Preparation containing biphenyl compound and application thereof

By developing a composite preparation of biphenyl compounds with surfactants and carriers, the problems of unqualified suspension rate and drug resistance during thermal storage are solved, the stability and broad-spectrum prevention and treatment of the preparation are achieved, and the production cost is reduced.

CN120283760APending Publication Date: 2025-07-11SHENYANG SINOCHEM AGROCHEMICALS R&D CO LTD +1
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Patent Information

Application Number
CN202410041171.2
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-01-11
Publication Date
2025-07-11

AI Technical Summary

Technical Problem

The existing biphenyl compound preparations are prone to solid particles adhesion and melting during the thermal storage process, resulting in unqualified suspension rate and the use of a single active component is prone to the problem of drug resistance and narrow prevention and treatment spectrum.

Method used

By adding biphenyl compounds and surfactants and carriers, the stabilizers coconut oil and calcium stearate are added to develop different dosage forms such as emulsion oil, water emulsion, microemulsion, suspension agent, etc., combined with the appropriate additive system, the heat storage problem is overcome and drug resistance is delayed.

Benefits of technology

It improves the stability and suspension rate of the preparation, expands the prevention and control spectrum, reduces production costs, extends the service life of the active components, and does not require ready-made use.

✦ Generated by Eureka AI based on patent content.

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Patent Text Reader

Abstract

The invention belongs to the field of insecticides and acaricides, and particularly relates to a biphenyl compound-containing preparation and application thereof. The preparation is composed of an active component A, an active component B, at least one surfactant and at least one carrier, the weight percentage of the active components is 0.1-95%, and the mass ratio of the active component A to the active component B is 1: 99-99: 1. The preparation provided by the invention can be used for preventing and treating various pests and mites.
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Description

Technical Field

[0001] The present invention belongs to the field of insecticides and acaricides, and particularly relates to a preparation containing a biphenyl compound and its application. Background Art

[0002] Insecticides and acaricides play an obvious role in controlling agricultural and forestry pests or urban sanitary pests. Chinese Invention Patent CN105541682A discloses that the biphenyl compound 2,2'-difluoro-4,4'-dimethyl-5,5'-bis[(2,2,2-trifluoroethyl)thio]-1,1'-biphenyl (hereinafter referred to as Compound A) has excellent insecticidal and acaricidal control effects, is a highly efficient insecticide and acaricide variety, and has broad market application prospects. However, there are certain defects in using insecticides and acaricides with a single active ingredient for a long time to control diseases, such as the target organisms are prone to develop drug resistance, reducing the use effect of the active ingredient. At the same time, the control spectrum is relatively narrow, and the ideal control effect cannot be achieved. By compounding two or more active ingredients, the occurrence of target drug resistance problems can be delayed, the service life of novel active ingredients can be extended, the disease control spectrum can be expanded, the control effect can be improved, the application amount of the active ingredient can be reduced, and the environmental pollution problem can be reduced. As a highly efficient chemical substance, the active ingredient is not suitable for direct use in agricultural production operations. At the same time, if you want to endow the active ingredient with the best use effect in different operation scenarios, it is necessary to select a suitable adjuvant to match the active ingredient according to different crops and target diseases, develop a dosage form product suitable for the agricultural operation scenario and then apply it. The selection of a suitable pesticide dosage form and the high quality of the pesticide preparation are the key factors determining the value and effect of the pesticide product. Patents CN111226945B, CN111226955A, CN111226927A, CN111657280B, CN111657281A, CN111657282B, CN112704075A, CN112704070B, CN114642204A, CN114642203B, CN115530170A report that the combination of Compound A and Compound B shows obvious synergistic effects on insecticidal and acaricidal activities within a certain ratio range, improving the control effect of the single active ingredient compound in the combination on pests. The patents only generally disclose that the above combination can be processed into a preparation, and the liquid medicine for controlling pests and mites is prepared according to the method mentioned in the above patents. The amount of organic solvent and adjuvant used is large, the cost is high, and it can only be prepared and used immediately, which is difficult to meet the actual needs. The combination of Compound A and Compound B mentioned in Patent CN115633687A can be prepared in the form of a dosage form in a certain ratio, which is a generally applicable preparation, but the physical properties of the prepared product cannot be guaranteed. Due to the low melting point characteristic of active ingredient A, the melting point is only 50-65°C. When the preparation product undergoes a heat storage experiment (54°C), Compound A undergoes a process of partially changing from a solid particle state to a molten liquid state. This characteristic poses certain challenges to the development of preparation products, especially when developing into solid preparation products, it is extremely easy to cause adhesion between the preparation powder or particles, generating dead particles that are difficult to disperse and disintegrate, resulting in the unqualified suspension rate of the preparation product. Summary of the Invention

[0003] The object of the present invention is to provide a preparation containing a biphenyl compound and its application.

[0004] To achieve the object of the present invention, the technical solution of the present invention is as follows:

[0005] A preparation containing a biphenyl compound, characterized in that: the preparation consists of active ingredient A, active ingredient B, at least one surfactant and at least one carrier, wherein the weight percentage content of the active ingredient is 0.1%-95%, and the mass ratio between active ingredient A and active ingredient B is 1:99-99:1. The structural formula of active ingredient A is as follows:

[0006]

[0007] Active ingredient B is selected from mitochondrial electron transport complex (II) inhibitors, allosteric modulators of nicotinic acetylcholine receptors, chloride channel agonists, mite growth inhibitors, acetyl-CoA carboxylase inhibitors, ATP synthase inhibitors, mitochondrial electron transport complex (I) inhibitors, mitochondrial electron transport complex (III) inhibitors, pyrethroids, insect growth regulators, organophosphates, nicotine-like compounds, feeding deterrents, nereistoxin analogs, ryanodine receptor modulators, voltage-dependent sodium channel blockers, GABA-gated chloride antagonists, microorganisms, isoxazoline insecticides and acaricides, or other insecticides and acaricides.

[0008] The dosage form of the preparation is emulsifiable concentrate, emulsion in water, microemulsion, suspoemulsion, seed treatment emulsion, suspension concentrate, seed treatment suspension concentrate, dispersible oil suspension, wettable powder, water dispersible granule or dry flowable.

[0009] When the preparation is a solid preparation, the surfactant contains a stabilizer, and the stabilizer accounts for 0.5%-5% of the mass of the preparation.

[0010] The surfactant is a stabilizer and one or several auxiliaries; the auxiliaries are wetting and dispersing agents, binders, disintegrants, defoamers.

[0011] The stabilizer is coconut oil and calcium stearate, and the ratio of coconut oil to calcium stearate is 2:1.

[0012] In the preparation by weight percentage, the active ingredient is 0.1%-95%, the wetting and dispersing agent is 1%-40%, the stabilizer is 0.5%-5%, the binder is 0-10%, the disintegrant is 0-10%, the defoamer is 0-10%, and the carrier is 1%-99%; the active ingredient is active ingredient A and active ingredient B, and the mass ratio between active ingredient A and active ingredient B is 1:50-50:1.

[0013] The active ingredient B is selected from cyetpyrafen, cyenopyrafen, cyflumetofen, avermectin, emamectin benzoate, spinosad, spinetoram, clofentezine, hexythiazox, etoxazole, flufenzine, spirodiclofen, spirotetramat, spiroacetamiprid, diafenthiuron, azocyclotin, propargite, pyridaben, fenpyroximate, pyrimidifen, pyrimidaben, flometoquin, hydramethylnon, pyflubumide, acynonapyr, chlorfenapyr, fluazinam, fenpropathrin, beta-cyfluthrin, lufenuron, hexaflumuron, tebufenozide, flonicamid, methoxyfenozide, chlorpyrifos, imidacloprid, thiamethoxam, pymetrozine, indoxacarb, chlorantraniliprole, butene-fipronil, veratrine, isoxazolinyl pyrrole carboxamide, flutriafol, afoxolaner, lotilaner, sarolaner, alphacypermethrin, quinoxyfen, Flipper TM (contact biopesticide / acaricide containing C7-C20 fatty acids), N-[[2-fluoro-4-[2-hydroxy-3-(3,4,5-trichlorophenyl)-3-(trifluoromethyl)pyrrolidin-1-yl]phenyl]methyl]cyclopropanecarboxamide or (S)-N-[[2-fluoro-4-[2-hydroxy-3-(3,4,5-trichlorophenyl)-3-(trifluoromethyl)pyrrolidin-1-yl]phenyl]methyl]cyclopropanecarboxamide.

[0014] The above active ingredient B can also be selected from Spidoxamat, Broflanilide, Nicofluprole, Cyflumetofen, 5-[[3-[3,5-bis(trifluoromethyl)phenyl]-2,2-dichloro-cyclopropanecarbonyl]amino]-2-chloro-N-[3-[(2,2-difluoroacetyl)amino]-2,4-difluoro-phenyl]benzamide, 5-[[(1R,3R)-3-[3,5-bis(trifluoromethyl)phenyl]-2,2-dichloro-cyclopropanecarbonyl]amino]-2-chloro-N-[3-[(2,2-difluoroacetyl)amino]-2,4-difluoro-phenyl]benzamide), 5-[[(1S,3S)-3-[3,5-bis(trifluoromethyl)phenyl]-2,2-dichloro-cyclopropanecarbonyl]amino]-2-chloro-N-[3-[(2,2-difluoroacetyl)amino]-2,4-difluoro-phenyl]benzamide), Tetrachlorantraniliprole, Afidopyropen, 4-dimethyl-2-[2-(3-pyridyl)indazol-5-yl]-1,2,4-triazolidine-3,5-dione, N-[3-chloro-1-(3-pyridyl)pyrazol-4-yl]-2-methylsulfonyl-propionamide, Tyclopyrazoflor, N-(1-methylcyclopropyl)-2-(3-pyridyl)indazole-4-carboxamide, Dimpropyridaz, Pyrifluquinazon, Fipronil, 3-(2-chlorothiazol-5-yl)-8-methyl-5-oxo-6-phenyl-2,3-dihydrothiazolo[3,2-a]pyrimidin-8-ium-7-olate, (3R)-3-(2-chlorothiazol-5-yl)-8-methyl-5-oxo-6-phenyl-2,3-dihydrothiazolo[3,2-a]pyrimidin-8-ium-7-olate, (3R)-3-(2-chlorothiazol-5-yl)-8-methyl-5-oxo-6-phenyl-2,3-dihydrothiazolo[3,2-a]pyrimidin-8-ium-7-olide (enol tautomer), (3R)-3-(2-chlorothiazol-5-yl)-8-methyl-5-oxo-6-phenyl-2,3-dihydrothiazolo[3,2-a]pyrimidin-8-ium-7-olate (diketone), Triflumezopyrim, 1-(2-cyanoethyl)-4-oxo-3-[3-(trifluoromethyl)phenyl]pyrido[1,2-a]pyrimidin-1-2--2-olate, Dichlorothripsidim, Flupyradifurone, Thiacloprid, Sulfoxaflor, Acetamiprid, Flupyrimin, Dinotefuran, Nitenpyram, Thiamethoxam, Tetramicramide, Flubendiamide, Cyantraniliprole, 5-bromo-2-(3-chloro-2-pyridyl)-N-[4,6-dichloro-3-fluoro-2-(methylcarbamoyl)phenyl]pyrazole-3-carboxamide, Cyclaniliprole, Chlorantraniliprole, 5-bromo-2-(3-chloro-2-pyridyl)-N-[2,4-dichloro-6-(isopropylaminothiocarbonyl)phenyl]pyrazole-3-carboxamide, 1-[6-(2,2-difluoro-7-methyl-[1,3]dioxoleno[4,5-f]benzimidazol-6-yl)-5-ethylsulfonyl-3-pyridyl]cyclopropanecarbonitrile, 6-(5-cyclopropyl-3-ethylsulfonyl-2-pyridyl)-2,2-difluoro-7-methyl-[1,3]dioxoleno[4,5-f]benzimidazole, 2-(5-cyclopropyl-3-ethylsulfonyl-2-pyridyl)-5-(trifluoromethylsulfonyl)-1,3-benzoxazole, 2-[3-ethylsulfonyl-5-(trifluoromethyl)pyrazolo[1,5-a]pyridin-2-yl]-3-methyl-6-(trifluoromethyl)imidazo[4,5-b]pyridine, 2-[3-ethylsulfonyl-6-(trifluoromethyl)pyrazolo[1,5-a]pyridin-2-yl]-3-methyl-6-(trifluoromethyl)imidazo[4,5-b]pyridine, 2-[3-ethylsulfonyl-6-(1,2,4-triazol-1-yl)-2-pyridyl]-3-methyl-6-(trifluoromethyl)imidazo[4,5-b]pyridine, 2-(3-ethylsulfonyl-2-pyridyl)-5-(2,2,3,3,3-pentafluoropropoxy)pyrazine, Oxazosulfyl, Benzpyrimoxan, metaflumizone, deltamethrin, bifenthrin, lambda-cyhalothrin, beta-cypermethrin, alpha-cypermethrin, fenvalerate, esfenvalerate, cyhalothrin, tefluthrin, (2Z)-2-[2-fluoro-4-methyl-5-(2,2,2-trifluoroethylsulfinyl)phenyl]imino-3-(2,2,2-trifluoroethyl)thiazolidin-4-one, (R)-(2Z)-2-[2-fluoro-4-methyl-5-(2,2,2-trifluoroethylsulfinyl)phenyl]imino-3-(2,2,2-trifluoroethyl)thiazolidin-4-one, 2-[2-fluoro-4-methyl-5-(2,2,2-trifluoroethylsulfinyl)phenyl]imino-3-(2,2,2-trifluoroethyl)thiazolidin-4-one, Flupentiofenox, Flufenerim, Fluhexafon, methoxyfenozide, Fluopyram, Fluazaindolizine, Guadipyr, 3,4,4-trifluorobut-3-en-1-yl 2-(2-methoxyphenyl)-5-oxotetrahydrofuran-3-carboxylate, Tioxazafen, Sarolaner and Tigolaner or a salt thereof.,

[0015] The emulsifiable concentrate comprises an active ingredient, a solvent and an emulsifier; by weight percentage, the active ingredient is 0.1-95%, the emulsifier is 1-30%, and the solvent is 1-98%;

[0016] The aqueous emulsion, microemulsion, and suspoemulsion include an active ingredient, a solvent, an emulsifier, an antifreeze agent, and a carrier; by weight percentage, the active ingredient is 0.1-95%, the solvent is 1-30%, the emulsifier is 1-30%, the antifreeze agent is 1-10%, and the carrier is 1-60%;

[0017] The seed treatment emulsion includes an active ingredient, a solvent, an emulsifier, an antifreeze agent, a carrier, and a warning colorant; by weight percentage, the active ingredient is 0.5-80%, the solvent is 1-30%, the emulsifier is 1-30%, the antifreeze agent is 1-10%, the carrier is 1-60%, and the warning colorant is 2-15%.

[0018] The solvent in the emulsifiable concentrate, aqueous emulsion, microemulsion, suspoemulsion, and seed treatment emulsion is: one or more of solvent oil, toluene, xylene, cyclohexanone, tributyl phosphate, methyl oleate, vegetable oil, dimethylformamide, acetonitrile, polyethylene glycol, methanol, ethanol, decanamide, butyrolactone, liquid paraffin, N-long chain alkyl pyrrolidone. Further optionally, the solvent is one or more of solvent oil, xylene, cyclohexanone, tributyl phosphate, methyl oleate, vegetable oil, dimethylformamide, decanamide, butyrolactone, liquid paraffin.

[0019] The emulsifier in the emulsifiable concentrate, aqueous emulsion, microemulsion, suspoemulsion, and seed treatment emulsion is: one or more of alkylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, polyoxyethylene fatty acid ester, polyoxyethylene sorbitan ester, polyoxyethylene-polyoxypropylene block copolymer, sorbitan fatty acid ester, calcium alkylbenzene sulfonate, ammonium styrene polyoxyethylene ether sulfate, phenethylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, alkylaryl phenol polyoxyethylene polyoxypropylene ether, sulfosuccinate; further optionally, the emulsifier in the emulsifiable concentrate is: one or more of sulfosuccinate, fatty alcohol polyoxyethylene ether, calcium alkylbenzene sulfonate, sorbitan fatty acid ester, castor oil polyoxyethylene ether, polyoxyethylene sorbitan. The emulsifier in the aqueous emulsion, microemulsion, suspoemulsion, and seed treatment emulsion is: one or more of alkylaryl phenol polyoxyethylene polyoxypropylene ether, sulfosuccinate, phenethylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, polyoxyethylene sorbitan ester, sorbitan fatty acid ester, polyoxyethylene-polyoxypropylene block copolymer, fatty alcohol polyoxyethylene ether.

[0020] The antifreeze agent in the aqueous emulsion, microemulsion, suspoemulsion, and seed treatment emulsion is: one or more of ethylene glycol, propylene glycol, glycerol, urea, diethylene glycol, isopropanol, ethylene glycol monobutyl ether, propylene glycol monobutyl ether, ethylene glycol monobutyl ether acetate, dimethyl sulfoxide, magnesium chloride, thiourea, calcium chloride, sodium acetate. Further optionally, the antifreeze agent is one or more of ethylene glycol, propylene glycol, glycerol, urea, dimethyl sulfoxide.

[0021] The carrier in the aqueous emulsion, microemulsion, suspoemulsion, and seed treatment emulsion is water.

[0022] The warning colorant in the seed treatment emulsion is one or more of dyes and pigments (including color powder and color paste).

[0023] The suspending agent and the dispersible oil suspending agent include an active ingredient, a wetting and dispersing agent, and a carrier; by weight percentage, the active ingredient is 0.1 - 95%, the wetting and dispersing agent is 1 - 30%, and the carrier is 1 - 99%;

[0024] The seed treatment suspending agent includes an active ingredient, a wetting and dispersing agent, an antifreeze agent, a carrier, a film-forming substance, and a warning colorant; by weight percentage, the active ingredient is 0.5 - 80%, the wetting and dispersing agent is 1 - 25%, the antifreeze agent is 1 - 10%, the carrier is 1 - 60%, the film-forming substance is 1 - 15%, and the warning colorant is 2 - 15%;

[0025] The wetting and dispersing agent in the suspending agent and the seed treatment suspending agent is one or more of polycarboxylate, alkylphenol polyoxyethylene ether, polyoxyethylene polyoxypropylene block copolymer, lignosulfonate, sulfate, phosphate ester salt, succinate ester salt, alkylnaphthalenesulfonate, fatty alcohol polyoxyethylene ether, sorbitan fatty acid ester polyoxyethylene ether, and polyvinyl alcohol monooleate. Further optionally, the wetting and dispersing agent in the suspending agent and the seed treatment suspending agent is one or more of polycarboxylate, polyoxyethylene polyoxypropylene block copolymer, lignosulfonate, succinate ester salt, alkylnaphthalenesulfonate, fatty alcohol polyoxyethylene ether, and sorbitan fatty acid ester polyoxyethylene ether.

[0026] The wetting and dispersing agent of the dispersible oil suspending agent is one or more of carboxylate, polyacrylate, naphthalenesulfonate, lignosulfonate, sulfate, sulfosuccinate, sorbitan fatty acid ester polyoxyethylene ether, castor oil polyoxyethylene ether, ethylene oxide-propylene oxide block copolymer, alkylbenzene sulfonate, phenethylphenol polyoxyethylene polyoxypropylene ether and formaldehyde condensate, and fatty alcohol polyoxyethylene ether. Further optionally, the wetting and dispersing agent of the dispersible oil suspending agent is one or more of carboxylate, polyacrylate, lignosulfonate, sorbitan fatty acid ester polyoxyethylene ether, castor oil polyoxyethylene ether, ethylene oxide-propylene oxide block copolymer, alkylbenzene sulfonate, and fatty alcohol polyoxyethylene ether.

[0027] The dispersion medium of the suspending agent and the seed treatment suspending agent is water.

[0028] The dispersion medium of the dispersible oil suspension is one or more of solvent oil, xylene, vegetable oil, methanol, methyl oleate, decanamide, dimethylformamide, butyrolactone, tributyl phosphate, and liquid paraffin. Further optionally, the dispersion medium of the dispersible oil suspension is one or more of solvent oil, vegetable oil, methanol, methyl oleate, decanamide, butyrolactone, tributyl phosphate, and liquid paraffin.

[0029] The wettable powder, water dispersible granule, and dry suspension include active ingredients, wetting and dispersing agents, binders, disintegrants, defoamers, stabilizers, and carriers; by weight percentage, the active ingredients are 0.1% - 95%, the wetting and dispersing agents are 1% - 40%, the stabilizers are 0.5% - 5%, the binders are 0 - 10%, the disintegrants are 0 - 10%, the defoamers are 0 - 10%, and the carriers are 1% - 99%.

[0030] The wetting and dispersing agents in the wettable powder, water dispersible granule, and dry suspension are one or more of sodium alkylphenol polyoxyethylene ether sulfate, fatty alcohol sulfate, sodium alkyl alcohol polyoxyethylene ether sulfate, sodium alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, alkyl naphthalene sulfonate, sodium alkyl sulfate, sulfonate of fatty alcohol ethylene oxide adduct, sulfonate of alkylphenol formaldehyde condensate ethylene oxide adduct, fatty alcohol polyoxyethylene ether, alkylamide sulfonate, sorbitan fatty acid ester, alkylphenol polyoxyethylene ether, sorbitan fatty acid ester polyoxyethylene agent ether, alkylphenol formaldehyde condensate polyoxyethylene ether, polyoxyethylene sorbitan ester, sulfonate of fatty alcohol ethylene oxide adduct, polyoxyethylene fatty acid ester, alkylphenol polyoxyethylene ether sulfonate, polycarboxylate, alkylphenol polyoxyethylene phosphate, polyoxyethylene polyoxypropylene ether block copolymer, lignosulfonate, sodium polyacrylate, polyvinylpyrrolidone, sulfonates, sulfates, carboxylates, succinate esters, phosphate esters, fatty amine polyoxyethylene ether, fatty acid polyoxyethylene ether, sodium alkyl naphthalene sulfonate fatty alcohol polyoxyethylene ether, and monooleate of polyvinyl alcohol;

[0031] Further optionally, the wetting and dispersing agents in the wettable powder include one or more of alkylphenol polyoxyethylene ether, fatty alcohol sulfate, sulfonate of fatty alcohol ethylene oxide adduct, sodium alkyl alcohol polyoxyethylene ether sulfate, sodium alkyl sulfate, alkyl naphthalene sulfonate, fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, polyoxyethylene polyoxypropylene ether block copolymer, polycarboxylate, lignosulfonate, and carboxylate.

[0032] Further optionally, the wetting and dispersing agents in the water dispersible granule are one or more of polycarboxylate, polyoxyethylene polyoxypropylene ether block copolymer, lignosulfonate, sulfate, and carboxylate.

[0033] Further optionally, the wetting and dispersing agent in the dry flowable agent is one or more of alkylphenol polyoxyethylene phosphate, polycarboxylate, ether formaldehyde condensate sulfate, lignosulfonate, polyoxyethylene polyoxypropylene ether block copolymer, polyvinylpyrrolidone, sodium polyacrylate, carboxylates, sulfonates, phosphate esters.

[0034] The carriers in the wettable powder, water dispersible granule and dry flowable agent are one or more of clay, diatomite, rock powder, chalk, montmorillonite, quartz, clay, sodium sulfate, silica, pumice, light calcium carbonate, gypsum, talc, bentonite, kaolin, starch, soluble starch, attapulgite, pottery clay, montmorillonite, benzofuran resin, magnesium aluminum silicate, activated clay, white carbon black, superphosphate, ammonium sulfate, alumina, pumice, calcite, marble, etc.

[0035] Further optionally, the carrier is one or more of clay, diatomite, rock powder, bentonite, attapulgite, kaolin, light calcium carbonate, activated clay, montmorillonite, white carbon black.

[0036] The binder can be one or more of gelatin, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol, dextrin.

[0037] The disintegrant can be one or more of calcium chloride, anhydrous sodium sulfate, sodium chloride, sodium carboxymethyl cellulose, soluble starch, bentonite, ethyl polyacrylate.

[0038] The defoaming agent can be one or more of defoaming agent SAG1522, silicone, phosphate ester, C8 - 10 fatty alcohol, C10 - 20 saturated fatty acids (such as capric acid) and amides or others.

[0039] An application of the preparation containing biphenyl compounds as described above, and the preparation can be applied to the control of agricultural pests and mites, forestry pests and mites or non - therapeutic hygienic pests and mites.

[0040] Compared with the prior art, the present invention has the following advantages:

[0041] 1. By developing the above - mentioned different active ingredient compositions (active ingredient A, active ingredient B) into preparations of different dosage forms, the present invention overcomes the defects that when the active ingredients are formulated into a simple preparation (i.e., a similar solution agent), it can only be prepared and used immediately, with a large amount of solvents and auxiliaries used and instability during long - term storage. According to the actual scenarios of agricultural operations, specific target pests and application methods, the active ingredients are formulated into preparations of different dosage forms, and a matching auxiliary system is screened, which improves the stability of the preparation dilution over time, facilitates spraying application, improves the wetting, spreading, retention and other properties of the active ingredients on the target crops, can improve the utilization rate of the effective ingredients of pesticides, effectively control pests and diseases, and reduce production costs.

[0042] 2. By adding stabilizers coconut oil and calcium stearate to wettable powders, water dispersible granules, and dry suspension concentrates, the present invention improves the problem that the suspension rate of wettable powders, water dispersible granules, and dry suspension concentrates is poor or even unqualified after thermal storage. Coconut oil is mainly applied in the food, cosmetics, and detergent industries, and calcium stearate is mainly used as a waterproofing agent, lubricant, and plastic additive. In the present invention, applying them to solid pesticide formulations has achieved an unexpected effect of improving suspension stability.

[0043] 3. By using the compounding of different active ingredients in the formulations of the present invention, compared with using single-active-ingredient formulations, the occurrence and development of target crop resistance can be delayed, and at the same time, the control spectrum can be expanded to control various crop diseases. Detailed implementation mode

[0044] To better understand the essence of the present invention, the content of the present invention will be further described in detail below in conjunction with examples. The content mentioned in the examples is not a limitation to the present invention. The following is only used to explain the present invention. Modifications, substitutions, or improvements made without departing from the spirit and principles of the present invention all fall within the scope of protection required by the present invention.

[0045] Formulation examples of the preparation

[0046] 1. Preparation of emulsifiable concentrates

[0047] Example 1. Preparation of 18% Compound A·cyenopyraf emulsifiable concentrate

[0048] According to the formulation requirements, 12% of Compound A, 6% of cyenopyraf, 5% of 0203B, 3% of Atlox 4838B, 5% of cyclohexanone, and solvent oil S-150 are added to a mixing kettle to make up 100%, and stirred and mixed evenly. If necessary, it is heated and dissolved in a hot water bath to obtain 18% Compound A·cyenopyraf emulsifiable concentrate.

[0049] Example 2. Preparation of 30% Compound A·spinosad emulsifiable concentrate

[0050] According to the formulation requirements, 10% of Compound A, 20% of spinosad, 10% of SK-51EC, 5% of SK-50EC, 10% of dimethylformamide, and solvent oil S-200 are added to a mixing kettle to make up 100%, and stirred and mixed evenly. If necessary, it is heated and dissolved in a hot water bath to obtain 30% Compound A·spinosad emulsifiable concentrate.

[0051] Example 3. Preparation of 40% Compound A·spirodiclofen emulsifiable concentrate

[0052] According to the formulation requirements, 30% of compound A, 10% of spirodiclofen, 8% of AEO-3, 7% of agricultural emulsifier 1601, 5% of butyrolactone, and solvent oil S-150 are added to a mixing kettle to make up 100%. Stir and mix evenly. If necessary, heat and dissolve with a hot water bath to obtain 40% compound A·spirodiclofen emulsifiable concentrate.

[0053] Example 4. Preparation of 55% compound A·fenpropathrin emulsifiable concentrate

[0054] According to the formulation requirements, 30% of compound A, 25% of fenpropathrin, 3% of 500#, 12% of 0201B, 5% of dimethylformamide, 10% of cyclohexanone, and solvent oil S-200 are added to a mixing kettle to make up 100%. Stir and mix evenly. If necessary, heat and dissolve with a hot water bath to obtain 55% compound A·fenpropathrin emulsifiable concentrate.

[0055] 2. Preparation of aqueous emulsion

[0056] Example 5. Preparation of 14% compound A·abamectin aqueous emulsion

[0057] According to the formulation requirements, 12% of compound A, 2% of abamectin, 3% of YusD3020, 1% of SK-560EP, 3% of 500#, and 20% of solvent oil S150 are added to a mixing kettle, stirred and mixed to dissolve into a homogeneous oil phase. Under high-speed shearing, 5% of ethylene glycol and deionized water (to make up 100%) are added to the oil phase and sheared to an appropriate particle size to obtain 14% compound A·abamectin aqueous emulsion.

[0058] Example 6. Preparation of 18% compound A·etoxazole aqueous emulsion

[0059] According to the formulation requirements, 12% of compound A, 6% of etoxazole, 3% of EL-40, 2% of agricultural emulsifier 1601, 2% of EF-68, and 30% of solvent oil S200 are added to a mixing kettle, stirred and mixed to dissolve into a homogeneous oil phase. Under high-speed shearing, 5% of glycerol and deionized water (to make up 100%) are added to the oil phase and sheared to an appropriate particle size to obtain 18% compound A·etoxazole aqueous emulsion.

[0060] Example 7. Preparation of 30% compound A·spirotetramat aqueous emulsion

[0061] According to the formulation requirements, 6% of compound A, 24% of spirotetramat, 2% of DOWFAX D800, 1.5% of Atlox 4916, 3% of EL-360, and 30% of methyl oleate are added to a mixing kettle, stirred and mixed to dissolve into a homogeneous oil phase. Under high-speed shearing, 5% of ethylene glycol and deionized water (to make up 100%) are added to the oil phase and sheared to an appropriate particle size to obtain 30% compound A·spirotetramat aqueous emulsion.

[0062] Example 8. Preparation of 40% Compound A·Ethoxazole Acaricide Emulsion in Water

[0063] According to the formulation requirements, add 20% of Compound A, 20% of Ethoxazole Acaricide, 2% of YusD3020, 2% of 500#, 2% of SK560EP, and 25% of Solvent Oil S150 into the mixing kettle, stir and mix to dissolve into a uniform oil phase. Under high-speed shearing, add 5% of glycerol and the balance deionized water (to make up to 100%) into the oil phase, and shear to an appropriate particle size to obtain 40% Compound A·Ethoxazole Acaricide Emulsion in Water.

[0064] Example 9. Preparation of 20% Compound A·Ethoxazole Acaricide Emulsion in Water

[0065] According to the formulation requirements, add 10% of Compound A, 10% of Ethoxazole Acaricide, 2% of Dowfax D800, 2% of Yus110, 1% of 1601, and 20% of Solvent Oil S150 into the mixing kettle, stir and mix to dissolve into a uniform oil phase. Under high-speed shearing, add 5% of glycerol and the balance deionized water (to make up to 100%) into the oil phase, and shear to an appropriate particle size to obtain 20% Compound A·Ethoxazole Acaricide Emulsion in Water.

[0066] 3. Preparation of Microemulsion

[0067] Example 10. Preparation of 18% Compound A·Azocyclotin Microemulsion

[0068] According to the formulation requirements, add 12% of Compound A, 6% of Azocyclotin, 8% of Agricultural Emulsifier 1601, 3% of G5002L, 2% of SK-25CH, 5% of ADMA810, 5% of glycerol, 10% of deionized water, and the balance Solvent Oil S150 (to make up to 100%) into the mixing kettle, stir and mix to dissolve into a homogeneous transparent liquid to obtain 18% Compound A·Azocyclotin Microemulsion.

[0069] Example 11. Preparation of 30% Compound A·Bifenazate Microemulsion

[0070] According to the formulation requirements, add 25% of Compound A, 5% of Bifenazate, 5% of 0201B, 3% of Yus5050PB, 3% of Agricultural Emulsifier 1602, 10% of dimethylformamide, 10% of deionized water, 5% of ethylene glycol, and the balance Solvent Oil S200 (to make up to 100%) into the mixing kettle, stir and mix to dissolve into a homogeneous transparent liquid to obtain 30% Compound A·Bifenazate Microemulsion.

[0071] 4. Preparation of Suspension Concentrate

[0072] Example 12. Preparation of 20% Compound A·Fluazinam Suspension Concentrate

[0073] According to the formulation requirements, add 5% of compound A, 15% of fluazinam, 2% of Tergitol W-600, 4% of Dowfax D800, 1% of magnesium aluminum silicate, 0.2% of xanthan gum, 5% of glycerol, and the balance of deionized water (to make up to 100%) into a high-shear mixing kettle. After shear mixing, use a sand mill to grind it to a moderate particle size, and then a 20% suspension concentrate of compound A·fluazinam can be obtained.

[0074] Preparation of 3.55% suspension concentrate of compound A·tebufenozide in Example

[0075] According to the formulation requirements, add 30% of compound A, 25% of tebufenozide, 2% of Duramax D-305, 3% of NNO, 1% of magnesium aluminum silicate, 0.14% of xanthan gum, 5% of ethylene glycol, and the balance of deionized water (to make up to 100%) into a high-shear mixing kettle. After shear mixing, use a sand mill to grind it to a moderate particle size, and then a 55% suspension concentrate of compound A·tebufenozide can be obtained.

[0076] Preparation of 40% suspension concentrate of compound A·imidacloprid in Example

[0077] According to the formulation requirements, add 8% of compound A, 32% of imidacloprid, 2% of Morwet D-500, 4% of Agrilan 755, 0.8% of magnesium aluminum silicate, 0.2% of xanthan gum, 5% of ethylene glycol, and the balance of deionized water (to make up to 100%) into a high-shear mixing kettle. After shear mixing, use a sand mill to grind it to a moderate particle size, and then a 40% suspension concentrate of compound A·imidacloprid can be obtained.

[0078] Preparation of 15% suspension concentrate of compound A·thiamethoxam in Example

[0079] According to the formulation requirements, add 10% of compound A, 5% of thiamethoxam, 2% of Morwet EFW, 3% of Morwet D-425, 1.5% of magnesium aluminum silicate, 0.16% of xanthan gum, 5% of ethylene glycol, and the balance of deionized water (to make up to 100%) into a high-shear mixing kettle. After shear mixing, use a sand mill to grind it to a moderate particle size, and then a 15% suspension concentrate of compound A·thiamethoxam can be obtained.

[0080] Preparation of 18% suspension concentrate of compound A·etoxazole in Example

[0081] According to the formulation requirements, add 12% of Compound A, 6% of etoxazole, 2% of Dowfax D800, 5% of SK34SC, 1% of magnesium aluminum silicate, 0.16% of xanthan gum, 5% of propylene glycol, and the balance of deionized water (made up to 100%) into a high-shear mixing kettle. After shear mixing and grinding with a sand mill to an appropriate particle size, an 18% Compound A·etoxazole suspension is obtained.

[0082] Example 17. Preparation of 14% Compound A·abamectin suspension

[0083] According to the formulation requirements, add 12% of Compound A, 2% of abamectin, 2% of SPSC3, 3% of SP2728, 1% of magnesium aluminum silicate, 0.6% of white carbon black, 5% of ethylene glycol, and the balance of deionized water (made up to 100%) into a high-shear mixing kettle. After shear mixing and grinding with a sand mill to an appropriate particle size, a 14% Compound A·abamectin suspension is obtained.

[0084] Example 18. Preparation of 20% Compound A·cyazofamid suspension

[0085] According to the formulation requirements, add 10% of Compound A, 10% of cyazofamid, 2% of SK24, 3% of SP27001, 1% of magnesium aluminum silicate, 0.12% of xanthan gum, 5% of ethylene glycol, and the balance of deionized water (made up to 100%) into a high-shear mixing kettle. After shear mixing and grinding with a sand mill to an appropriate particle size, a 20% Compound A·cyazofamid suspension is obtained.

[0086] Example 19. Preparation of 24% Compound A·etoxazole suspension

[0087] According to the formulation requirements, add 16% of Compound A, 8% of etoxazole, 2% of Atlox 4913, 4% of SK33SC, 1% of magnesium aluminum silicate, 0.1% of xanthan gum, 5% of propylene glycol, and the balance of deionized water (made up to 100%) into a high-shear mixing kettle. After shear mixing and grinding with a sand mill to an appropriate particle size, a 24% Compound A·etoxazole suspension is obtained.

[0088] Example 20. Preparation of 40% Compound A·bifenazate suspension

[0089] According to the formulation requirements, add 20% of Compound A, 20% of bifenazate, 2% of Atlox 4917, 4% of Termul 2500, 1.5% of magnesium aluminum silicate, 0.16% of xanthan gum, 5% of ethylene glycol, and the balance of deionized water (made up to 100%) into a high-shear mixing kettle. After shear mixing and grinding with a sand mill to an appropriate particle size, a 40% Compound A·bifenazate suspension can be obtained.

[0090] Example 2. Preparation of 30% Compound A·Spiromesifen Suspension Concentrate

[0091] According to the formulation requirements, 20% of Compound A, 10% of spiromesifen, 2% of SP2728, 3% of SK20TX, 1% of magnesium aluminum silicate, 0.6% of silica white, 5% of ethylene glycol, and the balance of deionized water (made up to 100%) were added to a high-shear mixing kettle. After shear mixing and grinding with a sand mill to an appropriate particle size, 30% Compound A·Spiromesifen Suspension Concentrate was obtained.

[0092] 5. Preparation of Suspension Emulsion Concentrate

[0093] Example 22. Preparation of 18% Compound A·Pymetrozine Suspension Emulsion Concentrate

[0094] According to the formulation requirements, 12% of Compound A, 6% of pymetrozine, 1% of YusD3020, 4% of Morwet D-425, 10% of methyl oleate, 5% of 0201B, 0.14% of xanthan gum, 5% of glycerol, 3% of silica white, and the balance of deionized water (made up to 100%) were added to a mixing kettle. After mixing and stirring with a high-shear mixer and then grinding with a sand mill to an appropriate particle size, 18% Compound A·Pymetrozine Suspension Emulsion Concentrate was obtained.

[0095] 6. Preparation of Dispersible Oil Suspension Concentrate

[0096] Example 23. Preparation of 18% Compound A·Indoxacarb Dispersible Oil Suspension Concentrate

[0097] According to the formulation requirements, 12% of Compound A, 6% of indoxacarb, 6% of Atlox 4912, 3% of Atlox 4838B, 4% of T-80, 1% of organic bentonite, and the balance of methyl oleate (made up to 100%) were added to a mixing kettle. After stirring and mixing with a high-shear mixer and grinding with a sand mill to an appropriate particle size, 18% Compound A·Indoxacarb Dispersible Oil Suspension Concentrate was obtained.

[0098] Example 24. Preparation of 30% Compound A·Chlorantraniliprole Dispersible Oil Suspension Concentrate

[0099] According to the formulation requirements, 20% of Compound A, 10% of chlorantraniliprole, 4% of Atlox 4914, 10% of SK25CH, 1.2% of organic bentonite, and the balance of methyl oleate (made up to 100%) were added to a mixing kettle. After stirring and mixing with a high-shear mixer and grinding with a sand mill to an appropriate particle size, 30% Compound A·Chlorantraniliprole Dispersible Oil Suspension Concentrate was obtained.

[0100] 7. Seed Treatment Suspension Concentrate

[0101] Example 25. Preparation of 18% Compound A · Isoxazoline Insecticide Seed Treatment Suspension

[0102] According to the formula requirements, add 12% of Compound A, 6% of Isoxazoline Insecticide, 2% of SK34SC, 4% of SK20TX, 1.0% of Magnesium Aluminum Silicate, 0.16% of Xanthan Gum, 5% of Ethylene Glycol, and the balance of deionized water (made up to 100%) into a high-shear mixing kettle. After shearing and mixing, use a sand mill to grind to a moderate particle size, and add 8% of Red131 and 10% of FmA002 through stirring and mixing to obtain 18% Compound A · Isoxazoline Insecticide Seed Treatment Suspension.

[0103] 8. Seed Treatment Emulsion

[0104] Example 26. Preparation of 18% Compound A · Butene Fipronil Seed Treatment Emulsion

[0105] According to the formula requirements, add 12% of Compound A, 6% of Butene Fipronil, 8% of Agricultural Emulsifier 1602, 3% of YusD3020, 2% of SK-25CH, 5% of Glycerol, 30% of Solvent Oil S150, 8% of Red131, and the balance of deionized water (made up to 100%) into a mixing kettle, stir and mix to dissolve into a uniform and transparent liquid to obtain 18% Compound A · Butene Fipronil Microemulsion.

[0106] 9. Preparation of Wettable Powder

[0107] Example 27. Preparation of 30% Compound A · Fluxapyroxad Wettable Powder

[0108] According to the formula requirements, add 20% of Compound A, 10% of Fluxapyroxad, 1% of Coconut Oil, 0.5% of Calcium Stearate, 5% of SK24N, 3% of Morwet D-425, 2% of White Carbon Black, and the balance of Light Calcium Carbonate (made up to 100%) into a mixer for mixing, and then crush through a jet mill to obtain 30% Compound A · Fluxapyroxad Wettable Powder.

[0109] Example 28. Preparation of 40% Compound A · Permethrin Wettable Powder

[0110] According to the formula requirements, add 20% of Compound A, 20% of Permethrin, 1.5% of Coconut Oil, 0.75% of Calcium Stearate, 3% of NNO, 2% of Dispersol CBZ, 1.5% of Sodium Lauryl Sulfate, 4% of Kaolin, and the balance of Light Calcium Carbonate (made up to 100%) into a mixer for mixing, and then crush through a jet mill to obtain 40% Compound A · Permethrin Wettable Powder.

[0111] Preparation of 29.14% Compound A·Abamectin Wettable Powder

[0112] According to the formulation requirements, 12% of Compound A, 2% of abamectin, 0.5% of coconut oil, 0.25% of calcium stearate, 3% of Yus-RXB, 4% of Morwet D-425, 2% of white carbon black, and the balance of light calcium carbonate (to make up 100%) are added to a mixer for mixing, and then pulverized by a jet mill to obtain 14% Compound A·Abamectin wettable powder.

[0113] Preparation of 30.18% Compound A·Etoxazole Wettable Powder

[0114] According to the formulation requirements, 12% of Compound A, 6% of etoxazole, 0.8% of coconut oil, 0.4% of calcium stearate, 45% of Yus-WG, 3% of Yus-SXC, 2% of montmorillonite, and the balance of light calcium carbonate (to make up 100%) are added to a mixer for mixing, and then pulverized by a jet mill to obtain 18% Compound A·Etoxazole wettable powder.

[0115] Preparation of 31.20% Compound A·Ethiprole Wettable Powder

[0116] According to the formulation requirements, 10% of Compound A, 10% of ethiprole, 1% of coconut oil, 0.5% of calcium stearate, 5% of SK24N, 3% of Yus-SXC, 2% of white carbon black, and the balance of light calcium carbonate (to make up 100%) are added to a mixer for mixing, and then pulverized by a jet mill to obtain 20% Compound A·Ethiprole wettable powder.

[0117] Comparative Example 1. Preparation of 30% Compound A·Fluxapyroxad Wettable Powder

[0118] According to the formulation requirements, 20% of Compound A, 10% of fluxapyroxad, 1% of coconut oil, 5% of SK24N, 3% of Morwet D-425, 2% of white carbon black, and the balance of light calcium carbonate (to make up 100%) are added to a mixer for mixing, and then pulverized by a jet mill to obtain 30% Compound A·Fluxapyroxad wettable powder.

[0119] Comparative Example 2. Preparation of 30% Compound A·Fluxapyroxad Wettable Powder

[0120] According to the formulation requirements, 20% of Compound A, 10% of fluxapyroxad, 0.5% of calcium stearate, 5% of SK24N, 3% of Morwet D-425, 2% of white carbon black, and the balance of light calcium carbonate (to make up 100%) are added to a mixer for mixing, and then pulverized by a jet mill to obtain 30% Compound A·Fluxapyroxad wettable powder.

[0121] Comparative Example 3. Preparation of 30% Compound A · Fluxapyroxad Wettable Powder

[0122] According to the formulation requirements, 20% of Compound A, 10% of fluxapyroxad, 5% of SK24N, 3% of Morwet D-425, 2% of silica white, and the balance of light calcium carbonate (made up to 100%) were added to a mixer for mixing, and then pulverized by a jet mill to obtain 30% Compound A · Fluxapyroxad Wettable Powder.

[0123] Comparative Example 4. Preparation of 40% Compound A · Permethrin Wettable Powder

[0124] According to the formulation requirements, 20% of Compound A, 20% of permethrin, 1.5% of coconut oil, 3% of NNO, 2% of Dispersol CBZ, 1.5% of sodium dodecyl sulfate, 4% of kaolin, and the balance of light calcium carbonate (made up to 100%) were added to a mixer for mixing, and then pulverized by a jet mill to obtain 40% Compound A · Permethrin Wettable Powder.

[0125] Comparative Example 5. Preparation of 40% Compound A · Permethrin Wettable Powder

[0126] According to the formulation requirements, 20% of Compound A, 20% of permethrin, 0.75% of calcium stearate, 3% of NNO, 2% of Dispersol CBZ, 1.5% of sodium dodecyl sulfate, 4% of kaolin, and the balance of light calcium carbonate (made up to 100%) were added to a mixer for mixing, and then pulverized by a jet mill to obtain 40% Compound A · Permethrin Wettable Powder.

[0127] Comparative Example 6. Preparation of 40% Compound A · Permethrin Wettable Powder

[0128] According to the formulation requirements, 20% of Compound A, 20% of permethrin, 3% of NNO, 2% of Dispersol CBZ, 1.5% of sodium dodecyl sulfate, 4% of kaolin, and the balance of light calcium carbonate (made up to 100%) were added to a mixer for mixing, and then pulverized by a jet mill to obtain 40% Compound A · Permethrin Wettable Powder.

[0129] Comparative Example 7. Preparation of 14% Compound A · Avermectin Wettable Powder

[0130] According to the formulation requirements, add 12% of Compound A, 2% of abamectin, 0.5% of coconut oil, 3% of Yus-RXB, 4% of Morwet D-425, 2% of silica white, and the balance of light calcium carbonate (to make up to 100%) into a mixer for mixing, and then crush it with a jet mill to obtain 14% Compound A·abamectin wettable powder.

[0131] Comparative Example 8. Preparation of 14% Compound A·abamectin wettable powder

[0132] According to the formulation requirements, add 12% of Compound A, 2% of abamectin, 0.25% of calcium stearate, 3% of Yus-RXB, 4% of Morwet D-425, 2% of silica white, and the balance of light calcium carbonate (to make up to 100%) into a mixer for mixing, and then crush it with a jet mill to obtain 14% Compound A·abamectin wettable powder.

[0133] Comparative Example 9. Preparation of 14% Compound A·abamectin wettable powder

[0134] According to the formulation requirements, add 12% of Compound A, 2% of abamectin, 3% of Yus-RXB, 4% of Morwet D-425, 2% of silica white, and the balance of light calcium carbonate (to make up to 100%) into a mixer for mixing, and then crush it with a jet mill to obtain 14% Compound A·abamectin wettable powder.

[0135] Comparative Example 10. Preparation of 18% Compound A·etoxazole wettable powder

[0136] According to the formulation requirements, add 12% of Compound A, 6% of etoxazole, 0.8% of coconut oil, 5% of Yus-WG4, 3% of Yus-SXC, 2% of montmorillonite, and the balance of light calcium carbonate (to make up to 100%) into a mixer for mixing, and then crush it with a jet mill to obtain 18% Compound A·etoxazole wettable powder.

[0137] Comparative Example 11. Preparation of 18% Compound A·etoxazole wettable powder

[0138] According to the formulation requirements, add 12% of Compound A, 6% of etoxazole, 0.4% of calcium stearate, 5% of Yus-WG4, 3% of Yus-SXC, 2% of montmorillonite, and the balance of light calcium carbonate (to make up to 100%) into a mixer for mixing, and then crush it with a jet mill to obtain 18% Compound A·etoxazole wettable powder.

[0139] Comparative Example 12. Preparation of 18% Compound A·etoxazole wettable powder

[0140] According to the formulation requirements, add 12% of Compound A, 6% of etoxazole, 5% of Yus-WG4, 3% of Yus-SXC, 2% of montmorillonite, and the balance of light calcium carbonate (to make up to 100%) into a mixer for mixing, and then crush it with a jet mill to obtain 18% Compound A·etoxazole wettable powder.

[0141] Preparation of 20% Compound A·cyazofamid wettable powder in Comparative Example 13

[0142] According to the formulation requirements, add 10% of Compound A, 10% of cyazofamid, 1% of coconut oil, 5% of SK24N, 3% of Yus-SXC, 2% of silica white, and the balance of light calcium carbonate (to make up to 100%) into a mixer for mixing, and then crush it with a jet mill to obtain 20% Compound A·cyazofamid wettable powder.

[0143] Preparation of 20% Compound A·cyazofamid wettable powder in Comparative Example 14

[0144] According to the formulation requirements, add 10% of Compound A, 10% of cyazofamid, 0.5% of calcium stearate, 5% of SK24N, 3% of Yus-SXC, 2% of silica white, and the balance of light calcium carbonate (to make up to 100%) into a mixer for mixing, and then crush it with a jet mill to obtain 20% Compound A·cyazofamid wettable powder.

[0145] Preparation of 20% Compound A·cyazofamid wettable powder in Comparative Example 15

[0146] According to the formulation requirements, add 10% of Compound A, 10% of cyazofamid, 5% of SK24N, 3% of Yus-SXC, 2% of silica white, and the balance of light calcium carbonate (to make up to 100%) into a mixer for mixing, and then crush it with a jet mill to obtain 20% Compound A·cyazofamid wettable powder.

[0147] 10. Preparation of water dispersible granules

[0148] Preparation of 18% Compound A·fenazaquin water dispersible granules in Example 32

[0149] According to the formulation requirements, add 12% of Compound A, 6% of fenazaquin, 0.5% of coconut oil, 0.25% of calcium stearate, 2% of Morwet EFW, 8% of SK24, 2% of carboxymethyl cellulose, 5% of kaolin, and ammonium sulfate to make up to 100%. Mix them evenly, crush them with a jet mill to obtain mother powder, then add appropriate amount of water for mixing, and granulate with an extrusion granulator to obtain 18% Compound A·fenazaquin water dispersible granules.

[0150] Preparation of 50% Compound A·afoxolaner Water Dispersible Granules in Example 3

[0151] According to the formulation requirements, 8% of Compound A, 42% of afoxolaner, 2.5% of coconut oil, 1.25% of calcium stearate, 2% of Morwet EFW, 10% of SK24N, 15% of kaolin, and ammonium sulfate are added to make up to 100%. Mix them evenly, grind them into mother powder by a jet mill, then add an appropriate amount of water for mixing, and granulate with an extrusion granulator to obtain 50% Compound A·afoxolaner water dispersible granules.

[0152] Preparation of 14% Compound A·avermectin Water Dispersible Granules in Example 34

[0153] According to the formulation requirements, 12% of Compound A, 2% of avermectin, 0.5% of coconut oil, 0.25% of calcium stearate, 2% of Yus-SXC, 10% of DF101, 15% of kaolin, and ammonium sulfate are added to make up to 100%. Mix them evenly, grind them into mother powder by a jet mill, then add an appropriate amount of water for mixing, and granulate with an extrusion granulator to obtain 14% Compound A·avermectin water dispersible granules.

[0154] Preparation of 18% Compound A·etoxazole Water Dispersible Granules in Example 35

[0155] According to the formulation requirements, 12% of Compound A, 6% of etoxazole, 1% of coconut oil, 0.5% of calcium stearate, 3% of Yus-SXC, 8% of YusWG4, 2% of carboxymethyl cellulose, 4% of kaolin, and ammonium sulfate are added to make up to 100%. Mix them evenly, grind them into mother powder by a jet mill, then add an appropriate amount of water for mixing, and granulate with an extrusion granulator to obtain 18% Compound A·etoxazole water dispersible granules.

[0156] Preparation of 20% Compound A·cyazofamid Water Dispersible Granules in Example 36

[0157] According to the formulation requirements, 10% of Compound A, 10% of cyazofamid, 0.8% of coconut oil, 0.4% of calcium stearate, 2% of Yus-SXC, 10% of Yus-RXB, 10% of kaolin, and ammonium sulfate are added to make up to 100%. Mix them evenly, grind them into mother powder by a jet mill, then add an appropriate amount of water for mixing, and granulate with an extrusion granulator to obtain 20% Compound A·cyazofamid water dispersible granules.

[0158] Preparation of 16% Compound A·fenazaquin Water Dispersible Granules in Comparative Example 1

[0159] According to the formulation requirements, take 12% of Compound A, 6% of fenazaquin, 0.5% of coconut oil, 2% of Morwet EFW, 248% of SK24, 2% of carboxymethyl cellulose, 5% of kaolin, and make up to 100% with ammonium sulfate. Mix them evenly, grind them into mother powder by a jet mill, then add an appropriate amount of water for mixing, and granulate with an extrusion granulator to obtain 18% Compound A·fenazaquin water dispersible granules.

[0160] Formulation of 18% Compound A·fenazaquin water dispersible granules in Comparative Example 17

[0161] According to the formulation requirements, take 12% of Compound A, 6% of fenazaquin, 0.25% of calcium stearate, 2% of Morwet EFW, 248% of SK24, 2% of carboxymethyl cellulose, 5% of kaolin, and make up to 100% with ammonium sulfate. Mix them evenly, grind them into mother powder by a jet mill, then add an appropriate amount of water for mixing, and granulate with an extrusion granulator to obtain 18% Compound A·fenazaquin water dispersible granules.

[0162] Formulation of 18% Compound A·fenazaquin water dispersible granules in Comparative Example 18

[0163] According to the formulation requirements, take 12% of Compound A, 6% of fenazaquin, 2% of Morwet EFW, 248% of SK24, 2% of carboxymethyl cellulose, 5% of kaolin, and make up to 100% with ammonium sulfate. Mix them evenly, grind them into mother powder by a jet mill, then add an appropriate amount of water for mixing, and granulate with an extrusion granulator to obtain 18% Compound A·fenazaquin water dispersible granules.

[0164] Formulation of 50% Compound A·afoxolaner water dispersible granules in Comparative Example 19

[0165] According to the formulation requirements, take 8% of Compound A, 42% of afoxolaner, 2.5% of coconut oil, 2% of Morwet EFW, 24N10% of SK24, 15% of kaolin, and make up to 100% with ammonium sulfate. Mix them evenly, grind them into mother powder by a jet mill, then add an appropriate amount of water for mixing, and granulate with an extrusion granulator to obtain 50% Compound A·afoxolaner water dispersible granules.

[0166] Formulation of 50% Compound A·afoxolaner water dispersible granules in Comparative Example 20

[0167] According to the formulation requirements, 8% of compound A, 42% of afoxolaner, 1.25% of calcium stearate, 2% of Morwet EFW, 10% of SK24N, 15% of kaolin, and ammonium sulfate are added to make up 100%. Mix them evenly, grind them into mother powder by a jet mill, then add an appropriate amount of water for mixing, and granulate with an extrusion granulator to obtain 50% compound A·afoxolaner water dispersible granules.

[0168] Preparation of 50% compound A·afoxolaner water dispersible granules in Comparative Example 2

[0169] According to the formulation requirements, 8% of compound A, 42% of afoxolaner, 2% of Morwet EFW, 10% of SK24N, 15% of kaolin, and ammonium sulfate are added to make up 100%. Mix them evenly, grind them into mother powder by a jet mill, then add an appropriate amount of water for mixing, and granulate with an extrusion granulator to obtain 50% compound A·afoxolaner water dispersible granules.

[0170] Preparation of 14% compound A·avermectin water dispersible granules in Comparative Example 22

[0171] According to the formulation requirements, 12% of compound A, 2% of avermectin, 0.5% of coconut oil, 2% of Yus-SXC, 10% of DF101, 15% of kaolin, and ammonium sulfate are added to make up 100%. Mix them evenly, grind them into mother powder by a jet mill, then add an appropriate amount of water for mixing, and granulate with an extrusion granulator to obtain 14% compound A·avermectin water dispersible granules.

[0172] Preparation of 14% compound A·avermectin water dispersible granules in Comparative Example 23

[0173] According to the formulation requirements, 12% of compound A, 2% of avermectin, 0.25% of calcium stearate, 2% of Yus-SXC, 10% of DF101, 15% of kaolin, and ammonium sulfate are added to make up 100%. Mix them evenly, grind them into mother powder by a jet mill, then add an appropriate amount of water for mixing, and granulate with an extrusion granulator to obtain 14% compound A·avermectin water dispersible granules.

[0174] Preparation of 14% compound A·avermectin water dispersible granules in Comparative Example 24

[0175] According to the formulation requirements, 12% of compound A, 2% of avermectin, 2% of Yus-SXC, 10% of DF101, 15% of kaolin, and ammonium sulfate are added to make up 100%. Mix them evenly, grind them into mother powder by a jet mill, then add an appropriate amount of water for mixing, and granulate with an extrusion granulator to obtain 14% compound A·avermectin water dispersible granules.

[0176] Formulation of 25.18% Compound A·Etoxazole Water Dispersible Granules (Comparative Example)

[0177] According to the formulation requirements, take 12% of Compound A, 6% of etoxazole, 1% of coconut oil, 3% of Yus-SXC, 8% of YusWG4, 2% of carboxymethyl cellulose, 4% of kaolin, and make up to 100% with ammonium sulfate. Mix them evenly, pulverize to obtain the mother powder by a jet mill, then add an appropriate amount of water for mixing, and granulate with an extrusion granulator to obtain 18% Compound A·Etoxazole Water Dispersible Granules.

[0178] Formulation of 26.18% Compound A·Etoxazole Water Dispersible Granules (Comparative Example)

[0179] According to the formulation requirements, take 12% of Compound A, 6% of etoxazole, 0.5% of calcium stearate, 3% of Yus-SXC, 8% of YusWG4, 2% of carboxymethyl cellulose, 4% of kaolin, and make up to 100% with ammonium sulfate. Mix them evenly, pulverize to obtain the mother powder by a jet mill, then add an appropriate amount of water for mixing, and granulate with an extrusion granulator to obtain 18% Compound A·Etoxazole Water Dispersible Granules.

[0180] Formulation of 27.18% Compound A·Etoxazole Water Dispersible Granules (Comparative Example)

[0181] According to the formulation requirements, take 12% of Compound A, 6% of etoxazole, 3% of Yus-SXC, 8% of YusWG4, 2% of carboxymethyl cellulose, 4% of kaolin, and make up to 100% with ammonium sulfate. Mix them evenly, pulverize to obtain the mother powder by a jet mill, then add an appropriate amount of water for mixing, and granulate with an extrusion granulator to obtain 18% Compound A·Etoxazole Water Dispersible Granules.

[0182] Formulation of 28.20% Compound A·Cyazofamid Water Dispersible Granules (Comparative Example)

[0183] According to the formulation requirements, take 10% of Compound A, 10% of cyazofamid, 0.8% of coconut oil, 2% of Yus-SXC, 10% of Yus-RXB, 10% of kaolin, and make up to 100% with ammonium sulfate. Mix them evenly, pulverize to obtain the mother powder by a jet mill, then add an appropriate amount of water for mixing, and granulate with an extrusion granulator to obtain 20% Compound A·Cyazofamid Water Dispersible Granules.

[0184] Formulation of 29.20% Compound A·Cyazofamid Water Dispersible Granules (Comparative Example)

[0185] According to the formula requirements, take 10% of Compound A, 10% of cyetpyrafen, 0.4% of calcium stearate, 2% of Yus-SXC, 10% of Yus-RXB, 10% of kaolin, and make up the balance to 100% with ammonium sulfate. Mix them evenly, grind them into mother powder by an air-flow pulverizer, then add an appropriate amount of water for mixing, and granulate with an extrusion granulator to obtain 20% Compound A·cyetpyrafen water dispersible granules.

[0186] Comparative Example 3. Preparation of 20% Compound A·cyetpyrafen water dispersible granules

[0187] According to the formula requirements, take 10% of Compound A, 10% of cyetpyrafen, 2% of Yus-SXC, 10% of Yus-RXB, 10% of kaolin, and make up the balance to 100% with ammonium sulfate. Mix them evenly, grind them into mother powder by an air-flow pulverizer, then add an appropriate amount of water for mixing, and granulate with an extrusion granulator to obtain 20% Compound A·cyetpyrafen water dispersible granules.

[0188] 11. Preparation of dry suspension concentrate

[0189] Example 37. Preparation of 70% Compound A·clofentezine dry suspension concentrate

[0190] According to the formula requirements, add 10% of Compound A, 15% of clofentezine, 3% of coconut oil, 1.5% of calcium stearate, 18% of DF101, 3% of kaolin, and make up the balance to 100% with deionized water into a mixing kettle, mix and stir with a high-shear mixer, then enter a sand mill for sand grinding to obtain 25% Compound A·clofentezine suspension concentrate. Then spray granulate with 25% Compound A·clofentezine suspension concentrate to obtain 70% Compound A·clofentezine dry suspension concentrate with good physical properties.

[0191] Example 38. Preparation of 30% Compound A·etoxazole dry suspension concentrate

[0192] According to the formula requirements, add 10% of Compound A, 5% of etoxazole, 1.5% of coconut oil, 0.75% of calcium stearate, 6% of YusRXB, 3% of white carbon black, and make up the balance to 100% with deionized water into a mixing kettle, mix and stir with a high-shear mixer, then enter a sand mill for sand grinding to obtain 15% Compound A·etoxazole suspension concentrate. Then spray granulate with 15% Compound A·etoxazole suspension concentrate to obtain 30% Compound A·etoxazole dry suspension concentrate with good physical properties.

[0193] Example 39. Preparation of 45% Compound A·avermectin dry suspension concentrate

[0194] According to the formulation requirements, add 20% of compound A, 5% of abamectin, 2% of coconut oil, 1% of calcium stearate, 8% of SK24N, 2% of Morwet EFW, 3% of kaolin, and make up to 100% with deionized water into the mixing kettle, mix and stir with a high-shear mixer, and then enter the sand mill for sanding to obtain a 25% compound A·abamectin suspension concentrate. Then, spray granulation is carried out with the 25% compound A·abamectin suspension concentrate to obtain a 45% compound A·abamectin dry suspension concentrate with good physical properties.

[0195] Example 4. Preparation of 50% compound A·etoxazole dry suspension concentrate

[0196] According to the formulation requirements, add 10% of compound A, 20% of etoxazole nitrile, 2.5% of coconut oil, 1.25% of calcium stearate, 10% of NNO, 4% of Dispersol CBZ, 3% of white carbon black, and make up to 100% with deionized water into the mixing kettle, mix and stir with a high-shear mixer, and then enter the sand mill for sanding to obtain a 30% compound A·etoxazole nitrile suspension concentrate. Then, spray granulation is carried out with the 30% compound A·etoxazole nitrile suspension concentrate to obtain a 50% compound A·etoxazole nitrile dry suspension concentrate with good physical properties.

[0197] Comparative Example 3. Preparation of 70% compound A·clofentezine dry suspension concentrate

[0198] According to the formulation requirements, add 10% of compound A, 15% of clofentezine, 3% of coconut oil, 8% of DF101, 3% of kaolin, and make up to 100% with deionized water into the mixing kettle, mix and stir with a high-shear mixer, and then enter the sand mill for sanding to obtain a 25% compound A·clofentezine suspension concentrate. Then, spray granulation is carried out with the 25% compound A·clofentezine suspension concentrate to obtain a 70% compound A·clofentezine dry suspension concentrate with good physical properties.

[0199] Comparative Example 32. Preparation of 70% compound A·clofentezine dry suspension concentrate

[0200] According to the formulation requirements, add 10% of compound A, 15% of clofentezine, 1.5% of calcium stearate, 8% of DF101, 3% of kaolin, and make up to 100% with deionized water into the mixing kettle, mix and stir with a high-shear mixer, and then enter the sand mill for sanding to obtain a 25% compound A·clofentezine suspension concentrate. Then, spray granulation is carried out with the 25% compound A·clofentezine suspension concentrate to obtain a 70% compound A·clofentezine dry suspension concentrate with good physical properties.

[0201] Comparative Example 33. Preparation of 70% compound A·clofentezine dry suspension concentrate

[0202] According to the formula requirements, add 10% of Compound A, 15% of clofentezine, 8% of DF101, 3% of kaolin, and make up to 100% with deionized water into the mixing kettle, mix and stir with a high-shear mixer, and then enter the sand mill for sanding to obtain a 25% Compound A·clofentezine suspension concentrate. Then, spray granulation is carried out with the 25% Compound A·clofentezine suspension concentrate to obtain a 70% Compound A·clofentezine dry flowable with good physical properties.

[0203] Preparation of 34.30% Compound A·etoxazole dry flowable for comparative example

[0204] According to the formula requirements, add 10% of Compound A, 5% of etoxazole, 1.5% of coconut oil, 6% of YusRXB, 3% of white carbon black, and make up to 100% with deionized water into the mixing kettle, mix and stir with a high-shear mixer, and then enter the sand mill for sanding to obtain a 15% Compound A·etoxazole suspension concentrate. Then, spray granulation is carried out with the 15% Compound A·etoxazole suspension concentrate to obtain a 30% Compound A·etoxazole dry flowable with good physical properties.

[0205] Preparation of 35.30% Compound A·etoxazole dry flowable for comparative example

[0206] According to the formula requirements, add 10% of Compound A, 5% of etoxazole, 0.75% of calcium stearate, 6% of YusRXB, 3% of white carbon black, and make up to 100% with deionized water into the mixing kettle, mix and stir with a high-shear mixer, and then enter the sand mill for sanding to obtain a 15% Compound A·etoxazole suspension concentrate. Then, spray granulation is carried out with the 15% Compound A·etoxazole suspension concentrate to obtain a 30% Compound A·etoxazole dry flowable with good physical properties.

[0207] Preparation of 36.30% Compound A·etoxazole dry flowable for comparative example

[0208] According to the formula requirements, add 10% of Compound A, 5% of etoxazole, 6% of YusRXB, 3% of white carbon black, and make up to 100% with deionized water into the mixing kettle, mix and stir with a high-shear mixer, and then enter the sand mill for sanding to obtain a 15% Compound A·etoxazole suspension concentrate. Then, spray granulation is carried out with the 15% Compound A·etoxazole suspension concentrate to obtain a 30% Compound A·etoxazole dry flowable with good physical properties.

[0209] Preparation of 45% Compound A·abamectin dry flowable for comparative example

[0210] According to the formulation requirements, add 20% of Compound A, 5% of abamectin, 2% of coconut oil, 8% of SK24N, 2% of Morwet EFW, 3% of kaolin, and make up to 100% with deionized water into the mixing kettle, mix and stir with a high-shear mixer, and then enter the sand mill for sanding to obtain a 25% Compound A·abamectin suspension. Then, spray granulation is carried out with the 25% Compound A·abamectin suspension to obtain a 45% Compound A·abamectin dry suspension with good physical properties.

[0211] Preparation of 38.45% Compound A·abamectin dry suspension in Comparative Example

[0212] According to the formulation requirements, add 20% of Compound A, 5% of abamectin, 1% of calcium stearate, 8% of SK24N, 2% of Morwet EFW, 3% of kaolin, and make up to 100% with deionized water into the mixing kettle, mix and stir with a high-shear mixer, and then enter the sand mill for sanding to obtain a 25% Compound A·abamectin suspension. Then, spray granulation is carried out with the 25% Compound A·abamectin suspension to obtain a 45% Compound A·abamectin dry suspension with good physical properties.

[0213] Preparation of 39.45% Compound A·abamectin dry suspension in Comparative Example

[0214] According to the formulation requirements, add 20% of Compound A, 5% of abamectin, 8% of SK24N, 2% of Morwet EFW, 3% of kaolin, and make up to 100% with deionized water into the mixing kettle, mix and stir with a high-shear mixer, and then enter the sand mill for sanding to obtain a 25% Compound A·abamectin suspension. Then, spray granulation is carried out with the 25% Compound A·abamectin suspension to obtain a 45% Compound A·abamectin dry suspension with good physical properties.

[0215] Preparation of 50% Compound A·cyazofamid dry suspension in Comparative Example 40

[0216] According to the formulation requirements, add 10% of Compound A, 20% of cyazomite, 2.5% of coconut oil, 10% of NNO, 4% of Dispersol CBZ, 3% of silica white, and make up to 100% with deionized water into the mixing kettle, mix and stir with a high-shear mixer, and then enter the sand mill for sanding to obtain a 30% Compound A·cyazofamid suspension. Then, spray granulation is carried out with the 30% Compound A·cyazofamid suspension to obtain a 50% Compound A·cyazofamid dry suspension with good physical properties.

[0217] Preparation of 50% Compound A·cyazofamid dry suspension in Comparative Example 41

[0218] According to the formulation requirements, add 10% of compound A, 20% of etoxazole nitrile, 1.25% of calcium stearate, 10% of NNO, 4% of Dispersol CBZ, 3% of silica white, and make up to 100% with deionized water into the mixing kettle, mix and stir with a high-shear mixer, and then enter the sand mill for sanding to obtain a 30% compound A·etoxazole nitrile suspension. Then, spray granulation is carried out with the 30% compound A·etoxazole nitrile suspension to obtain a 50% compound A·etoxazole nitrile dry suspension with good physical properties.

[0219] Formulation of 42.50% compound A·etoxazole nitrile dry suspension in Comparative Example

[0220] According to the formulation requirements, add 10% of compound A, 20% of etoxazole nitrile, 10% of NNO, 4% of Dispersol CBZ, 3% of silica white, and make up to 100% with deionized water into the mixing kettle, mix and stir with a high-shear mixer, and then enter the sand mill for sanding to obtain a 30% compound A·etoxazole nitrile suspension. Then, spray granulation is carried out with the 30% compound A·etoxazole nitrile suspension to obtain a 50% compound A·etoxazole nitrile dry suspension with good physical properties.

[0221] Preparation of control preparation (according to the method of Patent CN114642203B)

[0222] Comparative Example 43. Compound A + etoxazole (12% + 6%) medicament

[0223] Dissolve compound A (12%) and etoxazole (6%) in acetone, and prepare a solution with the required concentration with a 0.1% Tween 80 solution according to the application concentration.

[0224] Comparative Example 44. Compound A + abamectin (12% + 2%) medicament

[0225] Dissolve compound A (12%) and abamectin (2%) in acetone, and prepare a solution with the required concentration with a 0.1% Tween 80 solution according to the application concentration.

[0226] Example of application performance test

[0227] Compare the stability after standing over time of Examples 1, 5, 6, 10, 16, 17, 22, 23, 25, 26, 29, 30, 32, 34, 35, Comparative Example 43, and Comparative Example 44 (diluted 1000 times) (the results are shown in Table 1).

[0228] Table 1. Stability of the dilution of the biphenyl compound-containing preparation and the control preparation after standing over time

[0229]

[0230]

[0231] As can be seen from the data in the table, the 1000-fold dilutions of the preparations of Example 1, Example 5, Example 6, Example 10, Example 16, Example 17, Example 22, Example 23, Example 25, Example 26, Example 29, Example 30, Example 32, Example 34, and Example 35 still had good stability after being left standing for 12 h. The 1000-fold dilutions of the agents in Comparative Example 43 and Comparative Example 44 had good stability only when left standing for 1 h, and crystal precipitation occurred when left standing for 2 h, 6 h, and 12 h. There was a phenomenon of instability of the dilution when preparing the agents by the methods of Comparative Example 43 and Comparative Example 44, which was not conducive to the application of the agents and could only be prepared and used immediately when in use.

[0232] The suspension rates of the normal temperature samples and the samples after heat storage expiration (heat storage at 54 °C for 14 d) of Example 27 - Example 40 and Comparative Example 1 - Comparative Example 42 were measured, and the results are shown in Table 2.

[0233] Table 2. Suspension rates of the preparations containing biphenyl compounds and the control preparations for normal temperature and heat storage samples

[0234]

[0235]

[0236]

[0237] As can be seen from the data in the table, when no stabilizer was added or only one component of the stabilizer (coconut oil or calcium stearate) was added in Comparative Example 1 - Comparative Example 42 (wettable powder, water dispersible granule, dry suspension), the suspension rate of the normal temperature sample was above 95%, and the suspension rate of the sample after heat storage expiration decreased significantly, only about 70%, and the suspension rate of some products was lower than 70%, not meeting the quality standard requirements. When stabilizers (coconut oil and calcium stearate) were added to the formulation (Example 27 - Example 40), the suspension rates of the normal temperature and heat storage expiration samples could both reach above 95%. It shows that adding stabilizers to wettable powders, water dispersible granules, and dry suspensions significantly improved the problem of poor suspension rates after heat storage expiration of wettable powders, water dispersible granules, and dry suspensions.

[0238] Examples of Biological Activity Tests

[0239] 1. Test Purpose

[0240] Under greenhouse conditions, compare the control effects of the preparations containing biphenyl compounds and the control preparations in the above examples on adult Tetranychus cinnabarinus.

[0241] 2. Test reagents

[0242] Example 29.14% Compound A·Avermectin Wettable Powder

[0243] Example 30.18% Compound A·Ethioxazole Wettable Powder

[0244] Example 34.14% Compound A·Avermectin Water Dispersible Granules

[0245] Example 35.18% Compound A·Ethioxazole Water Dispersible Granules

[0246] Comparative Example 43. Compound A + etoxazole (12% + 6%)

[0247] Comparative Example 44. Compound A + Avermectin (12% + 2%)

[0248] 3. Test Target

[0249] Tetranychus cinnabarinus, adult, sensitive strain reared indoors.

[0250] 4. Test methods

[0251] 4.1 Test conditions:

[0252] Temperature: 25-27℃

[0253] Humidity: RH 60%

[0254] Lighting: L:D=14:10

[0255] 4.2 Preparation of drug solution

[0256] Use an electronic analytical balance to accurately weigh the test drug, first dissolve the original drug completely with the solvent and add an appropriate amount of emulsifier, then add water to the required concentration to prepare the mother solution of the required concentration. Use distilled water to prepare the required mother solution, and dilute it into a series of drug solutions with a certain concentration gradient according to the designed dosage of the experiment.

[0257] 4.3 Treatment methods

[0258] Use pot spray method. Leave one true leaf of greenhouse-cultivated bean seedlings (2 true leaves) and inoculate 20-30 adult mites on it. Use Airbrush to evenly spray on the front and back of the test material and dry it naturally in the shade. First treat the blank control with clean water, then repeat the above operation in order from low to high doses according to the experimental design, with 3 replicates for each treatment, and set up a blank control.

[0259] 4.4 Survey Methods

[0260] Place the processed test materials in the observation chamber. After 72 hours, investigate the mortality of the test insects and record the number of dead insects.

[0261] 4.5 Calculation method:

[0262] Place the processed test materials in the observation chamber. Conduct a test investigation after 72 hours, record the number of dead and live insects, and calculate the corrected mortality rate using the Abbott formula. Use the DPS data statistical software to obtain the virulence regression equation and 95% confidence limit of the test agents.

[0263] 5. Test results

[0264] Table 3. Control effects of the formulations containing biphenyl compounds and the control formulation on adult Tetranychus cinnabarinus

[0265]

[0266] As can be seen from the data in the table, the control effects of Example 29, Example 34 and Comparative Example 44 on adult Tetranychus cinnabarinus are comparable; the control effects of Example 30, Example 35 and Comparative Example 43 on adult Tetranychus cinnabarinus are comparable.

[0267] Compared with the prior art, the formulation containing a biphenyl compound obtained by the present invention selects a dosage form according to the application scenario and selects a suitable adjuvant system according to the dosage form. The stability of the preparation dilution is good after standing for 12 hours, there is no crystal precipitation phenomenon, and it does not need to be prepared and used immediately, so it is easy to spray and apply. In the development of solid preparations such as wettable powders, water-dispersible granules, and dry suspensions, by using stabilizers, the problem of the suspension rate decreasing or even being unqualified after heat storage caused by the low melting point of the active ingredient A and melting and sticking during the heat storage process is significantly improved. The formulation containing a biphenyl compound obtained by the present invention has reliable quality and application performance, has a good control effect on the target pest mites, and is expected to have good economic benefits.

[0268] The content not described in detail in this specification belongs to the prior art well-known to those skilled in the art.

Claims

1. A preparation containing a biphenyl compound, characterized in that: The preparation consists of active ingredient A, active ingredient B, at least one surfactant and at least one carrier, wherein the weight percentage of the active ingredients is 0.1%-95%, the mass ratio between active ingredient A and active ingredient B is 1:99-99:1, and the structural formula of active ingredient A is as follows: Active ingredient B is selected from inhibitors of mitochondrial electron transport complex (II), allosteric modulators of nicotinic acetylcholine receptors, chloride channel agonists, mite growth inhibitors, acetyl-CoA carboxylase inhibitors, ATP synthase inhibitors, inhibitors of mitochondrial electron transport complex (I), inhibitors of mitochondrial electron transport complex (III), pyrethroids, insect growth regulators, organophosphorus, nicotine, feeding deterrents, nereistoxin analogs, ryanodine receptor regulators, voltage-dependent sodium channel blockers, GABA-gated chloride antagonists, microorganisms, isoxazoline insecticides and acaricides or other insecticides and acaricides.

2. The preparation containing biphenyl compounds according to claim 1, characterized in that: The dosage form of the preparation is emulsifiable concentrate, emulsion in water, microemulsion, suspoemulsion, seed treatment emulsion, suspending agent, seed treatment suspending agent, dispersible oil suspension, wettable powder, water dispersible granule or dry suspension.

3. The wettable powder, water dispersible granule, or dry flowable agent according to claim 2, wherein: When the preparation is a solid preparation, the surfactant contains a stabilizer, and the stabilizer accounts for 0.5%-5% of the mass of the preparation.

4. The preparation containing a biphenyl compound according to claim 3, characterized in that: The surfactant is a stabilizer and one or several auxiliaries; the auxiliaries are wetting and dispersing agents, binders, disintegrants, defoamers.

5. The preparation containing biphenyl compounds according to claim 3 or 4, characterized in that: The stabilizer is coconut oil and calcium stearate, and the ratio between coconut oil and calcium stearate is 2:

1.

6. The wettable powder, water dispersible granule or dry flowable agent according to any one of claims 2 to 5, characterized in that: In the preparation by weight percentage, the active ingredient is 0.1%-95%, the wetting and dispersing agent is 1%-40%, the stabilizer is 0.5%-5%, the binder is 0-10%, the disintegrant is 0-10%, the defoamer is 0-10%, and the carrier is 1%-99%; The active ingredient is active ingredient A and active ingredient B, and the mass ratio between active ingredient A and active ingredient B is 1:50-50:

1.

7. The biphenyl compound-containing preparation according to claim 1, characterized in that: The active ingredient B is selected from cyazofamid, cyenopyrafen, cyflumetofen, abamectin, emamectin benzoate, spinosad, spinetoram, clofentezine, hexythiazox, etoxazole, flufenzine, spirodiclofen, spirotetramat, spiroethrin, diafenthiuron, azocyclotin, propargite, pyridaben, fenpyroximate, pyrimidifen, pyrimidaben, Flometoquin, hydramethylnon, Pyflubumide, Acynonspyr, chlorfenapyr, fluazinam, fenpropathrin, beta-cyfluthrin, lufenuron, hexaflumuron, tebufenozide, flonicamid, pyriproxyfen, chlorpyrifos, imidacloprid, thiamethoxam, pymetrozine, indoxacarb, chlorantraniliprole, butene-fipronil, veratrine, isoxazoline insecticide, flucoxazolamide, fluralaner, afoxolaner, lotilaner, sarolaner, alphacyfluthrin, quinoxyfen, Flipper TM (contact biological insecticide / acaricide containing C7-C20 fatty acids), N-[[2-fluoro-4-[2-hydroxy-3-(3,4,5-trichlorophenyl)-3-(trifluoromethyl)pyrrolidin-1-yl]phenyl]methyl]cyclopropanecarboxamide or (S)-N-[[2-fluoro-4-[2-hydroxy-3-(3,4,5-trichlorophenyl)-3-(trifluoromethyl)pyrrolidin-1-yl]phenyl]methyl]cyclopropanecarboxamide.

8. Use of the preparation containing biphenyl compounds as claimed in claim 1, characterized in that: The application of the preparation in the control of agricultural pests and mites, forestry pests and mites or non-therapeutic hygienic pests and mites.

Citation Information

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