Synergistic pesticide composition for preventing and treating monochamus alternatus hope as well as preparation method and application thereof

Abstract

The invention belongs to the field of insecticides, and particularly relates to a synergistic pesticide composition for preventing and treating monochamus alternatus hope as well as a preparation method and application of the synergistic pesticide composition. The weight ratio of thiacloprid to cypermethrin in the synergistic pesticide is (0.05-6): 1. The dosage forms of the synergistic pesticide are microemulsion, suspoemulsion, soluble liquid and microcapsule suspension. The effective components of thiacloprid and cypermethrin are combined and matched with a preparation, so that the effective prevention and control of monochamus alternatus hope on pine wood nematode infected wood are improved, the pesticide effect is improved, the pesticide application amount is reduced, and the use cost is reduced.

Description

Technical Field

[0001] The present invention belongs to the field of insecticides, and particularly relates to a synergistic pesticide composition for controlling Monochamus alternatus, a preparation method thereof, and an application thereof. Background Art

[0002] Pine wilt disease, also known as pine wilt, is a devastating pine disease and a quarantine pest that causes the most serious harm to forests in China, seriously threatening the safety of the pine forest ecosystem in China. In China, Monochamus alternatus is the main vector insect of pine wilt disease. Monochamus alternatus carries Bursaphelenchus xylophilus when emerging from diseased trees and spreads it to healthy pine trees during supplementary nutrition and egg-laying. Monochamus alternatus is a stem-boring pest, and the entire larval stage bores and damages inside the tree trunk, with strong concealment, making it very difficult to control. The emergence period of Monochamus alternatus adults is long. After the infected diseased trees are cut down, if disinfection and killing treatment are not carried out in time, it will continue to provide a breeding ground for Monochamus alternatus, exacerbating the reproduction of the insect population and the spread of Bursaphelenchus xylophilus. Therefore, controlling Monochamus alternatus is the key to preventing and controlling pine wilt disease.

[0003] The cleaning of diseased trees is an important measure to ensure the control effect of pine wilt disease and reduce the spread of the disease, and it is a key link in the prevention and control of pine wilt disease. At present, the forestry industry generally takes felling, burning or fumigation treatment for infected and dead pine trees, with high control costs, complex operations, and serious environmental pollution. Burning the infected diseased trees is extremely likely to cause forest fires, with high and uncontrollable risks. A slight mistake in the burning operation may cause huge economic losses. Burning a large number of diseased trees will release a large amount of carbon dioxide (CO2), exacerbating global warming and causing drastic changes in the temperature of the forest environment. The burning of diseased trees harms non-target organisms, seriously damages the forest ecosystem, and reduces biodiversity. The current method of fumigating and disinfecting infected diseased trees, although the fumigant has good chemical stability and high drug efficacy. However, since the fumigants used are all highly toxic agents, strict requirements are imposed on the operation specifications, the operation is highly dangerous, and it will also harm non-target organisms and damage the forest ecosystem.

[0004] Thiacloprid is a neonicotinoid insecticide with a broad insecticidal spectrum and high activity, and is particularly effective against piercing-sucking mouthpart pests, chewing mouthpart pests, and Lepidoptera pests. Thiacloprid has diverse action pathways, with good stomach toxicity, contact activity, and strong systemic conductivity and permeability. With the prominent problem of insecticide resistance, using a single agent can no longer achieve the best drug effect. Cypermethrin, as a pyrethroid insecticide, has significant characteristics such as high activity, broad insecticidal spectrum, and low toxicity to mammals and birds. By mixing thiacloprid with a pyrethroid insecticide, the drug efficacy can be further enhanced, and at the same time, the generation of resistance can be avoided. There is no relevant report in the prior art on combining thiacloprid and cypermethrin for controlling Monochamus alternatus. Summary of the Invention

[0005] The present invention has developed a highly efficient and well-conductive mixed pesticide, and its application method is to directly spray it on the surface of felled diseased wood. Its application method is unique, which solves the problem that the diseased wood becomes a potential breeding place and nutrient source for Monochamus alternatus when it is stored in the outdoor forest area. The present invention provides the following technical solutions:

[0006] A synergistic pesticide composition for controlling Monochamus alternatus, wherein the weight ratio of thiacloprid to cypermethrin is (0.05 - 6):1; preferably, the weight ratio of thiacloprid to cypermethrin is (0.1 - 5):1; more preferably, the weight ratio of thiacloprid to cypermethrin is 1:3 - 3:1.

[0007] The present invention provides a microemulsion containing thiacloprid and cypermethrin. The preparation raw materials include, by weight percentage:

[0008] 5% thiacloprid technical material, 15% cypermethrin technical material, 10% block polyether, 5% ethanol, 10% propylene glycol, 15% lauroyl amide, 10% cyclohexanone, and the balance is made up to 100% with water.

[0009] 20% thiacloprid technical material, 5% cypermethrin technical material, 12% block polyether, 5% ethanol, 5% propylene glycol, 20% lauroyl amide, 5% cyclohexanone, and the balance is made up to 100% with water.

[0010] 10% thiacloprid technical material, 10% cypermethrin technical material, 15% block polyether, 3% ethanol, 10% propylene glycol, 10% lauroyl amide, 5% cyclohexanone, and the balance is made up to 100% with water.

[0011] The preparation method of the microemulsion containing the composition of thiacloprid and cypermethrin includes the following steps: First, add the solvent, co-solvent, thiacloprid, cypermethrin and penetrant into the reaction kettle, and stir at a speed of 2000 r / min for 10 min. After the solution becomes clear and transparent, add the emulsifier and water, and stir at a speed of 2000 r / min for 30 min to obtain the thiacloprid·cypermethrin microemulsion composition.

[0012] The present invention provides a suspo-emulsion containing thiacloprid and cypermethrin. The preparation raw materials include, by weight percentage:

[0013] 5% thiacloprid technical material, 15% cypermethrin technical material, 3% carboxylate complex, 3% phosphonate wetting agent, 3% block polyether, 0.2% xanthan gum, 0.2% Kathon, 0.3% silicone defoamer, 5% ethylene glycol, 0.5% magnesium aluminum silicate, 1% white carbon black, 10% solvent oil No. 1500, and the balance is made up to 100% with deionized water.

[0014] 10% thiacloprid technical, 10% cypermethrin technical, 5% carboxylate complex, 3% phosphonate wetting agent, 5% block polyether, 0.2% xanthan gum, 0.2% Kathon, 0.3% silicone defoamer, 5% ethylene glycol, 0.5% magnesium aluminum silicate, 1% white carbon black, 10% solvent oil No. 1500, deionized water to make up 100%.

[0015] 2% thiacloprid technical, 20% cypermethrin technical, 6% carboxylate complex, 5% phosphonate wetting agent, 6% block polyether, 0.2% xanthan gum, 0.2% Kathon, 0.3% silicone defoamer, 5% ethylene glycol, 0.5% magnesium aluminum silicate, 1% white carbon black, 15% solvent oil No. 1500, deionized water to make up 100%.

[0016] The preparation method of the suspoemulsion containing the composition of thiacloprid and cypermethrin includes the following steps: First, inject solvent oil No. 1500 into the reaction kettle, add cypermethrin technical and start stirring at the same time. After the technical is completely dissolved, add block polyether. After complete dissolution, slowly add deionized water and start shearing at the same time. Shear for 30 minutes to obtain the cypermethrin aqueous emulsion for standby. Then, add the dispersant, anti-settling agent, antioxidant, wetting agent, defoamer, preservative, antifreeze and water into another shearing kettle. After shearing for 10 minutes, add thiacloprid technical, stir and shear for 10 minutes, and then grind in a sand mill for 2 hours. Stop grinding when the particle diameter is below 5 μm. After passing the inspection, add the cypermethrin aqueous emulsion and thiacloprid suspension in proportion in another reaction kettle, mix the aqueous emulsion and suspension prepared in this example, and stir at 2000 r / min for 30 minutes to obtain the suspoemulsion.

[0017] The present invention provides a soluble liquid formulation containing thiacloprid and cypermethrin. The preparation raw materials include, by weight percentage:

[0018] 5% thiacloprid technical, 15% cypermethrin technical, 15% anionic surfactant, 15% anionic-nonionic surfactant, 2% special silicone surfactant, 15% fatty alcohol polyether, 10% decanamide, 5% ethanol, 5% cyclohexanone, 10% propylene glycol, dimethylformamide to make up 100%.

[0019] 10% thiacloprid technical, 10% cypermethrin technical, 8% anionic surfactant, 7% anionic-nonionic surfactant, 1% special silicone surfactant, 18% fatty alcohol polyether, 15% decanamide, 3% ethanol, 5% cyclohexanone, 8% propylene glycol, dimethylformamide to make up 100%.

[0020] 5% thiacloprid technical, 10% cypermethrin technical, 6% anionic surfactant, 5% anionic-nonionic surfactant, 5% special silicone surfactant, 30% fatty alcohol polyether, 12% decanamide, 5% ethanol, 8% cyclohexanone, 4% propylene glycol, and dimethylformamide to make up 100%.

[0021] The preparation method of the soluble liquid formulation containing the thiacloprid and cypermethrin composition includes the following steps: First, pump the solvent and co-solvent into the reaction kettle through the material pump, start the agitator of the reaction kettle, and sequentially add thiacloprid and cypermethrin technical into the feeding port of the reaction kettle. (The cypermethrin technical needs to be heated in a water bath at a temperature controlled at 80°C until the technical becomes liquid.) Stir in the reaction kettle for about 1 hour until it becomes clear. Finally, add the emulsifier and water through the material pump and stir for 1 hour until it becomes clear. After the prepared soluble liquid formulation returns to room temperature, take a sample for testing. After passing the test, the soluble liquid formulation is pumped into the finished product tank.

[0022] The present invention provides a microcapsule suspension containing thiacloprid and cypermethrin. The preparation raw materials include, by weight percentage:

[0023] 2.5% thiacloprid technical, 5% cypermethrin technical, 25% xylene, 2% DM2601, 2% D8969, 0.2% defoamer, 4% ethylene glycol, 0.3% WM2501, 3% 8532CS, 0.2% cason, 0.1% xanthan gum, and water to make up 100%.

[0024] 5% thiacloprid technical, 10% cypermethrin technical, 20% xylene, 2% DM2601, 2% D8969, 0.2% defoamer, 4% ethylene glycol, 0.3% WM2501, 3% 8532CS, 0.2% cason, 0.1% xanthan gum, and water to make up 100%.

[0025] 10% thiacloprid technical, 2% cypermethrin technical, 30% xylene, 2% DM2601, 2% D8969, 0.2% defoamer, 4% ethylene glycol, 0.3% WM2501, 3% 8532CS, 0.2% cason, 0.1% xanthan gum, and water to make up 100%.

[0026] The preparation method of the microcapsule agent containing the thiacloprid and cypermethrin composition includes the following steps: Prepare the materials for formulating the microcapsule suspension. Preparation of the oil phase: Add the solvent to the oil phase kettle, add the original drugs of thiacloprid and cypermethrin to the material port, turn on the heating device of the oil phase kettle, set the heating temperature to 60 °C, turn on the stirrer for about 15 minutes until the solution is clear, add the oil phase wall material, and stir for about 10 minutes until clear. Preparation of the water phase: Add water, defoamer, and dispersant to the water phase kettle and stir for 15 minutes. Turn on the shearing machine, slowly add the oil phase to the water phase, continue shearing for 15 minutes, shear the particle size to the appropriate range, and then turn off the shearing machine. Turn on the stirrer, slowly add the water phase wall material, after the dropping is completed, react for 10 minutes, then add the antifreeze, thickener, preservative, and dispersant and continue stirring for 30 minutes. Wait for the prepared microcapsule suspension to return to room temperature, take samples for testing, and transfer to the finished product tank after passing the test.

[0027] The present invention provides an application of a synergistic pesticide containing a thiacloprid and cypermethrin composition in controlling Monochamus alternatus in the pine wood nematode-infected diseased pine wood.

[0028] Compared with the prior art, the present invention has the following beneficial effects:

[0029] 1. For the microemulsion or suspoemulsion of the pesticide containing the thiacloprid and cypermethrin composition of the present invention, using block polyether as the dispersant can improve the product stability, has good hard water dilution resistance, increases the deposition amount of the pesticide on the target, and improves the pesticide efficacy.

[0030] 2. For the synergistic pesticide containing the thiacloprid and cypermethrin composition of the present invention, the combination of the active ingredients of thiacloprid and cypermethrin improves the effective control of Monochamus alternatus on the pine wood nematode-infected diseased pine wood, improves the pesticide efficacy, reduces the application amount of the pesticide, and reduces the use cost. Description of the Drawings

[0031] Figure 1 Change of the strawberry red water-soluble dye on the wooden strip;

[0032] Figure 2 Absorption situation of the wooden strip after 3 hours;

[0033] Figure 3 Absorption situation after taking out and splitting the wooden strip after 5 hours;

[0034] Figure 4 Wettability experiment situation by the canvas sedimentation method;

[0035] Figure 5 Drilling schematic diagram. Specific Embodiments

[0036] The following further explains the specific embodiments of the present invention in conjunction with specific examples.

[0037] I. Indoor Toxicity Determination

[0038] Test agents: Thiacloprid technical and Cypermethrin technical

[0039] Test method: First, conduct preliminary tests on each test agent. According to the results of the preliminary tests, set 5 concentration gradients for single agents and compound agents respectively. Lay filter paper at the bottom of the plastic insect rearing box, and set up filter paper strips in the box for longhorn beetles to climb on. Introduce adult Monochamus alternatus into the insect rearing box, with 20 in each box. Spray the agents evenly in the box with a sprayer to ensure that the insects are wet, there is no water accumulation in the box, and open the ventilation holes to ensure ventilation of the box. Repeat each treatment 3 times and set a control treatment. Place the insect rearing boxes of each treatment and the control indoors, observe after 48h, record the number of dead insects, and calculate the corrected mortality rate.

[0040] Synergistic evaluation method: Evaluate the combined effect between active ingredients according to the Sun Yunpei method. When CTC < 80, it is antagonistic effect; when CTC > 120, it is synergistic effect; when 80 ≤ CTC ≤ 120, it is additive effect.

[0041] Test results:

[0042] As can be seen from the following table, when thiacloprid and cypermethrin are compounded under appropriate ratio conditions, when the mass ratio of thiacloprid to cypermethrin is 3:1 - 1:3, it has a significant synergistic effect on Monochamus alternatus. When the composition shows a synergistic effect, it can significantly reduce the dosage of active ingredients, reduce environmental pollution, and slow down the generation of pest resistance.

[0043] Table 1-1: Indoor Toxicity Determination

[0044]

[0045]

[0046] II. Formulation Examples

[0047] Example 1: Microemulsion

[0048] A synergistic pesticide microemulsion containing a composition of thiacloprid and cypermethrin, the raw materials include, by weight percentage: 5% thiacloprid technical, 15% cypermethrin technical, 10% block polyether, 5% ethanol, 10% propylene glycol, 15% lauroylamide, 10% cyclohexanone, and water is added to make up 100%.

[0049] Thiacloprid technical is purchased from Limin Chemical Co., Ltd., and the original drug content is 98.4 wt%.

[0050] Cypermethrin technical is purchased from Jiangsu Nongbo Biotechnology Co., Ltd., and the original drug content is 98.4 wt%.

[0051] The block polyether is Ethylan NS-500LQ, purchased from Nanjing Jierun Technology Co., Ltd.

[0052] Ethanol, purchased from Hangzhou Gaojing Fine Chemical Co., Ltd.

[0053] Propylene glycol, purchased from Zhejiang Tengyu New Materials Technology Co., Ltd.

[0054] The lauroyl amide co-solvent, purchased from Shanghai Shennong New Materials Co., Ltd.

[0055] Cyclohexanone, purchased from Hangzhou Xinwanneng Fine Chemical Co., Ltd.

[0056] Preparation method

[0057] When the dosage form of the composition containing thiamethoxam and cypermethrin is a microemulsion, the preparation method is as follows: First, add cyclohexanone, lauroyl amide, ethanol, thiamethoxam, cypermethrin and propylene glycol into the reaction kettle, and stir at a speed of 2000 r / min for 10 min. After the solution is clear and transparent, add the block polyether Ethylan NS-500LQ and water, and stir at a speed of 2000 r / min for 30 min to obtain the thiamethoxam·cypermethrin microemulsion composition.

[0058] Example 2: Microemulsion

[0059] A synergistic pesticide microemulsion containing a composition of thiamethoxam and cypermethrin, the raw materials are in weight percentages including: 20% thiamethoxam technical, 5% cypermethrin technical, 12% block polyether, 5% ethanol, 5% propylene glycol, 20% lauroyl amide, 5% cyclohexanone, and water to make up 100%.

[0060] The raw material sources and preparation methods are the same as above.

[0061] Example 3: Microemulsion

[0062] A synergistic pesticide microemulsion containing a composition of thiamethoxam and cypermethrin, the raw materials are in weight percentages including: 10% thiamethoxam technical, 10% cypermethrin technical, 15% block polyether, 3% ethanol, 10% propylene glycol, 10% lauroyl amide, 5% cyclohexanone, and water to make up 100%.

[0063] The raw material sources and preparation methods are the same as above.

[0064] Example 4: Suspo-emulsion

[0065] A synergistic pesticide suspo-emulsion containing a composition of thiacloprid and cypermethrin, the raw materials include, by weight percentage: 5% thiacloprid technical, 15% cypermethrin technical, 3% carboxylate complex, 3% phosphonate wetting agent, 3% block polyether, 0.2% xanthan gum, 0.2% Kathon, 0.3% silicone defoamer, 5% ethylene glycol, 0.5% magnesium aluminum silicate, 1% silica white, 10% solvent oil No. 1500, and deionized water to make up 100%.

[0066] The thiacloprid technical is purchased from Limin Chemical Co., Ltd., and the content of the technical is 98.4 wt%.

[0067] The cypermethrin technical is purchased from Jiangsu Nongbo Biotechnology Co., Ltd., and the content of the technical is 98.4 wt%.

[0068] The carboxylate complex SP-2836 is purchased from Jiangsu Qingyu Chemical Technology Co., Ltd.

[0069] The phosphonate JR-P wetting agent is purchased from Nanjing Jierun Technology Co., Ltd.

[0070] The block polyether Ethylan NS-500LQ is purchased from Nanjing Jierun Technology Co., Ltd.

[0071] The xanthan gum is purchased from Hangzhou Haishuo Trading Co., Ltd.

[0072] The Kathon is purchased from Hangzhou Haishuo Trading Co., Ltd.

[0073] The silicone defoamer 1522 is purchased from Nanjing Jierun Technology Co., Ltd.

[0074] The ethylene glycol is purchased from Ningbo Zhenhai Lingang Chemical Industry Co., Ltd.

[0075] The magnesium aluminum silicate is purchased from Anji Chengnong Bentonite Co., Ltd.

[0076] The silica white is purchased from Fujian Jiaxiang Silicon Industry Co., Ltd.

[0077] The solvent oil No. 1500 is purchased from Deqing Yuansheng Oil Chemical Factory

[0078] Example 5: Suspo-emulsion

[0079] A synergistic pesticide suspo-emulsion containing a composition of thiacloprid and cypermethrin, the raw materials include, by weight percentage: 10% thiacloprid technical, 10% cypermethrin technical, 5% carboxylate complex, 3% phosphonate wetting agent, 5% block polyether, 0.2% xanthan gum, 0.2% Kathon, 0.3% silicone defoamer, 5% ethylene glycol, 0.5% magnesium aluminum silicate, 1% silica white, and deionized water to make up 100%.

[0080] The sources of raw materials and the preparation method are the same as above.

[0081] Example 6: Suspension concentrate

[0082] A synergistic pesticidal suspension concentrate containing a composition of thiacloprid and cypermethrin, the raw materials in weight percentages include: 2% thiacloprid technical, 20% cypermethrin technical, 6% carboxylate complex, 5% phosphonate wetting agent, 6% block polyether, 0.2% xanthan gum, 0.2% Kathon, 0.3% silicone defoamer, 5% ethylene glycol, 0.5% magnesium aluminum silicate, 1% silica white, deionized water to make up 100%.

[0083] The sources of raw materials and the preparation method are the same as above.

[0084] Example 7: Soluble concentrate

[0085] A synergistic pesticidal soluble concentrate containing a composition of thiacloprid and cypermethrin, the raw materials in weight percentages include: 5% thiacloprid technical, 15% cypermethrin technical, 15% anionic surfactant SC3, 15% anionic-nonionic surfactant SC29, 2% silicone surfactant, 15% fatty alcohol polyether, 10% lauroylamide, 5% ethanol, 5% cyclohexanone, 10% propylene glycol, dimethylformamide to make up 100%.

[0086] Thiacloprid technical is purchased from Limin Chemical Co., Ltd., and the technical content is 98.4 wt%.

[0087] Cypermethrin technical is purchased from Jiangsu Nongbo Biotechnology Co., Ltd., and the technical content is 98.4 wt%.

[0088] Anionic surfactant SC3 is purchased from Jiangsu Qingyu Chemical Technology Co., Ltd.

[0089] Anionic-nonionic surfactant SC29 is purchased from Jiangsu Qingyu Chemical Technology Co., Ltd.

[0090] Silicone surfactant 302 is purchased from Jiangsu Kaiyuan Technology Co., Ltd.

[0091] Fatty alcohol polyether 3060 is purchased from Jiangsu Qingyu Chemical Technology Co., Ltd.

[0092] Lauroylamide co-solvent is purchased from Shanghai Shennong New Materials Co., Ltd.

[0093] Ethanol is purchased from Hangzhou Gaojing Fine Chemical Co., Ltd.

[0094] Cyclohexanone is purchased from Hangzhou Xinwanneng Fine Chemical Co., Ltd.

[0095] Propylene glycol is purchased from Zhejiang Tengyu New Material Technology Co., Ltd.

[0096] Dimethylformamide, purchased from Zhejiang Tengyu New Material Technology Co., Ltd.

[0097] A preparation method of a soluble concentrate containing thiacloprid and cypermethrin composition, comprising the following steps: First, capramide, ethanol, cyclohexanone, propylene glycol, and dimethylformamide are pumped into a reaction kettle through a material pump. The stirrer of the reaction kettle is started, and thiacloprid and cypermethrin technical are sequentially added into the feeding port of the reaction kettle. (The cypermethrin technical needs to be heated in a water bath, and the temperature of the water bath is controlled at 80 °C until the technical becomes liquid.) Stir in the reaction kettle for about 1 hour until it is clear. Finally, an anionic surfactant SC3, an anionic-nonionic surfactant sc29, a fatty alcohol polyether 3060, and an organosilicon 302 surfactant, and water are added through a material pump, and stirred for 1 hour until it is clear. After the prepared soluble concentrate returns to room temperature, a sample is taken for testing. After passing the test, the soluble concentrate is pumped into a finished product tank.

[0098] Example 8: Soluble concentrate

[0099] An enhanced-efficiency pesticidal soluble concentrate containing thiacloprid and cypermethrin composition, the raw materials are in weight percentages: 10% thiacloprid technical, 10% cypermethrin technical, 8% anionic surfactant, 7% anionic-nonionic surfactant, 1% special organosilicon surfactant, 18% special fatty alcohol polyether, 15% capramide, 3% ethanol, 5% cyclohexanone, 8% propylene glycol, and dimethylformamide to make up 100%.

[0100] The raw material sources and preparation methods are the same as above.

[0101] Example 9: Soluble concentrate

[0102] An enhanced-efficiency pesticidal soluble concentrate containing thiacloprid and cypermethrin composition, the raw materials are in weight percentages: 5% thiacloprid technical, 10% cypermethrin technical, 6% anionic surfactant, 5% anionic-nonionic surfactant, 5% special organosilicon surfactant, 30% special fatty alcohol polyether, 12% capramide, 5% ethanol, 8% cyclohexanone, 4% propylene glycol, and dimethylformamide to make up 100%.

[0103] The raw material sources and preparation methods are the same as above.

[0104] Example 10: Microcapsule suspension

[0105] An enhanced-efficiency pesticidal microcapsule containing thiacloprid and cypermethrin composition, the raw materials are in weight percentages: 2.5% thiacloprid technical, 5% cypermethrin technical, 25% xylene, 2% DM2601, 2% D8969, 0.2% defoamer, 4% ethylene glycol, 0.3% WM2501, 3% 8532CS, 0.2% Kathon, 0.1% xanthan gum, and 55.7% water.

[0106] The thiacloprid technical material was purchased from Limin Chemical Co., Ltd., and the content of the technical material was 98.4 wt%.

[0107] The cypermethrin technical material was purchased from Jiangsu Nongbo Biotechnology Co., Ltd., and the content of the technical material was 98.4 wt%.

[0108] Xylene was purchased from Ningbo Zhenhai Fluke Chemical Co., Ltd.

[0109] The said DM2601 was purchased from Shanghai Pairun Industrial Technology Co., Ltd.

[0110] The said D8969 was purchased from Shanghai Pairun Industrial Technology Co., Ltd.

[0111] Defoamer 1522 was purchased from Nanjing Jierun Technology Co., Ltd.

[0112] Ethylene glycol was purchased from Ningbo Zhenhai Lingang Chemical Co., Ltd.

[0113] The said WM2501 was purchased from Shanghai Pairun Industrial Technology Co., Ltd.

[0114] The said 8532CS was purchased from Shanghai Pairun Industrial Technology Co., Ltd.

[0115] Kathon was purchased from Hangzhou Haishuo Trading Co., Ltd.

[0116] Xanthan gum was purchased from Hangzhou Haishuo Trading Co., Ltd.

[0117] The preparation method of the microcapsule agent containing the thiacloprid and cypermethrin composition comprises the following steps: Prepare the materials for formulating the microcapsule suspension. Preparation of the oil phase: Add xylene to the oil phase kettle, add the thiacloprid and cypermethrin technical materials to the material inlet, turn on the heating device of the oil phase kettle, set the heating temperature to 60 °C, turn on the stirrer for about 15 minutes until the solution is clear, add the oil phase wall material DM2601, and stir for about 10 minutes until clear. Preparation of the water phase: Add water, defoamer 1522, and dispersant D8969 to the water phase kettle and stir for 15 minutes. Turn on the shearing machine, slowly add the oil phase to the water phase, continue shearing for 15 minutes, and close the shearing machine when the particle size is sheared to the appropriate range. Turn on the stirrer, slowly add the water phase wall material WM2501, after the dropping is completed, react for 10 minutes, then add the antifreeze ethylene glycol, thickener xanthan gum, preservative Kathon, and dispersant 8532CS and continue stirring for 30 minutes. Wait for the prepared microcapsule suspension to return to room temperature, take samples for testing, and transfer to the finished product tank after passing the test.

[0118] Example 11: Microcapsule suspension

[0119] A synergistic pesticide microcapsule containing a thiacloprid and cypermethrin composition, the raw materials include, by weight percentage: 5% thiacloprid technical material, 10% cypermethrin technical material, 20% xylene, 2% DM2601, 2% D8969, 0.2% defoaming agent, 4% ethylene glycol, 0.3% WM2501, 3% 8532CS, 0.2% Kathon, 0.1% xanthan gum, and water to make up 100%.

[0120] The raw material sources and preparation methods are the same as above.

[0121] Example 12: Microcapsule suspension

[0122] A synergistic pesticide microcapsule containing a thiacloprid and cypermethrin composition, the raw materials include, by weight percentage: 10% thiacloprid technical material, 2% cypermethrin technical material, 30% xylene, 2% DM2601, 2% D8969, 0.2% defoaming agent, 4% ethylene glycol, 0.3% WM2501, 3% 8532CS, 0.2% Kathon, 0.1% xanthan gum, and water to make up 100%.

[0123] The raw material sources and preparation methods are the same as above.

[0124] Comparative Example 1: In Example 1, the block polyether Ethylan NS-500LQ was replaced with FTRT 500L1; the other components and dosages remained unchanged.

[0125] Comparative Example 2: In Example 4, the block polyether Ethylan NS-500LQ was replaced with Ethylan 324; the other components and dosages remained unchanged.

[0126] Comparative Example 3: In Example 7, the anionic surfactant SC3 was 30%, and the anionic-nonionic surfactant SC29 was not included; the other components and dosages remained unchanged.

[0127] Comparative Example 4: In Example 7, the anionic-nonionic surfactant SC29 was 30%, and the anionic surfactant SC3 was not included; the other components and dosages remained unchanged.

[0128] II. Formulation performance test

[0129] Physicochemical property test:

[0130] 1.1 Experimental process

[0131] 1.1.1 Select a branch and cut it into five pieces, with a length between 14 - 15 cm and a diameter between 2.9 - 3.1 cm, numbered 1-. Their weights are 60.29 g, 64.16 g, 57.68 g, 87.4 g, and 70.45 g in sequence.

[0132] 1.1.2 Weigh 5 grams of sample 1 into a beaker and dilute it 50 times, denoted as No. 1; weigh 5 grams of sample 2 into a beaker and dilute it 50 times, denoted as No. 2; weigh 5 grams of sample 3 into a beaker and dilute it 50 times, denoted as No. 3; weigh 5 grams of sample 4 into a beaker and dilute it 50 times, denoted as No. 4; weigh 5 grams of sample 5 into a beaker and dilute it 50 times, denoted as No. 5.

[0133] Note: For convenient observation, an equal amount of strawberry red water-soluble dye is added to samples No. 1 - 5.

[0134] 1.1.3 At the same time, put the No. 1 wooden stick into the beaker numbered 1; put the No. 2 wooden stick into the beaker numbered 2; put the No. 3 wooden stick into the beaker numbered 3; put the No. 4 wooden stick into the beaker numbered 4; put the No. 5 wooden stick into the beaker numbered 5 (as Figure 1 ).

[0135] Record the weight of the wooden stick every hour. The results are shown in Table 2 - 1, and the mass change rate of the wooden stick is shown in Table 2 - 2.

[0136] Table 2 - 1 Mass change of the wooden stick

[0137]

[0138] Table 2 - 2 Mass change rate of the wooden stick

[0139]

[0140] It is found that the top of the No. 2 wooden stick already has red dye reaching the top after 3 hours, and its absorption is the fastest as follows Figure 2 . After 5 hours, take out the wooden stick, split it open and observe the absorption situation. The results Figure 3 .

[0141] 1.2 Wettability experiment

[0142] Dilute samples 1 - 6 50 times and conduct a wettability experiment using the canvas sedimentation method (No. 6 is thiamethoxam suspension concentrate). Among them, No. 6 is still floating on the liquid surface after 2 minutes. The test data are shown in Table 2 - 3, Figure 4 .

[0143] Table 2 - 3 Wettability test

[0144]

[0145] III. Formulation performance test

[0146] 1. Indoor residual efficacy performance test of the pesticide microcapsule suspension containing the combination of thiamethoxam and cypermethrin

[0147] Test insect source:

[0148] The Monochamus alternatus Hope was reared indoors in the laboratory all year round, and adults of uniform size were selected for the experiment.

[0149] Test method:

[0150] According to the test results, the best drug efficacy concentration was selected for the indoor residual efficacy test. The prepared liquid medicine was evenly sprayed on the filter paper. Ten male adult longhorn beetles with basically the same emergence time and similar size were selected and placed on the filter paper. After they crawled about 50 cm on the filter paper, they were transferred into a clean acrylic container, and fresh pine branches were added as feed. Each treatment was repeated 3 times, and the blank control was water. The insect rearing container was sealed with a clean gauze. The rearing conditions were: temperature 24 - 26 °C, humidity 70% - 80%, and photoperiod L:D = 14:10. The results were investigated after 24 h, and those that could not crawl normally were regarded as dead insects. The test was repeated according to the above method after 10 d until the knockdown rate of the treatment was lower than 70%, and then the final indoor residual efficacy period was determined.

[0151] Drug treatment:

[0152] 1. The pesticide product formulated in Example 10;

[0153] 2. The pesticide product formulated in Example 11;

[0154] 3. The pesticide product formulated in Example 12;

[0155] 4. 2% thiacloprid (Shandong Tomple Crop Science Co., Ltd.);

[0156] 5. 8% cypermethrin microcapsule suspension (Chongqing Zhongbang Pharmaceutical Co., Ltd.);

[0157] 6. Water control.

[0158] Data statistics:

[0159]

[0160] Test results:

[0161] Analysis of the results of the indoor residual efficacy test of the thiacloprid and cypermethrin combined microcapsule suspension against Monochamus alternatus Hope adults is shown in Table 2 - 4.

[0162] Table 2 - 4 Results of the indoor residual efficacy test of the microcapsule suspension against Monochamus alternatus Hope adults

[0163]

[0164] 2. Forest trial - microemulsion:

[0165] Drug treatment:

[0166] 1. The pesticide product formulated in Example 1;

[0167] 2. The pesticide product formulated in Example 2;

[0168] 3. The pesticide product formulated in Example 3;

[0169] 4. The pesticide product configured in Comparative Example 1;

[0170] 5. 2% thiacloprid (Shandong Tomple Crop Science Co., Ltd.);

[0171] 6. 8% cypermethrin microcapsule suspension (Chongqing Zhongbang Pharmaceutical Co., Ltd.);

[0172] 7. Water control.

[0173] Test site and test method:

[0174] The field test was carried out in Pinghu Forest Farm, Pinghu City, Zhejiang Province. The test variety was Masson pine, with an average tree height of 10 m and an average tree age of 10 years, and the slope was about 5 - 20 degrees. The surface spraying method on diseased wood was adopted, and the test was carried out from late May to late August, the peak period of Monochamus alternatus occurrence.

[0175] Select pine trees without grooves, eggs, and insects. Cut wooden sections with a diameter of 10 - 15 cm and a length of 100 cm. Seal the two ends of each group of processed wooden sections with wax. Drill holes on the wooden sections, and the distance between the holes should be evenly distributed on the surface of the wooden section. An example of the hole arrangement is shown in the following schematic diagram. The hole diameter is slightly larger than the larvae of Monochamus alternatus, and the hole depth is 4 cm. Place the mature larvae with the same age into the holes on the drilled wooden sections, one larva in each hole, 15 larvae in each section, then put in moist sawdust and wrap it with phloem. Spray the surface of the above wooden sections with the medicaments treated differently, and slowly and evenly spray the prepared liquid medicine (all diluted 6,000 times) onto the surface of the diseased wood until the surface is wet and the liquid medicine does not drip and flow away. Put the wooden sections with larvae into insect cages (200 - mesh net), and then place the insect cages in the corresponding outdoor environment. 30 days after the treatment, observe the number of Monochamus alternatus emerging. The schematic diagram of drilling holes is as Figure 5 .

[0176] Plot setting:

[0177] A total of 7 treatments were set. The plots of the test medicament, control medicament, and blank control were randomly arranged. Each treatment plot contained 3 wooden sections as a group of replicates, and each treatment had 4 groups of replicates. The blank control was sprayed with water.

[0178] Investigation method:

[0179] 30 days after the application of the medicine, calculate the reduction rate of the insect population through the number of emerged insects after eclosion and the number of inoculated insects before the application of the medicine.

[0180]

[0181] Test results:

[0182] The test results are shown in Table 2-5. The test results indicate that the medicaments in Examples 1, 2, and 3 have good control effects against Monochamus alternatus, which are higher than those of the control medicament.

[0183] Table 2-5 Field control effects of pesticide microemulsion containing thiacloprid and cypermethrin

[0184]

[0185]

[0186] 4. Forest trial II suspension concentrate:

[0187] Medicament treatment:

[0188] 1. The pesticide product formulated in Example 4;

[0189] 2. The pesticide product formulated in Example 5;

[0190] 3. The pesticide product formulated in Example 6;

[0191] 4. The pesticide product prepared in Comparative Example 2;

[0192] 5. 2% thiacloprid (Shandong Tomple Crop Science Co., Ltd.);

[0193] 6. 8% cypermethrin microcapsule suspension (Chongqing Zhongbang Pharmaceutical Co., Ltd.);

[0194] 7. Water control.

[0195] Test site and test method:

[0196] The forest trial was conducted in the forest farm of Anji County, Zhejiang Province. The test variety was Masson pine, with an average tree height of 14 m and an average tree age of 40 years, and the slope was about 10 - 20 degrees. The surface spraying method on diseased wood was adopted, and the test was carried out from late May to late August, the peak period of Monochamus alternatus occurrence.

[0197] Select pine trees without grooves, eggs, and insects. Cut wooden segments with a diameter of 10 - 15 cm and a length of 100 cm. Seal the two ends of each group of processed wooden segments with wax. Drill holes in the wooden segments, and the distance between the holes should be evenly distributed on the surface of the wooden segments. An example of the hole arrangement is shown in the following schematic diagram. The hole diameter is slightly larger than that of the longhorn beetle larvae, and the hole depth is 4 cm. Place the selected mature larvae of the same age in the holes on the drilled wooden segments, put one longhorn beetle larva in each hole, and put 15 longhorn beetle larvae in each segment. Then put in moist sawdust and wrap it with phloem. Spray the surface of the above-mentioned wooden segments with the medicaments treated differently above, and slowly and evenly spray the prepared liquid medicine (all diluted 6000 times) onto the surface of the diseased wood until the surface is wet and the liquid medicine does not drip and flow away. Put the wooden segments with larvae into an insect cage (200-mesh net), and then place the insect cage in the corresponding outdoor environment. 30 days after treatment, observe the number of longhorn beetles that emerge. The schematic diagram of drilling holes is as Figure 5 。

[0198] Plot setting:

[0199] A total of 7 treatments were set up. The plots of the test medicament, the control medicament, and the blank control were randomly arranged. Each treatment plot contained 3 wooden segments, which were a set of replicates, and each treatment had 4 sets of replicates. The blank control was sprayed with clear water.

[0200] Investigation method:

[0201] 30 days after the application of the medicine, calculate the reduction rate of the insect population through the number of insects after emergence and the number of inoculated insects before the application of the medicine.

[0202]

[0203] Test results:

[0204] The test results are shown in Table 2 - 6. The test results show that the medicaments in Examples 4, 5, and 6 have good control effects on Monochamus alternatus, which are higher than those of the control medicament.

[0205] Table 2 - 6 Field control effect of the pesticide suspoemulsion containing thiacloprid and cypermethrin

[0206]

Claims

1. Use of a synergistic pesticide containing a thiacloprid and cypermethrin composition for controlling Monochamus alternatus, characterized in that, The weight ratio of thiacloprid to cypermethrin is 3:1 - 1:

3.

2. The use according to claim 1, characterized in that, The dosage form of the synergistic pesticide is microemulsion, suspo-emulsion, soluble concentrate, or microcapsule suspension.

3. A synergistic pesticide containing a composition of thiacloprid and cypermethrin, characterized in that, When the dosage form is microemulsion, the preparation raw materials by weight percentage include: 5 - 20% thiacloprid technical, 5 - 15% cypermethrin technical, 10 - 15% block polyether, 3 - 6% ethanol, 5 - 10% propylene glycol, 10 - 20% decanamide, 5 - 10% cyclohexanone, and water to make up 100%; the block polyether is Ethylan NS-500LQ.

4. A synergistic pesticide containing a composition of thiacloprid and cypermethrin, characterized in that, When the dosage form is suspo-emulsion, the preparation raw materials by weight percentage include: 2 - 10% thiacloprid technical, 10 - 40% cypermethrin technical, 3 - 6% carboxylate complex, 3 - 5% phosphonate wetting agent, 3 - 6% block polyether, 0.1 - 0.3% xanthan gum, 0.1 - 0.3% Kathon, 0.2 - 0.4% silicone defoamer, 3 - 7% ethylene glycol, 0.3 - 0.7% magnesium aluminum silicate, 0.5 - 2% white carbon black, and deionized water to make up 100%; the block polyether is Ethylan NS-500LQ.

5. A synergistic pesticide containing a composition of thiacloprid and cypermethrin, characterized in that, When the dosage form is soluble concentrate, the preparation raw materials by weight percentage include: 5 - 10% thiacloprid technical, 10 - 15% cypermethrin technical, 5 - 15% anionic surfactant, 5 - 15% anionic-nonionic surfactant, 1 - 5% silicone surfactant, 15 - 30% fatty alcohol polyether, 10 - 15% decanamide, 2 - 5% ethanol, 5 - 8% cyclohexanone, 4 - 10% propylene glycol, and dimethylformamide to make up 100%; the anionic surfactant is SC3, and the anionic-nonionic surfactant is SC29.

6. A synergistic pesticide containing a composition of thiacloprid and cypermethrin, characterized in that, When the dosage form is microcapsule suspension, the preparation raw materials by weight percentage include: 2.5 - 10% thiacloprid technical, 2 - 10% cypermethrin technical, 20 - 30% xylene, 1 - 3% DM2601, 1 - 3% D8969, 0.1 - 0.3% defoamer, 3 - 5% ethylene glycol, 0.2 - 0.4% WM2501, 2 - 4% 8532CS, 0.1 - 0.3% Kathon, 0.1 - 0.2% xanthan gum, and water to make up to 100%.

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