example is compared with Example 1 only by replacing "11.5 g of insecticidal adjuvant A, 0.2 g of insecticidal adjuvant B, and 4 g of insecticidal adjuvant C" with "11.5 g of insecticidal adjuvant A, 2 g of insecticidal adjuvant B, and 4 g of insecticidal adjuvant C", and the rest of the steps and parameters are the same. This comparative example will not be repeated here. Finally, a composite insecticide is obtained.

[0109] Performance test:

[0110] 1. The control effect on cowpea seedlings:

[0111] A piece of cowpea seedling planting land was evenly divided into 16 groups, and the composite insecticides prepared in Examples 1-5 and Comparative Examples 1-11 were evenly applied to the soil. Each hole was applied before the cowpea seedlings were planted, and the crops were planted after half an hour. When the cowpea seedlings were in the bud stage, the composite insecticides prepared in Examples 1-5 and Comparative Examples 1-11 were diluted with water at a ratio of 100 g to 10 kg of water, and the control effect on nematodes (10 d, 30 d), yield increase, and safety of each group of composite insecticides were recorded.

[0112] 2. The control effect on peanuts:

[0113] Each of the 16 groups of Example 1-Example 5 and Comparative Example 1-Comparative Example 11 took 100 peanut seeds to measure the germination rate, indoor germination rate (%) = germinated seeds / total number of treated seeds x 100%; whether there was phytotoxicity from emergence to the end of the growth period was observed; at 3-4 leaf stage after seedling emergence, the investigation of underground pests was carried out, and the number of seedlings injured or killed by peanut root-knot nematodes and grubs was recorded as the number of insect-damaged seedlings, the insect control effect was calculated, and the insect-damaged seedling rate (%) = the number of insect-damaged seedlings / the total number of investigated plants x 100%,

[0114] The insect control effect (%) = (the insect-damaged seedling rate in the control area - the insect-damaged seedling rate in the treatment area) / the insect-damaged seedling rate in the control area x 100%. The control area used clean water. The composite insecticide of the examples and comparative examples was treated at 20 g / mu of active ingredient, and the control was not treated, and 100 peanut seeds were taken from each group to test the germination rate;

[0115] The experimental area was 66.7 m 2 , repeated 3 times; the investigation method of the control effect after application was that 5 points were randomly sampled in the experimental treatment area, the number of insect-damaged seedlings was investigated according to the national field test related standards, and the control effect was calculated.

[0116] Disease index = x 100

[0117] Control effect (%) = x 100

[0118] Table 1 Summary of experimental data in Example 1-Example 5 and Comparative Example 1-Comparative Example 11

[0119]

[0120] Table 2 Summary of experimental data in Example 1-Example 5 and Comparative Example 1-Comparative Example 11

[0121]

[0122] Data analysis:

[0123] As can be seen from Table 1 and Table 2, the composite insecticide prepared in the application has better insecticidal effect and utilization, which may be because flupyradifurone has low solubility in water, poor thermal stability and light stability, and low bioavailability, and in the application, polylactic acid with high thermal stability and biodegradability and cellulose nanocrystals with emulsifying capacity are used to load flupyradifurone, so that flupyradifurone microspheres with high light and thermal stability, high utilization and slow release performance are obtained, and the flupyradifurone microspheres are mixed with flupyradifurone, so that the flupyradifurone composition can not only kill insects quickly, but also continuously exert insecticidal effect; in the insecticidal adjuvant, the insecticidal adjuvant A can enhance soil organic matter and promote the reproduction of nematode antagonistic microorganisms, and also has a small amount of irritating odor, accelerates the death of nematodes and inhibits the hatching of nematode eggs; the insecticidal adjuvant B is absorbed into the body of nematodes, and then affects the survival of nematode larvae; the insecticidal adjuvant C has a significant control effect on nematodes, and is mixed with the insecticidal adjuvant A and the insecticidal adjuvant B to control nematodes from multiple dimensions, so that the insecticidal effect is significantly improved; in Comparative Example 8, flupyradifurone microspheres are prepared by a spray drying method, finally resulting in poor control effect on nematodes and yield-increasing effect, which is because flupyradifurone has poor light and thermal stability, and the spray drying needs high temperature, which greatly affects the stability of flupyradifurone, and then affects the insecticidal effect; in Comparative Example 11, the mass fraction of the insecticidal adjuvant B in the insecticidal adjuvant is changed, finally resulting in poor control effect on nematodes and yield-increasing effect, which may be because when the amount of silicon carbide nanoparticles is excessive, the silicon carbide nanoparticles can adsorb nutrients in the soil, affect the microbial community structure, destroy the ecological balance of the soil, and be not conducive to the control of nematodes and the growth of crops.

[0124] It should be understood by those of ordinary skill in the art that the discussion of any of the above examples is merely exemplary and is not intended to suggest that the scope of the application is limited to these examples; under the idea of the application, the technical features in the above examples or different examples can also be combined, the steps can be implemented in any order, and there are many other changes of different aspects of the application as described above, which are not provided in details for the sake of brevity.

[0125] The present application is intended to cover all such changes and modifications that come within the scope of the appended claims and their equivalents. Accordingly, any and all modifications, variations, or equivalents that fall under the spirit and principle of the application fall within the scope of the application.

Claims

1. A fluopyram-based composite insecticide, characterized by, The composition comprises the following ingredients by mass: fluopyram 37.2-49 parts; insecticidal active 15.5-26.7 parts; defoaming agent 1-2 parts; dispersing agent 8-11.3 parts; emulsifier 13.5-17 parts; insecticide adjuvant 4.5-8.2 parts; deionized water 480-650 parts; The insecticide adjuvant is prepared from insecticide adjuvant A, insecticide adjuvant B and insecticide adjuvant C; The fluopyram composition is prepared by mixing fluopyram, fluopyram microspheres in a mass ratio of 6-9:13-17; The fluopyram microspheres are prepared from fluopyram, cellulose nanocrystals and polylactic acid; The insecticide adjuvant A is prepared by mixing limonene, garlicin and humic acid in a mass ratio of 4-7:4-7:13-19; The insecticide adjuvant B is a suspension of silicon carbide nanoparticles; The insecticide adjuvant C is prepared from Bacillus subtilis and Bacillus megaterium; The preparation method of the silicon carbide nanoparticle suspension is as follows: Carboxymethyl cellulose sodium is added to deionized water, stirred uniformly, and then silicon carbide nanoparticles are added to obtain a silicon carbide nanoparticle suspension; The amount ratio of the deionized water, carboxymethyl cellulose sodium and silicon carbide nanoparticles is 40-60 mL:0.01-0.02 mg:0.75-1 mg; The particle size of the silicon carbide nanoparticles is 50-60 nm; The mass ratio of the insecticide adjuvant A, insecticide adjuvant B and insecticide adjuvant C in the insecticide adjuvant is 11.5-15:0.2-0.5:4-6; The preparation method of the fluopyram microspheres is as follows: Step A1. Disperse cellulose nanocrystals in deionized water, add sodium chloride and mix uniformly to obtain an aqueous phase suspension; Step A2. Add fluopyram and polylactic acid to dichloromethane, mix uniformly to obtain an oil phase, then add the oil phase to the aqueous phase suspension, ultrasonic treat at 0-4℃ for 10-15 min, then place in a fume hood and stir at a speed of 400-550 rpm for 22-24 h, centrifuge, deionized water wash, freeze-dry to obtain fluopyram microspheres; The insecticidal active is prepared by mixing imidacloprid, abamectin and thiamethoxam in a mass ratio of 18.6-24:7-11.3:5.3-8.5; The amount ratio of the cellulose nanocrystals, deionized water and sodium chloride in step A1 is 0.04-0.08 g:20-40 mL:0.04-0.08 g; The amount ratio of the fluopyram, polylactic acid and dichloromethane in step A2 is 8-13 mg:0.18-0.25 g:9-15 mL; The defoaming agent is silicone defoamer HY1572; The dispersing agent is at least one of phosphate ester dispersing agent 1015, sodium dodecyl benzene sulfonate and sodium dodecyl sulfate; The emulsifier is at least one of Tween 60, calcium dodecyl benzene sulfonate and pesticide emulsifier 2201; The Bacillus subtilis and Bacillus megaterium are in the form of Bacillus subtilis bacterial suspension and Bacillus megaterium bacterial suspension to constitute the insecticide adjuvant C; The mass ratio of the Bacillus subtilis bacterial suspension and the Bacillus megaterium bacterial suspension is 3-7:2-5; The viable cell number of Bacillus subtilis in the insecticidal adjuvant C is 4 x 10 8 CFU / mL, and the viable cell number of Bacillus megaterium is 2 x 10 10 CFU / mL. 7 CFU / mL. 9 CFU / mL.

2. The preparation method of the fluopyram-based composite insecticide according to claim 1, characterized in that, The method comprises the following steps: Step S1. mixing the pesticide adjuvant B with the pesticide adjuvant A and the pesticide adjuvant C to obtain a pesticide adjuvant; Step S2. adding the dispersant and the emulsifier into the deionized water, stirring at a rotation speed of 300-400 rpm for 10-15 min, then adding the fluopyram composition and the pesticide active substance, stirring for 30-50 min, and then adding the pesticide adjuvant and the defoaming agent, and uniformly mixing to obtain the fluopyram-based composite pesticide.

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