A sanitary insecticide composition and its application

Abstract

The invention discloses a sanitary insecticide composition and application thereof. The active ingredients are compounded by component A and component B. By weight, the total weight of component A and component B accounts for 1% to 80% of the total weight of the insecticide composition, and the balance is other components. The component A is a compound shown in formula I; the component B is any one of dinotefuran, thiacloprid, thiamethoxam, sulfoxaflor and flupyrazone. The insecticide composition of the invention is low-toxic or slightly toxic, and has higher safety in use. The compounded agent has a synergistic effect at a certain ratio, and compared with a single agent, has improved knockdown and lethal effects, and is suitable for sanitary pests resistant to pyrethroids.

Description

Technical Field

[0001] The invention relates to a sanitary insecticide composition and application thereof. Background Art

[0002] The pyrethroid compound shown in formula I is a novel sanitary insecticide with good basic activity in preventing and controlling sanitary pests; the pyrethroid compound shown in formula I can be prepared according to the following reaction route:

[0003]

[0004] Wherein R is methyl or ethyl, M is sodium or potassium and R1 is hydrogen.

[0005] For example, 3-formyl-2,2-dimethylcyclopropanecarboxylic acid methyl ester (CAS No. 62138-41-4) is used as the starting material, and acetonitrile is reacted with sodium ethoxide at 60°C for 4 hours, dilute hydrochloric acid is added to neutralize the pH to 8, ethyl acetate and water are added to separate, and the oil layer is desolvated to obtain the intermediate 3-(2-cyano-1-vinyl)-2,2-dimethylcyclopropanecarboxylic acid methyl ester.

[0006] 2,3,5,6-tetrafluorobenzyl alcohol (CAS No. 4084-38-2), a catalytic amount of tetraisopropyl titanate and a toluene solvent are added to the obtained 3-(2-cyano-1-vinyl)-2,2-dimethylcyclopropanecarboxylic acid methyl ester, and the temperature is slowly raised to reflux to remove the by-product methanol, and the gas phase is controlled. After the raw material is completely converted, the temperature is lowered to 0-5° C., a small amount of water is added dropwise, the liquid is separated, and the solvent is removed to obtain the pyrethroid compound of formula I.

[0007] Using cyclopropanecarboxylates of different single configurations as starting materials, pyrethroid compounds of formula I of corresponding configurations can be obtained. For example, using (1R, 3R)-3-formyl-2,2-dimethylcyclopropanecarboxylic acid methyl ester (CAS No. 27335-33-7) as the starting material for synthesis, the obtained product is the 1R, 3R part of the chrysanthemum acid. After distributed crystallization and separation of the double bond CN group Z, E isomers, a single 2,3,4,5-tetrafluorobenzyl-(1R, 3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate or 2,3,4,5-tetrafluorobenzyl-(1R, 3R)-3-[(1E)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate can be obtained. 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-(-2-cyano-1-vinyl)-2,2-dimethylcyclopropylcarboxylate or 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate or 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1E)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate can be obtained from methyl (1R,3S)-3-(-2-cyano-1-vinyl)-2,2-dimethylcyclopropylcarboxylate.

[0008] Due to the long-term use of pesticides, the resistance of sanitary pests to organophosphorus, carbamate, and pyrethroid insecticides is getting higher and higher. In practical applications, highly active compounds are needed to improve the prevention effect and reduce the amount of pesticides used. Since the compound of formula I is first applied to the control of sanitary pests in space spraying and retention spraying, the activity is relatively high, and the nicotine products lack a rapid knockdown effect in the field of sanitary pest control when used alone, and the application is relatively difficult. The present invention has been screened out by experiments that the two have obvious synergistic effects, and the efficacy is significantly higher than that of commercially available products, solving the problem of cross-resistance between pyrethroids. The high lethal activity of nicotine and the high knockdown activity of formula I pyrethroid compounds complement each other in the control of sanitary pests, and the lethal compound currently used, such as pyrethroids, carbamates and organophosphorus, is mostly poisoning or highly toxic, and the nicotine compounds screened in this experiment are all low-toxic, safer to use, and the development of this type of original medicine with higher safety meets the needs of social development. Summary of the invention

[0009] The technical problem to be solved by the present invention is to provide a sanitary insecticide composition and its application in view of the deficiencies existing in the prior art, wherein the high-efficiency pyrethroid shown in formula I is used as one of the active ingredients, and is compounded with a nicotinoid insecticide to complement each other's advantages, thereby ensuring a rapid knockdown effect and high lethal activity, and solving the problem of cross-resistance caused by compounding between pyrethroids.

[0010] In order to achieve the above object, the present invention adopts the following technical solution:

[0011] The present invention provides an insecticide composition, wherein the active ingredient is compounded from component A and component B, wherein the total weight of component A and component B accounts for 1% to 80% of the total weight of the insecticide composition, and the remainder is an adjuvant;

[0012] The component A is a compound represented by formula I, namely 2,3,4,5-tetrafluorobenzyl-3-[-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate;

[0013] The component B is any one of dinotefuran, thiacloprid, thiamethoxam, sulfoxaflor, and flupyrazone;

[0014]

[0015] In the above technical scheme, the component A is preferably selected from any one of the four isomers of 2,3,4,5-tetrafluorobenzyl-(1R, 3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropyl carboxylate, 2,3,4,5-tetrafluorobenzyl-(1S, 3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropyl carboxylate, 2,3,4,5-tetrafluorobenzyl-(1R, 3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropyl carboxylate, and 2,3,4,5-tetrafluorobenzyl-(1S, 3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropyl carboxylate, or a mixture of two or more of the four isomers in any proportion.

[0016] In the above technical solution, the weight ratio of component A to component B is 5:1 to 1:20.

[0017] In the above technical solution, the weight ratio of component A to component B is preferably 1:2 to 1:20.

[0018] In the above technical solution, the auxiliary agent is any two or more of a dispersant, a wetting agent, a disintegrant, a filler, an antifreeze agent, a thickener, a preservative, a defoaming agent, a solvent, an emulsifier, an encapsulating material, an organic amine and deionized water.

[0019] In the above technical solution, the insecticide composition has the dosage form of emulsifiable concentrate, aqueous emulsion, microemulsion, wettable powder, suspension, water-dispersible granules, dry suspension or microcapsule suspension.

[0020] In the above technical scheme, the insecticide composition, when in the form of emulsifiable concentrate, comprises the following raw materials in weight percentage: 0.5-20% of component A, 0.5-20% of component B, 5-30% of emulsifier, and solvent to make up to 100%.

[0021] In the above technical scheme, the insecticide composition, when in the form of an aqueous emulsion, comprises the following raw materials in weight percentage: 2-15% of component A, 4-15% of component B, 5-20% of solvent, 6-20% of emulsifier, 3-8% of antifreeze, 0.1-1% of defoaming agent, and deionized water is added to 100%.

[0022] In the above technical scheme, the insecticide composition, when in the form of a microemulsion, comprises the following raw materials in weight percentage: 1-15% of component A, 1-15% of component B, 3-30% of solvent, 10-35% of emulsifier, and deionized water is added to 100%.

[0023] In the above technical scheme, the insecticide composition, when in the form of a wettable powder, comprises the following raw materials in weight percentage: 1-20% of component A, 1-50% of component B, 2-6% of a wetting agent, 7-18% of a dispersant, and the filler is supplemented to 100%.

[0024] In the above technical scheme, the insecticide composition, when in the form of a suspension, comprises the following raw materials in weight percentage: 1-20% of component A, 1-20% of component B, 1-8% of a wetting agent, 1-8% of a dispersant, 3-7% of an antifreeze agent, 0.3-2% of a preservative, 0.1-1% of a defoaming agent, 0.5-3% of a thickener, and deionized water is added to 100%.

[0025] In the above technical scheme, the insecticide composition, when in the form of water-dispersible granules, comprises the following raw materials in weight percentage: 1-20% of component A, 1-40% of component B, 2-12% of wetting agent, 5-18% of dispersant, 2-8% of disintegrant, and the filler is supplemented to 100%.

[0026] In the above technical scheme, the insecticide composition, when in the form of a dry suspension, comprises the following raw materials in weight percentage: 1-20% of component A, 1-40% of component B, 1-8% of a wetting agent, 1-8% of a dispersant, and the filler is supplemented to 100%.

[0027] In the above technical scheme, the insecticide composition, when in the form of a microcapsule suspension, comprises the following percentages of raw materials: 1-20% of component A, 1-20% of component B, 1-5% of a wetting agent, 1-10% of an encapsulation material, 1-8% of a dispersant, 2-6% of an antifreeze agent, 0.3-1% of a preservative, 0.1-1% of a defoaming agent, 0.5-2% of a thickener, 0.1-5% of an organic amine, and deionized water is supplemented to 100%.

[0028] In the above technical scheme, the dispersant is selected from any one of polycarboxylates, lignin sulfonates, alkylphenol polyoxyethylene ether formaldehyde condensates, naphthalenesulfonic acid formaldehyde condensates sodium salts, nonionic hydroxy polyethylene oxide block copolymers, fatty amine polyoxyethylene ethers, fatty acid polyoxyethylene esters, and glycerol fatty acid ester polyoxyethylene ethers, or a mixture of two or more in any proportion.

[0029] In the above technical scheme, the wetting agent is selected from: any one of alkylbenzene polyoxyethylene ether phosphate, phenethylphenol polyoxyethylene ether phosphate, alkyl sulfates, naphthalene sulfonates, sodium dodecyl sulfate, pull-opening powder BX, alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, alkyl sulfonates, dodecylbenzene sulfonic acid, or a mixture of two or more in any proportion.

[0030] In the above technical solution, the disintegrant is selected from: any one of sodium bicarbonate, sodium chloride, ammonium sulfate, sodium carbonate, sodium sulfate, or a mixture of two or more of them in any proportion.

[0031] In the above technical solution, the filler is selected from: any one of attapulgite, calcium carbonate, kaolin, white carbon, corn starch, light calcium, diatomaceous earth, or a mixture of two or more of them in any proportion.

[0032] In the above technical solution, the antifreeze agent is any one of ethylene glycol, propylene glycol, glycerol, glycerin, and urea, or a mixture of two or more of them in any proportion.

[0033] In the above technical solution, the thickener is any one of xanthan gum, hydroxyethyl cellulose, methyl cellulose, magnesium aluminum silicate, and organic bentonite, or a mixture of two or more of the above in any proportion.

[0034] In the above technical solution, the preservative is any one of sodium benzoate, benzoic acid, potassium sorbate, and kasone, or a mixture of two or more of them in any proportion.

[0035] In the above technical solution, the defoaming agent is any one of silicone compounds, silicone oil, C8-10 fatty alcohol compounds, and C10-20 saturated fatty acid compounds, or a mixture of two or more of them in any proportion.

[0036] In the above technical scheme, the solvent is selected from: 100# solvent oil, 150# solvent oil, 200# solvent oil, dimethylformamide, dimethylacetamide, xylene, N-methylpyrrolidone, methanol, ethanol, n-butanol, turpentine, soybean oil, methyl oleate, corn oil, rapeseed oil, castor oil, any one of C8-16 alkane solvents, or a mixture of two or more in any proportion.

[0037] In the above technical scheme, the C8-16 alkane solvent is selected from: D60 (ExxonMobil Petrochemical Company), D80 (ExxonMobil Petrochemical Company), D100 (ExxonMobil Petrochemical Company), D110 (ExxonMobil Petrochemical Company), Isopar-E (ExxonMobil Petrochemical Company), Isopar-G (ExxonMobil Petrochemical Company), Isopar-H (ExxonMobil Petrochemical Company), Isopar-L (ExxonMobil Petrochemical Company), Isopar-M (ExxonMobil Petrochemical Company), quinane, undecane, dodecane, tridecane, tetradecane, pentadecane, hexadecane, heptadecane, octadecane, any one of them, or a mixture of two or more of them in any proportion.

[0038] In the above technical scheme, the emulsifier is selected from: any one of calcium dodecylbenzene sulfonate, OP series phosphate, nonylphenol polyoxyethylene ether, alkylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, Span series, Tween series, fatty alcohol polyoxyethylene ether, styrylphenol polyoxyethylene ether, styrylphenol polyoxyethylene ether phosphate, alkylaryl polyoxyethylene ether polyoxypropylene ether, or a mixture of two or more in any proportion.

[0039] In the above technical solution, the capsule-forming material is selected from: any one of diphenylmethane diisocyanate and tolyl diisocyanate, or a mixture of the two in any proportion.

[0040] In the above technical solution, the organic amine is selected from: any one of ethylenediamine, propylenediamine, butylenediamine, octanediamine, diethylenetriamine, and 1,6-hexanediamine, or a mixture of any two of them in any proportion.

[0041] The invention also provides an application of the insecticide composition for preventing and controlling sanitary pests in places where sanitary pests appear.

[0042] In the above technical solution, the sanitary pests are mosquitoes, flies, fleas, ants, cockroaches, mites, wasps and bedbugs.

[0043] In the above technical scheme, the sanitary pests are preferably Culex pipiens pallens, Culex pipiens quinquefasciatus, Culex tritaeniorhynchus, Aedes albopictus, Aedes aegypti, Anopheles sinensis, Aedes harassingus, Chironomids, housefly, city fly, Chrysopa longituba, Lucilia sericata, Lucilia cuprina, Lucilia brevifolia, summer toilet fly, Yuan toilet fly, German cockroach, American cockroach, bedbug, flea, Ixodes persulcatus, Ixodes sinensis, Ixodes prairies, Boophilus microplus, Gamas, scabies, ants and wasps.

[0044] In the above technical solution, the places where sanitary pests appear refer to hotels, airplanes, schools, factories, home residences or livestock habitats.

[0045] In the above technical scheme, the insecticide composition is used to control sanitary pests by residual spraying: the insecticide composition is diluted 50-1000 times with water and sprayed on the surfaces of objects such as walls, doors and windows, ceilings, plants and homes where sanitary pests are present, so that the insecticide composition remains on the surfaces of the above objects, knocking down and killing the sanitary pests. The applicable dosage forms are suspension concentrate, wettable powder, water dispersible granules and dry suspension concentrate.

[0046] In the above technical scheme, the insecticide composition is used to control sanitary pests by space spraying. The insecticide composition is diluted 5-200 times with water and sprayed evenly into the space where the sanitary pests are present by normal spraying, low volume spraying or ultra-low volume spraying. When the sanitary pests are active in the spraying space, they are exposed to the agent, which knocks them down and kills them, thereby controlling the sanitary pests. The applicable dosage forms are emulsifiable concentrates, water emulsions and microemulsions.

[0047] The insecticide composition of the present invention uses pyrethroids and nicotine compounds to complement each other and have obvious synergistic effect, thereby ensuring a rapid knockdown effect and high lethal activity, and has higher safety and meets the needs of social development. DETAILED DESCRIPTION

[0048] The specific implementation of the technical solution of the present invention is described in detail below, but the present invention is not limited to the following description:

[0049] The present invention will be described below in conjunction with specific embodiments:

[0050] The laboratory preparation method of wettable powder is as follows: add component A, component B, wetting agent, dispersant and filler into a food processor and mix them evenly, then put them into a jet mill for crushing.

[0051] The laboratory preparation method of the suspension concentrate is as follows: weigh the wetting agent, dispersant, antifreeze, preservative, defoamer and deionized water according to the proportion, add them into a beaker and mix them evenly, then add component A and component B into the beaker, and then transfer it to a sand mill, add zirconium oxide beads into the sand mill, grind for 2-3 hours, add thickener and continue grinding for 0.5 hours to make the particle size D 95 The product can be obtained by controlling the particle size below 5 microns and filtering to remove the zirconium oxide beads.

[0052] The laboratory preparation method of water-dispersible granules is as follows: add component A, component B, wetting agent, dispersant, disintegrant and filler into a food processor and mix them evenly, then put them into a jet mill for grinding, mix them again with a food processor, add an appropriate amount of water, and extrude and granulate them with a granulator.

[0053] The laboratory preparation method of the dry suspension is as follows: weigh the wetting agent, dispersant, filler and water according to the proportion, add them into a beaker and mix them evenly, then add component A and component B into the beaker, and then transfer it to a sand mill, add zirconium oxide beads into the sand mill, grind for 2-3 hours, and make the particle size D 95 The particle size is controlled below 5 microns, the zirconium oxide beads are removed by filtration, and the obtained material is dried by a spray dryer to obtain the product.

[0054] The preparation method of emulsifiable concentrate is as follows: dissolving component A and component B in a solvent, adding an emulsifier, mixing and dissolving under stirring to form a transparent liquid.

[0055] The preparation method of the water emulsion is as follows: component A, component B, solvent and emulsifier are dissolved into oil phase, deionized water, antifreeze agent and defoaming agent form water phase, and the water phase is added to the oil phase or the oil phase is added to the water phase under high-speed shearing to obtain the water emulsion.

[0056] The preparation method of the microemulsion is as follows: after component A, component B, solvent and emulsifier are uniformly dissolved, deionized water is added to form a transparent liquid to obtain the microemulsion.

[0057] Preparation method of microcapsule suspension: Component A, capsule material and solvent are heated and dissolved to form an oil phase, and then added to the water phase under shearing conditions, sheared for 5 minutes, and organic amine was slowly added dropwise, and then kept warm at a certain temperature and solidified. After the reaction is completed, the pH is adjusted, and finally deionized water is added to make up to 100g to obtain a microcapsule suspension.

[0058] Formulation Example 1: 1% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate·dinotefuran emulsifiable concentrate

[0059] 0.5 g of 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 0.5 g of dinotefuran, 4 g of calcium dodecylbenzenesulfonate, 8 g of castor oil polyoxyethylene ether, 6 g of dimethylformamide, and 150# solvent oil are added to make up to 100 g, and emulsifiable concentrate is prepared according to the above method.

[0060] Formulation Example 2: 12% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate·dinotefuran emulsifiable concentrate

[0061] 2g of 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 10g of dinotefuran, 4g of calcium dodecylbenzenesulfonate, 13g of alkylphenol polyoxyethylene ether, 7g of N-methylpyrrolidone, and 150# solvent oil are added to make up to 100g, and emulsifiable concentrate is prepared according to the above method.

[0062] Formulation Example 3: 8% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate·thiacloprid emulsifiable concentrate

[0063] 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate 1g, thiacloprid 7g, Span 803g, alkylphenol polyoxyethylene ether 9g, dimethylformamide 5g, 150# solvent oil is added to make up to 100g, and emulsifiable concentrate is prepared according to the above method.

[0064] Formulation Example 4: 16% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate·thiamethoxam emulsifiable concentrate

[0065] 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate 1g, thiamethoxam 15g, calcium dodecylbenzenesulfonate 6g, styrylphenol polyoxyethylene ether 10g, N-methylpyrrolidone 5g, and xylene are added to make up to 100g, and an emulsifiable concentrate is prepared according to the above method.

[0066] Formulation Example 5: 21% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate·sulfoxaflor emulsifiable concentrate

[0067] 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate 1g, sulfoxaflor 20g, calcium dodecylbenzenesulfonate 6g, castor oil polyoxyethylene ether 12g, N-methylpyrrolidone 5g, 150# solvent oil is added to make up to 100g, and emulsifiable concentrate is prepared according to the above method.

[0068] Formulation Example 6: 10% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate·sulfoxaflor aqueous emulsion

[0069] 2g of 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 8g of sulfoxaflor, 4g of calcium dodecylbenzenesulfonate, 8g of castor oil polyoxyethylene ether, 5g of styrylphenol polyoxyethylene ether, 2g of n-butanol, 15g of 150# solvent oil, 5g of ethylene glycol, 0.5g of polydimethylsiloxane, and deionized water are added to make up to 100g, and a water emulsion is prepared according to the above method.

[0070] Formulation Example 7: 9% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate·fluoropyranone microemulsion

[0071] 6 g of 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 3 g of fluoropyranone, 12 g of castor oil polyoxyethylene ether, 20 g of styrylphenol polyoxyethylene ether phosphate, 28 g of 150# solvent oil, 2 g of n-butanol, and deionized water are added to make up to 100 g, and a microemulsion is prepared according to the above method.

[0072] Formulation Example 8: 15% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate·furantoin microemulsion

[0073] 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate 10g, dinotefuran 5g, calcium dodecylbenzenesulfonate 4g, castor oil polyoxyethylene ether 30g, 150# solvent oil 30g, deionized water to make up to 100g, and a microemulsion was prepared according to the above method.

[0074] Formulation Example 9: 11% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate·thiacloprid aqueous emulsion

[0075] 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate 1g, thiacloprid 10g, calcium dodecylbenzenesulfonate 4g, styrylphenol polyoxyethylene ether 15g, n-butanol 2g, 150# solvent oil 18g, ethylene glycol 5g, polydimethylsiloxane 0.5g, deionized water is added to make up to 100g, and an aqueous emulsion is prepared according to the above method.

[0076] Formulation Example 10: 16% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate·thiamethoxam aqueous emulsion

[0077] 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate 1g, thiamethoxam 15g, calcium dodecylbenzenesulfonate 3g, castor oil polyoxyethylene ether 14g, n-butanol 2g, 150# solvent oil 18g, ethylene glycol 5g, polydimethylsiloxane 0.5g, deionized water is added to make up to 100g, and an aqueous emulsion is prepared according to the above method.

[0078] Formulation Example 11: 20% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate·dinotefuran suspension

[0079] 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate 10g, dinotefuran 10g, alkylbenzene polyoxyethylene ether phosphate 4g, alkylphenol polyoxyethylene ether formaldehyde condensate 8g, propylene glycol 2g, ethylene glycol 3g, potassium sorbate 0.5g, silicone oil 0.2g, magnesium aluminum silicate 1g, xanthan gum 0.3g, deionized water is added to 100g. The suspension is prepared according to the above method.

[0080] Formulation Example 12: 15% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate·dinotefuran suspension

[0081] 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate 5g, dinotefuran 10g, sodium dodecyl sulfate 3g, alkylphenol polyoxyethylene ether formaldehyde condensate 8g, propylene glycol 1g, urea 3g, potassium sorbate 0.5g, silicone oil 0.2g, magnesium aluminum silicate 0.5g, xanthan gum 0.4g, deionized water is added to make up to 100g. The suspension is prepared according to the above method.

[0082] Formulation Example 13: 25% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate·thiacloprid suspension

[0083] 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate 5g, thiacloprid 20g, alkylbenzene polyoxyethylene ether phosphate 3g, glycerol fatty acid ester polyoxyethylene ether 8g, glycerol 5g, sodium benzoate 0.5g, kason 0.3g, silicone oil 0.2g, magnesium aluminum silicate 0.5g, xanthan gum 0.2g, deionized water is added to 100g. The suspension is prepared according to the above method.

[0084] Formulation Example 14: 60% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate·thiacloprid water dispersible granules

[0085] 20g of 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 40g of thiacloprid, 2g of lakai powder BX, 2g of sodium dodecyl sulfate, 6g of naphthalenesulfonic acid formaldehyde condensate sodium salt, 4g of ammonium sulfate, and kaolin is added to make up to 100g. Water dispersible granules are prepared according to the above method.

[0086] Formulation Example 15: 50% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate·sulfoxaflor water dispersible granules

[0087] 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate 10g, sulfoxaflor 40g, sodium dodecyl sulfate 4g, alkylphenol polyoxyethylene ether formaldehyde condensate 6g, naphthalenesulfonic acid formaldehyde condensate sodium salt 10g, sodium sulfate 4g, corn starch is supplemented to 100g. Water dispersible granules are prepared according to the above method.

[0088] Formulation Example 16: 40% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate·sulfoxaflor water dispersible granules

[0089] 20 g of 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 20 g of sulfoxaflor, 6 g of sodium dodecyl sulfate, 12 g of naphthalenesulfonic acid formaldehyde condensate sodium salt, 4 g of sodium sulfate, and corn starch to make up to 100 g. Water dispersible granules were prepared according to the above method.

[0090] Formulation Example 17: 50% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate·fluoropyranone wettable powder

[0091] 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate 5g, fluoropyranone 45g, sodium dodecyl sulfate 3g, naphthalenesulfonic acid formaldehyde condensate sodium salt 12g, white carbon black 4g, kaolin is added to make up to 100g. Wettable powder is prepared according to the above method.

[0092] Formulation Example 18: 30% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate·fluoropyranone wettable powder

[0093] 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate 10g, fluoropyranone 20g, sodium dodecyl sulfate 5g, naphthalenesulfonic acid formaldehyde condensate sodium salt 10g, fatty amine polyoxyethylene ether 2g, white carbon black 3g, kaolin is supplemented to 100g. Wettable powder is prepared according to the above method.

[0094] Formulation Example 19: 60% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate·thiamethoxam dry suspension

[0095] 20 g of 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 40 g of thiamethoxam, 4 g of alkylbenzene polyoxyethylene ether phosphate, 8 g of naphthalenesulfonic acid formaldehyde condensate sodium salt, and kaolin to make up to 100 g. A dry suspension was prepared according to the above method.

[0096] Formulation Example 20: 12% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate·thiamethoxam microcapsule suspension

[0097] 4 g of 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 8 g of thiamethoxam, 3 g of sodium dodecyl sulfate, 4 g of nonionic hydroxy polyethylene oxide block copolymer, 2 g of phenethylphenol polyoxyethylene ether phosphate and 1 g of diphenylmethane diisocyanate are heated and dissolved, and then added to 60 g of an aqueous solution containing 5% glycerol under shearing conditions, sheared for 5 minutes, 0.25 g of diethylenetriamine was slowly added dropwise, and then kept warm at 50° C. for 5 hours. After the reaction is completed, the pH is adjusted to 4-6 with acetic acid, and then 1 g of xanthan gum, 0.5 g of potassium sorbate and 0.5 g of silicone oil are added, and finally the amount is supplemented to 100 g with deionized water, and stirred evenly to obtain a microcapsule suspension.

[0098] Formulation Example 21: 21% 2,3,4,5-tetrafluorobenzyl-3-[-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate·sulfoxaflor emulsifiable concentrate

[0099] 2,3,4,5-tetrafluorobenzyl-3-[-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate 1g, sulfoxaflor 20g, calcium dodecylbenzenesulfonate 6g, castor oil polyoxyethylene ether 12g, N-methylpyrrolidone 5g, 150# solvent oil is added to make up to 100g, and emulsifiable concentrate is prepared according to the above method.

[0100] Formulation Example 22: 20% 2,3,4,5-tetrafluorobenzyl-3-[-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate·dinotefuran suspension

[0101] 2,3,4,5-tetrafluorobenzyl-3-[-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate 10g, dinotefuran 10g, alkylbenzene polyoxyethylene ether phosphate 4g, alkylphenol polyoxyethylene ether formaldehyde condensate 8g, propylene glycol 2g, ethylene glycol 3g, potassium sorbate 0.5g, silicone oil 0.2g, magnesium aluminum silicate 1g, xanthan gum 0.3g, deionized water is added to make up to 100g. The suspension is prepared according to the above method.

[0102] Comparative Example 1: 10% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate emulsifiable concentrate

[0103] 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate 10g, calcium dodecylbenzenesulfonate 6g, castor oil polyoxyethylene ether 8g, 150# solvent oil to 100g, and prepare emulsifiable concentrate according to the above method

[0104] Comparative Example 2: 10% Dinotefuran EC

[0105] Dinotefuran 10g, calcium dodecylbenzene sulfonate 6g, castor oil polyoxyethylene ether 10g, dimethylformamide 10g, 150# solvent oil to 100g, according to the above method to prepare emulsifiable concentrate

[0106] Comparative Example 3: 20% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate wettable powder

[0107] 20g of 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 5g of sodium dodecyl sulfate, 10g of naphthalenesulfonic acid formaldehyde condensate sodium salt, 2g of fatty amine polyoxyethylene ether, 3g of white carbon black, and kaolin to make up to 100g. Wettable powder was prepared according to the above method.

[0108] Comparative Example 4: 30% sulfoxaflor wettable powder

[0109] 30g of sulfoxaflor, 6g of sodium dodecyl sulfate, 12g of sodium salt of naphthalenesulfonic acid formaldehyde condensate, 2g of fatty amine polyoxyethylene ether, 5g of white carbon black, and kaolin to make up to 100g. A wettable powder was prepared according to the above method.

[0110] Control agent 1: 10% highly effective cyhalothrin wettable powder (commercially available)

[0111] Control agent 2: 5% tetrafluthrin / permethrin emulsion in water (commercially available)

[0112] Verification test 1: Co-toxicity coefficient test

[0113] (1) Test subjects: Culex pipiens, Musca domestica (laboratory reared)

[0114] (2) Test method: Refer to GB / T26350-2010 "Methods for detecting insecticide resistance in flies - Housefly bioassay" and NY / T1154.7-2006 "Guidelines for indoor bioassay of pesticides - Insecticides - Part 7: Determination of the combined effect of mixtures"

[0115] (3) Data statistics: Take the drug to be tested and dissolve it in dichloromethane first, then use an aqueous solution containing 0.1% Triton-X100 to perform a series of dilutions at a ratio of 1:9, take 1mL of each diluted concentration and add it to a 150mL serum bottle, keep rotating the serum bottle to make the drug solution evenly distributed on the inner wall of the bottle, place it in a fume hood overnight to allow the organic solvent to evaporate completely, and then put the test insects in to determine the concentration range of the drug that causes 100% death and 100% survival. Take the appropriate concentration within this range and use an aqueous solution containing 0.1% Triton-X100 to perform a series of multiple dilutions. Take 1mL of each diluted concentration and add it to a 150mL serum bottle, keep rotating the serum bottle to make the drug solution evenly distributed on the inner wall of the bottle, place it in a fume hood overnight to allow the organic solvent to evaporate completely. Then apply vaseline on the bottleneck of the serum bottle, put 20 test insects in each bottle, and repeat the experiment 5 times. The corresponding solvent treatment is used as the control group. After 1 hour, all test insects were transferred to clean containers for standard feeding. After 24 hours, the number of deaths was checked and counted. The statistical analysis software SPSS was used for analysis to calculate the LC50 of each agent and its 95% confidence limit. The test results are shown in the following table:

[0116] Table 1 Co-toxicity coefficient of 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate and dinotefuran to houseflies

[0117]

[0118] It can be seen from Table 1 that when the compound ratio of 2,3,4,5-tetrafluorobenzyl-(1R, 3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate: dinotefuran is 5:1 to 1:20, the co-toxicity coefficient to houseflies is greater than 120, showing a synergistic effect. In particular, when the compound ratio is 1:2 to 1:20, the co-toxicity coefficient to houseflies is greater than 150, showing a significant synergistic effect.

[0119] Table 2 The co-toxicity coefficient of 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate and sulfoxaflor to Culex pipiens pallens

[0120]

[0121] It can be seen from Table 2 that when the combined ratio of 2,3,4,5-tetrafluorobenzyl-(1R, 3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate:sulfoxaflor is 5:1 to 1:20, the co-toxicity coefficient to Culex pipiens is greater than 120, showing a synergistic effect. In particular, when the combined ratio is 1:2 to 1:20, the co-toxicity coefficient to Culex pipiens is greater than 150, showing a significant synergistic effect.

[0122] In addition, when the compounding ratio of 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate and other components B is 1:2 to 1:20, there is also a similar synergistic effect on mosquitoes and flies.

[0123] Verification test 2: Efficacy test of mosquito and fly control spray

[0124] (1) Test subjects: Culex pipiens and housefly (laboratory reared)

[0125] (2) Test method: Refer to GB / T13917.1-2009 Indoor efficacy test and evaluation of public health insecticides for pesticide registration, spray test.

[0126] (3) Test agents: Preparation Examples 2, 3, 4, 5, 6, 7, 8, 9, 10, and 21 were diluted with water to 1000 ppm, and Comparative Example 1, Comparative Example 2, and Control Agent 2 were diluted with water to 1000 ppm.

[0127] (4) Statistics:

[0128] Table 3 Results of efficacy tests of several treatments against Culex pipiens and houseflies

[0129]

[0130]

[0131] Verification test 3: Efficacy test for preventing and controlling mosquitoes and flies

[0132] (1) Test subjects: Culex pipiens and Musca domestica

[0133] (2) Test method: Refer to GB / T13917.1-2009 Indoor efficacy test and evaluation of public health insecticides for pesticide registration, residual spraying test.

[0134] (3) Test agents: Preparation Examples 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, and 22 were diluted with water to 800 ppm, and Comparative Example 3, Comparative Example 4, and Control Agent 1 were diluted with water to 800 ppm.

[0135] (4) Statistics:

[0136] Table 4 Results of efficacy tests of several treatments against Culex pipiens and houseflies

[0137]

[0138]

[0139] The above examples are only for illustrating the technical concept and technical features of the present invention, and cannot be used to limit the protection scope of the present invention. Any equivalent transformation or modification made according to the essence of the present invention should be included in the protection scope of the present invention.

Claims

1. A sanitary insecticide composition, characterized in that: The active ingredient is compounded from component A and component B, wherein the total weight of component A and component B accounts for 1% to 80% of the total weight of the insecticide composition, and the remainder is adjuvant; The component A is a compound represented by formula I, namely 2,3,5,6-tetrafluorobenzyl-3-(-2-cyano-1-vinyl)-2,2-dimethylcyclopropylcarboxylate; The component B is any one of dinotefuran and sulfoxaflor; 2. The composition according to claim 1, characterized in that The component A is selected from any one of the four isomers of 2,3,5,6-tetrafluorobenzyl-(1R, 3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 2,3,5,6-tetrafluorobenzyl-(1S, 3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 2,3,5,6-tetrafluorobenzyl-(1R, 3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, and 2,3,5,6-tetrafluorobenzyl-(1S, 3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, or a mixture of two or more of the four isomers in any proportion.

3. The sanitary insecticidal composition according to claim 1, characterized in that The weight ratio of component A to component B is 5:1 to 1:

20.

4. The sanitary insecticidal composition according to claim 1, characterized in that The weight ratio of component A to component B is 1:2 to 1:

20.

5. The sanitary insecticidal composition according to claim 1, characterized in that: The auxiliary agent is any two or more of a dispersant, a wetting agent, a disintegrant, a filler, an antifreeze agent, a thickener, a preservative, a defoamer, a solvent, an emulsifier, an encapsulation material and deionized water.

6. The sanitary insecticidal composition according to claim 1, characterized in that: The insecticide composition has the following dosage forms: emulsifiable concentrate, water emulsion, microemulsion, wettable powder, suspension, water dispersible granules, dry suspension or microcapsule suspension.

7. Use of the sanitary insecticide composition according to any one of claims 1 to 6 for controlling sanitary pests in places where sanitary pests are present, characterized in that: The sanitary pests are mosquitoes, flies, fleas, ants, cockroaches, mites, bees and bedbugs; the places where sanitary pests appear are hotels, airplanes, schools, factories, family residences or livestock habitats.

8. The use according to claim 7, characterized in that: When the insecticide composition is used to control sanitary pests, it adopts a residual spraying method to control sanitary pests: the insecticide composition is diluted with water and sprayed on the surfaces of walls, doors and windows, ceilings, plants and homes in places where sanitary pests are present. Applicable dosage forms are suspensions, wettable powders, water-dispersible granules, microcapsule suspensions and dry suspensions.

9. The use according to claim 7, characterized in that: When the insecticide composition is used to control sanitary pests, it is sprayed in space. After the insecticide composition is diluted with water, it is evenly sprayed into the space where the sanitary pests are present by means of constant volume spray, low volume spray or ultra-low volume spray. Applicable dosage forms are emulsifiable concentrate, water emulsion and microemulsion.

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