A miticidal composition

Abstract

The present application belongs to the technical field of pesticides, and relates to a kind of acaricidal composition;The effective component of the acaricidal composition comprises active ingredient A and active ingredient B;The active ingredient A is fluorine mite sulfide, and the active ingredient B is selected from Acynonapyr.The acaricidal composition or its preparation of the present application can enhance efficacy, expand the acaricidal spectrum, reduce the use cost, reduce the amount of drug, prolong the effective period and delay the development of drug resistance.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of pesticide combination, in particular to a kind of acaricidal composition, the acaricidal composition or its preparation can enhance efficacy, reduce the amount of drug, while it can improve the speed of efficiency, prolong the effective period and delay the development of drug resistance. BACKGROUND

[0002] In the process of agricultural production, plant diseases and insect pests have been one of the main disasters. According to incomplete statistics, the world's grain and cotton production is lost more than 10% per year due to plant diseases and insect pests. These diseases not only cause the reduction of crop yield, but also pose a threat to the quality and safety of crop products and their international trade to some extent. Among them, phytophagous spider mites have seriously threatened the quality and safety of agricultural products, causing a lot of losses to farmers.

[0003] Fluensulfene has the chemical name of (4'-chloro-6-fluoro-4-methyl-[1,1'-biphenyl]-3-yl)(2,2,2-trifluoroethyl) sulfide, and the chemical structural formula is as follows:

[0004]

[0005] Acynonapyr is a novel acaricide with a cyclic amine skeleton developed by Nippon Soda Co., Ltd. of Japan. It acts on inhibitory glutamate receptors (IGluRs) to interfere with the nerve transmission of harmful mites, making the muscle cells lose their original movement ability, showing a state similar to paralysis, thereby affecting feeding or movement, and ultimately killing the harmful mites. It has good control effect on spider mites of fruit trees, vegetables and tea trees.

[0006] In the process of agricultural production, chemical pesticides are the most effective means to control plant diseases and insect pests. Long-term continuous high-dose use of a single chemical pesticide can easily cause the harmful mites to develop resistance, environmental pollution and a series of problems. Reasonable chemical pesticide combination or mixing has the positive characteristics of expanding the insecticidal spectrum, improving the control effect, prolonging the application period, reducing the amount of pesticide, reducing pesticide damage, reducing residues, delaying the occurrence of pest resistance and drug resistance, etc. The applicant is surprised to find that the combination of fluensulfene and acynonapyr has obvious synergistic effect through indoor toxicity test and field efficacy test, and there is no report on the acaricidal composition and application of the combination of fluensulfene and acynonapyr. SUMMARY

[0007] Based on the above situation, the present application aims to provide an acaricidal composition and its preparation, mainly used for controlling phytophagous spider mites. The acaricidal composition or its preparation can enhance efficacy, reduce the amount of drug, while it can prolong the effective period and delay the development of drug resistance.

[0008] To achieve the above objectives, the present invention provides the following technical solution: an acaricide composition comprising active ingredient A, flufenoxuron, and active ingredient B, Acynonapyr;

[0009] Furthermore, the mass ratio of the flumethrin to Acynonapyr is 1:30 to 35:1;

[0010] Furthermore, the mass ratio of the flumethrin to Acynonapyr is 1:20 to 25:1;

[0011] Furthermore, the mass ratio of the flumethrin to Acynonapyr is 1:30 to 35:1;

[0012] Furthermore, the mass ratio of flufenoxuron to Acynonapyr is 1:30, 1:20, 1:15, 2:15, 1:3, 3:4, 15:2, 15:1, 25:1, or 35:1.

[0013] Furthermore, the mass ratio of the flumethrin to Acynonapyr is 1:20 to 25:1;

[0014] Furthermore, the mass ratio of the flumethrin to Acynonapyr is 1:20, 1:15, 2:15, 1:3, 3:4, 15:2, 15:1, or 25:1.

[0015] Furthermore, the mass ratio of the flumethrin to Acynonapyr is 1:20, 1:12, 2:17, 1:6, 1:2, 8:1, 12:1, or 25:1;

[0016] Furthermore, the mass ratio of the flumethrin to Acynonapyr is 2:17 to 12:1;

[0017] Furthermore, the mass ratio of the flumethrin to Acynonapyr is 2:17, 1:6, 1:2, 8:1, or 12:1.

[0018] An acaricide composition containing flufenoxuron and Acynonapyr, wherein, based on a total weight of 100 wt% of the acaricide composition, the sum of the contents of active ingredient A and active ingredient B in the acaricide composition is 1-95 wt%.

[0019] Furthermore, based on a total mass of 100 wt% of the acaricide composition, the sum of the contents of flufenoxuron and Acynonapyr in the acaricide composition is 5 to 50 wt%.

[0020] Further, based on a total mass of 100 wt% of the acaricide composition, the sum of the contents of flufenoxuron and Acynonapyr in the acaricide composition is 10 wt%, 15 wt%, 20 wt%, 25 wt%, 40 wt%, and 45 wt%.

[0021] Furthermore, the acaricidal composition further includes an adjuvant selected from one or more of wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreeze agents, defoamers, solvents, preservatives, stabilizers, synergists, and carriers;

[0022] The wetting agent is selected from one or more of the following: alkylbenzene sulfonates, alkylnaphthalene sulfonates, lignin sulfonates, sodium dodecyl sulfate, sodium dioctyl succinate sulfonate, α-olefin sulfonates, alkylphenol polyoxyethylene ethers, castor oil polyoxyethylene ethers, alkylphenol ethoxylates, fatty alcohol ethoxylates, sodium fatty alcohol polyoxyethylene ether sulfate, silkworm excrement, soapberry powder, soapberry powder, SOPA, detergents, emulsifiers 2000 series, and wetting and penetrating agents F; and / or

[0023] The dispersant is selected from one or more of the following: lignin sulfonates, alkyl naphthalene sulfonates formaldehyde condensates, naphthalene sulfonates, tristyrylphenol ethoxylate phosphates, fatty alcohol ethoxylates, alkylphenol polyoxyethylene ethers, alkylphenol polyoxyethylene ether methyl ether condensates sulfates, fatty amine polyoxyethylene ethers, glycerol fatty acid ester polyoxyethylene ethers, polycarboxylates, polyacrylic acids, phosphates, EO-PO block copolymers, and EO-PO graft copolymers; and / or

[0024] The emulsifier is selected from one or more of the following: calcium dodecylbenzenesulfonate, alkylphenol formaldehyde resin polyoxyethylene ether, phenethylphenol polyoxyethylene polyoxypropylene ether, fatty alcohol ethylene oxide-propylene oxide copolymer, styrene-phenol polyoxyethylene ether, castor oil polyoxyethylene ether, and alkylphenol ether phosphate; and / or

[0025] The thickener is selected from one or more of xanthan gum, organobentonite, gum arabic, sodium alginate, magnesium aluminum silicate, carboxymethyl cellulose, and silica; and / or

[0026] The disintegrant is selected from one or more of sodium sulfate, ammonium sulfate, aluminum chloride, sodium chloride, ammonium chloride, bentonite, glucose, sucrose, starch, cellulose, urea, sodium carbonate, sodium bicarbonate, citric acid, and tartaric acid; and / or

[0027] Antifreeze is selected from one or more of alcohols, alcohol ethers, chlorinated hydrocarbons, and inorganic salts; and / or

[0028] Defoamer selected from C 10 -C 20 Saturated fatty acid compounds, silicone oil, silicone compounds, C8-C 10One or more of the fatty alcohols; and / or

[0029] The solvent is selected from one or more of benzene, toluene, xylene, mesitylene, methanol, ethanol, isopropanol, n-butanol, dimethyl sulfoxide, dimethylformamide, cyclohexanone, hydrocarbon carbonates, diesel oil, solvent oil, vegetable oil, vegetable oil derivatives, and water; and / or

[0030] The preservative is selected from one or more of propionic acid, sodium propionate, sorbic acid, sodium sorbate, potassium sorbate, benzoic acid, sodium benzoate, sodium p-hydroxybenzoate, methyl p-hydroxybenzoate, Kathon, and 1,2-benzisothiazolin-3-one; and / or

[0031] The stabilizer is selected from one or more of the following: disodium hydrogen phosphate, oxalic acid, succinic acid, adipic acid, borax, 2,6-di-tert-butyl-p-cresol, triethanolamine oleate, epoxidized vegetable oil, kaolin, bentonite, attapulgite, silica, talc, montmorillonite, and starch; and / or

[0032] Synergists are selected from synergistic phosphorus, synergistic ether; and / or

[0033] The carrier is selected from one or more of the following: ammonium salts, ground natural minerals, ground artificial minerals, silicates, resins, waxes, solid fertilizers, water, organic solvents, mineral oils, vegetable oils, and vegetable oil derivatives.

[0034] This invention optimizes the content of active ingredients and adjuvants in the acaricide composition to achieve a better balance between toxicity and residue, thereby enhancing efficacy, reducing dosage, and lowering costs.

[0035] Furthermore, the pesticide composition can be prepared into an agriculturally permissible formulation, wherein the formulation is selected from solid and / or liquid formulations;

[0036] Furthermore, the solid formulation is selected from wettable powders and water-dispersible granules; the liquid formulation is selected from emulsifiable concentrates, water emulsions, microemulsions, suspensions, suspension emulsions, and dispersible oil suspensions.

[0037] The specific implementation scheme of the pesticide formulation prepared from the acaricidal composition of the present invention is as follows:

[0038] When the acaricide composition is a wettable powder, the mass parts of the components are: 1-40 parts of flufenoxuron; 1-40 parts of Acynonapyr; 3-10 parts of dispersant; 1-5 parts of wetting agent; and filler to make up the balance.

[0039] The specific production steps of the wettable powder are as follows: the active ingredients, dispersant, wetting agent and filler are mixed according to the above formula, stirred evenly in a mixer, and then mixed evenly after air jet pulverization, so as to prepare the wettable powder of the composition of the present invention.

[0040] When the acaricide composition is a water-dispersible granule, the mass parts of the components are: 1-40 parts of flufenoxuron; 1-40 parts of Acynonapyr; 3-10 parts of dispersant; 1-10 parts of wetting agent; 1-5 parts of disintegrant; and filler to make up the balance.

[0041] The specific production steps of the water-dispersible granules are as follows: the active ingredients, dispersant, wetting agent, disintegrant and filler are mixed evenly according to the above formula, pulverized by an ultra-micro airflow pulverizer, kneaded, and then added to a fluidized bed granulation dryer for granulation, drying, sieving and sampling analysis, and the water-dispersible granules of the composition of the present invention can be produced.

[0042] When the acaricide composition is an emulsifiable concentrate, the mass fractions of the components are: 1-40 parts of flufenoxuron; 1-40 parts of Acynonapyr; 10-30 parts of conventional emulsifier; 20-50 parts of conventional solvent; and 1-5 parts of conventional synergist.

[0043] The specific production steps of this emulsifiable concentrate are as follows: first, the active ingredient is added to a solvent and completely dissolved, then emulsifier and synergist are added and stirred evenly to form a uniform and transparent oily liquid, which is then filled into a container to produce the emulsifiable concentrate of the composition of this invention.

[0044] When the acaricide composition is an emulsion, the mass parts of the components are as follows: 1-40 parts of flufenoxuron; 1-40 parts of Acynonapyr; 3-30 parts of emulsifier; 5-15 parts of solvent; 2-15 parts of stabilizer; 1-5 parts of antifreeze; 0.1-8 parts of defoamer; 0.2-2 parts of thickener; and deionized water to make up the balance.

[0045] The specific production steps of this water-in-oil emulsion are as follows: First, the active ingredient, solvent, emulsifier, and cosolvent are added together to dissolve into a uniform oil phase; then, deionized water, antifreeze, antimicrobial agents, and other pesticide adjuvants are mixed together to form a uniform aqueous phase; while stirring at high speed in a reaction vessel, the oil phase is added to the aqueous phase, and a shearing machine is turned on for high-speed shearing for about half an hour to form an oil-in-water emulsion, thus producing the water-in-oil emulsion of the composition of this invention.

[0046] When the acaricide composition is a microemulsion, the mass parts of the components are: 1-40 parts of flufenoxuron; 1-40 parts of Acynonapyr; 10-30 parts of emulsifier; 1-8 parts of antifreeze; 0.5-10 parts of stabilizer; and 20-50 parts of conventional solvents and cosolvents.

[0047] The specific production steps of this microemulsion are as follows: the active ingredient is completely dissolved in a cosolvent, then other ingredients such as emulsifiers, antifreeze stabilizers, etc. are added, mixed evenly, and finally water is added and stirred thoroughly to form a microemulsion.

[0048] When the acaricide composition is a suspension, the mass parts of the components are as follows: 1-40 parts of flufenoxuron; 1-40 parts of Acynonapyr; 1-10 parts of wetting and dispersing agent; 1-5 parts of antifreeze agent; 0.1-2 parts of thickener; 0.1-0.8 parts of defoamer; 0-10 parts of solvent; 1-5 parts of stabilizer; and deionized water to make up the balance.

[0049] The specific production steps of the suspension are as follows: using zirconium beads, wet pulverizing is performed using a sand mill until D90 (the particle size of 90% of the particles) is <5μm, thus preparing the suspension formulation of the composition of the present invention.

[0050] When the insecticidal composition is a suspension emulsion, the mass parts of the components are as follows: 1-40 parts of flufenoxuron; 1-40 parts of Acynonapyr; 1-10 parts of wetting and dispersing agent; 1-5 parts of antifreeze agent; 0.1-2 parts of thickener; 0.1-0.8 parts of defoamer; 1-40 parts of solvent; 1-5 parts of stabilizer; and deionized water to make up the balance.

[0051] The specific production steps of the suspension emulsion are as follows: Acynonapyr is completely solventized to form an oil phase; flufenoxuron, wetting and dispersing agent, antifreeze agent, defoamer, deionized water, etc. are wet-milled until D90 is less than 5μm to form a suspension mother liquor; the oil phase is added to the suspension mother liquor and stirred evenly, and then a thickener is added and stirred and sheared evenly to prepare the suspension emulsion formulation of the composition of the present invention.

[0052] When the insecticidal composition is a dispersible oil suspension, the mass parts of the components are: 1-40 parts of flufenoxuron; 1-40 parts of Acynonapyr; 1-10 parts of wetting and dispersing agent; 0.1-2 parts of thickener; 0.1-0.8 parts of defoamer; 0-10 parts of solvent; 1-5 parts of stabilizer; and vegetable oil to make up the balance.

[0053] The specific production steps of this dispersible oil suspension are as follows: using zirconium beads, wet pulverizing is performed using a sand mill until D90 (the particle size of 90% of the particles) is <5μm, thereby preparing the dispersible oil suspension formulation of the composition of the present invention.

[0054] The acaricidal composition of the present invention is used for the prevention and control of harmful mites;

[0055] Furthermore, the mites mentioned are phytophagous mites;

[0056] Furthermore, the phytophagous mites are Tetranychus carmineus, Tetranychus truncatus, Tetranychus two-spotted, and Tetranychus citrus red spider mite;

[0057] Furthermore, the acaricidal composition and / or its formulation are applied at an effective dose to the mites that need to be controlled and / or the medium in which they grow.

[0058] Compared with the prior art, the beneficial effects of the technical solution of the present invention are as follows:

[0059] (1) The compound acaricide of the present invention has a significant synergistic effect compared with the single agent, thus improving the control effect;

[0060] (2) The compound acaricide of the present invention improves the control effect while reducing the amount of drug used, reducing costs and reducing residues;

[0061] (3) The compound acaricide of the present invention is composed of two agents with different mechanisms of action, and there is no cross-resistance, which is beneficial to delaying the development of drug resistance in mites. Detailed Implementation

[0062] To make the technical solution, objectives and advantages of the present invention clearer, the present invention is described with reference to the following specific embodiments. However, the present invention can be implemented in various forms and should not be limited to the embodiments described herein.

[0063] Indoor toxicity testing

[0064] Test insect source: Citrus red spider mite (raised at the R&D center);

[0065] Specimen preparation: Select mites (adult females or nymphs) that are kept indoors and have the same physiological state. Cut double-sided tape into 2cm lengths and attach them to one end of a glass slide. Then select healthy mites and stick their backs onto the double-sided tape, 30 mites per slide. Place them in a container lined with a damp sponge, cover the container, and place it at (25±1)℃. After 2 hours, examine the slide under a microscope, remove any dead or injured individuals, and replenish the slide to 30 mites.

[0066] Reagent preparation: The technical grade drug was prepared into a stock solution using acetone. The stock solution was then diluted with a 0.1% Tween-80 aqueous solution to prepare test reagents in different proportions. The specific proportions and concentration gradients are as follows:

[0067] Table 1 Concentration gradients of single and combined agents of flufenoxuron and Acynonapyr for various treatments

[0068] Serial number Tested treatment Dilution concentration (mg / L) 1 Fluensulfone 0.75、1.5、3、6、12 2 Acynonapyr 0.5、1、2、4、8 3 Fluensulfone: Acynonapyr = 1:30 0.5、1、2、4、8 4 Fluensulfone: Acynonapyr = 1:20 0.5、1、2、4、8、16 5 Fluensulfone: Acynonapyr = 1:15 0.5、1、2、4、8 6 Fluensulfone: Acynonapyr = 1:12 1、2、4、8、16 7 Fluensulfone: Acynonapyr = 2:17 1、2、4、8、16 8 Fluensulfone: Acynonapyr = 2:15 0.5、1、2、4、8 9 Fluensulfone: Acynonapyr = 1:6 0.5、1、2、4、8 10 Fluensulfone: Acynonapyr = 1:3 0.5、1、2、4、8 11 Fluensulfone: Acynonapyr = 1:2 0.5、1、2、4、8 12 Fluensulfone: Acynonapyr = 3:4 0.25、0.5、1、2、4 13 Fluensulfone: Acynonapyr = 15:2 0.25、0.5、1、2、4 14 Fluensulfone: Acynonapyr = 8:1 0.5、1、2、4、8 15 Fluensulfone: Acynonapyr = 12:1 0.5、1、2、4、8 16 Fluensulfone: Acynonapyr = 15:1 0.25、0.5、1、2、4 17 Fluensulfone: Acynonapyr = 25:1 0.5、1、2、4、8、16 18 Fluensulfone: Acynonapyr = 35:1 0.5、1、2、4、8

[0069] Drug treatment: Immerse the glass slide in the drug solution and gently shake for 5 seconds, then remove it, absorb excess drug solution with absorbent paper, place it in a white porcelain dish lined with a damp sponge, cover with a transparent plastic film, and keep it at (25±1)℃ for observation. Each treatment was repeated 4 times, and a blank control without drug treatment was set up.

[0070] Experimental investigation: 48 hours after treatment, the mortality of the test insects was checked, and the total number of insects and the number of dead insects were recorded. The mortality rate was calculated.

[0071]

[0072] In the formula:

[0073] P – Mortality rate, expressed as a percentage (%);

[0074] K represents the number of dead insects, in heads;

[0075] N represents the total number of insects treated, in units of heads.

[0076]

[0077] In the formula:

[0078] P1 – Corrected mortality rate, in percentage (%);

[0079] P t —The mortality rate is expressed as a percentage (%).

[0080] P0 – Mortality rate in the blank control group, expressed as a percentage (%).

[0081] If the control mortality rate is <5%, no correction is needed; if the control mortality rate is between 5% and 20%, correction should be performed according to the above formula; if the control mortality rate is >20%, the experiment needs to be repeated.

[0082] The LC ratio of each drug was determined by linear regression analysis between the probability value of mortality and the logarithm of the series concentrations. 50 The co-toxicity coefficient (CTC) of the mixture was calculated using the Sun Yunpei method to evaluate the activity of the test agent against the test insects; the specific calculation formula is as follows:

[0083]

[0084] In the formula:

[0085] ATI – Actual Measured Toxicity Index of Mixtures;

[0086] S – LC50 of standard acaricides 50 The unit is milligrams per liter (mg / L);

[0087] M – LC of the mixture 50 The unit is milligrams per liter (mg / L).

[0088] TTI = TI A *P A +TI B *P B

[0089] In the formula:

[0090] TTI – Theoretical Toxicity Index of Mixtures;

[0091] TI A —A. Toxicity index of drug A;

[0092] P A —Percentage content of drug A in the mixture, expressed as percentage (%);

[0093] TI B —Toxicity index of drug B;

[0094] P B —Percentage content of agent B in the mixture, expressed as percentage (%).

[0095]

[0096] In the formula:

[0097] CTC – Cotoxicity Coefficient;

[0098] ATI – Actual Measured Toxicity Index of Mixtures;

[0099] TTI – Theoretical Toxicity Index of Mixtures.

[0100] According to the criteria for classifying combined effects: a co-toxicity coefficient (CTC) ≥ 120 indicates an synergistic effect, a co-toxicity coefficient (CTC) ≤ 80 indicates an antagonistic effect, and 80 < CTC < 120 indicates an additive effect.

[0101] Experimental results:

[0102] Combined toxicity assay of flufenoxuron and Acynonapyr at different ratios against adult female citrus red spider mites: Table 2 shows the results of flufenoxuron against adult female citrus red spider mites (LC50). 50 The value was 3.518 mg / L, indicating that Acynonapyr had an LC50 value of 3.518 mg / L against citrus red spider mites. 50 The value was 1.963 mg / L.

[0103] Flufenoxam and Acynonapyr did not show antagonistic effects on the control efficacy of citrus red spider mites in the range of 1:30–35:1, but showed a synergistic effect in the range of 1:20–25:1. When the ratio of flufenoxam to Acynonapyr was 3:4, the LC50 ratio was [not specified]. 50 The value was 1.068 mg / L, with the highest co-toxicity coefficient of 226.705.

[0104] Table 2. Results of indoor activity assays of flufenoxuron and Acynonapyr combination on adult female citrus red spider mites.

[0105]

[0106] Combined toxicity assay of flufenoxuron and Acynonapyr at different ratios against citrus red spider mite (nymph): Table 3 shows the results of flufenoxuron LC50 against citrus red spider mite. 50 The value was 3.971 mg / L, indicating that Acynonapyr had an LC50 value of 3.971 mg / L against citrus red spider mites. 50 The value was 5.428 mg / L. Flufenoxuron and Acynonapyr showed a synergistic effect in controlling citrus red spider mites within a ratio range of 1:20 to 25:1. The highest co-toxicity coefficient (232.117) was observed when the ratio of flufenoxuron to Acynonapyr was 1:2. 50 The value was 2.083 mg / L.

[0107] Table 3. Results of indoor activity assays of flufenoxuron and Acynonapyr combination against citrus red spider mites (nymphs).

[0108]

[0109] Formulation Examples

[0110] Preparation Example 1: 21% Flufenoxuron·Acynonapyr Suspension (9+12)

[0111] Formulation: Flufenoxam 9%, Acynonapyr 12%, sodium dioctyl succinate sulfonate 2%, EO-PO block copolymer 2%, styrene-phenol polyoxyethylene ether phosphate salt 3%, sodium polycarboxylate salt 1%, silicone defoamer 0.5%, xanthan gum 0.2%, magnesium aluminum silicate 1%, ethylene glycol 5%, sodium benzoate 0.5%, deionized water to 100%;

[0112] Formulation method: Add flufenoxuron and Acynonapyr to the wetting and dispersing agent and defoamer, stir well, and wet grind with zirconium beads using a sand mill until D is achieved. 90 (90% of the particles have a particle size) < 5 μm to obtain a pulverized slurry; add thickener, antifreeze, and preservative to the pulverized slurry and mix thoroughly, then add deionized water to make up to 100%, and shear at high speed to obtain a suspension. Preparation Example 2: 24% Flufenoxuron·Acynonapyr suspension (8+16)

[0113] Formulation: Flufenoxam 8%, Acynonapyr 16%, Alkyl naphthalene sulfonate formaldehyde condensate 3%, Sodium lignosulfonate 2%, EO-PO block copolymer 1%, Sodium dodecyl sulfate 2%, Organosilicon defoamer 0.5%, Xanthan gum 0.2%, Magnesium aluminum silicate 1%, Ethylene glycol 3%, Glycerin 2%, Sodium benzoate 0.5%, Deionized water to 100%;

[0114] Formulation method: Add flufenoxuron and Acynonapyr to the wetting and dispersing agent and defoamer, stir evenly, and wet grind using a sand mill with zirconium beads until D90 (the particle size of 90% of the particles) < 5 μm to obtain a pulverized slurry; add thickener, antifreeze, and preservative to the pulverized slurry and mix evenly, then add deionized water to make up to 100%, and shear at high speed to obtain a suspension. Preparation example 3: 40% flufenoxuron·Acynonapyr wettable powder (10+30)

[0115] Formulation: 10% flufenoxuron, 30% Acynonapyr, 15% sodium lignosulfonate, 3% sodium dodecyl sulfate, 6% bentonite, and kaolin to 100%;

[0116] Preparation method: First, pre-crush and mix evenly, then pulverize with an air jet mill until the fineness meets the requirement of at least 98 wt% passing through a 45 μm test sieve to obtain a wettable powder.

[0117] Preparation Example 4: 45% Flufenoxuron·Acynonapyr Wettable Powder (20+25)

[0118] Formulation: Flufenoxam 20%, Acynonapyr 25%, sodium lignosulfonate 12%, sodium dodecyl sulfate 3%, starch 10%, kaolin to 100%;

[0119] Preparation method: First, pre-crush and mix evenly, then pulverize with an air jet mill until the fineness meets the requirement of at least 98 wt% passing through a 45 μm test sieve to obtain a wettable powder.

[0120] Preparation Example 5: 32% Flufenoxuron·Acynonapyr Water Dispersible Granules (16+16)

[0121] Formulation: Flufenoxuron 16%, Acynonapyr 16%, lignin sulfonate 6%, naphthalene sulfonate formaldehyde condensate 10%, α-olefin sulfonate 2%, ammonium sulfate 2%, kaolin 20%, bentonite to 100%;

[0122] Preparation method: First, mix evenly, then pulverize to below 15μm using an air jet mill, mix evenly with water, granulate using a rotary granulator, dry at 60℃ until the moisture content is ≤3%, and sieve using 20-mesh and 60-mesh test sieves, discarding the large particles at the top and the dust filtered at the bottom to obtain water-dispersible granules.

[0123] Preparation Example 6: 8% Flufenoxuron·Acynonapyr EC (5:3)

[0124] Preparation formula: 5% flufenoxuron, 3% Acynonapyr, 15% DMF, 15% cyclohexanone, 3% calcium dodecylbenzenesulfonate, 12% styrene-phenol polyoxyethylene ether, and solvent oil to 100%;

[0125] Preparation method: Add the active ingredients to the cosolvent according to the formulation ratio of the example, and add surfactants and other functional additives thereto. Stir and mix evenly in a stirring mixing tank to obtain the emulsifiable oil product.

[0126] Preparation Example 7: 15% Flufenoxuron·Acynonapyr suspension emulsion (10:5)

[0127] Preparation formula: 10% flufenoxuron, 5% Acynonapyr, 20% cyclohexanone, 2% sodium lignosulfonate, 3% fatty amine polyoxyethylene ether, 2% polycarboxylate, 5% naphthalene sulfonate, 0.5% sodium p-hydroxybenzoate, 0.2% xanthan gum, 1% magnesium aluminum silicate, 3.5% propylene glycol, 0.5% glycerin, 0.2% silicone defoamer, and deionized water to 100%.

[0128] Preparation method: According to the formulation ratio in the example, Acynonapyr was completely dissolved in a solvent to prepare an oil phase; flufenoxuron, wetting and dispersing agent, antifreeze agent, defoamer, deionized water, etc., were wet-milled to D. 90 A suspension mother liquor with a particle size of less than 5 μm is prepared; after adding the oil phase to the suspension mother liquor and stirring evenly, a thickener is added and stirred and sheared evenly to prepare the suspension emulsion formulation of the composition of the present invention.

[0129] Preparation Example 8: 14% Flufenoxuron·Acynonapyr Dispersible Oil Suspension (8:6)

[0130] Preparation formula: 8% flufenoxuron, 6% Acynonapyr, 2% sodium diisooctyl sulfosuccinate, 3% fatty amine polyoxyethylene ether, 13% castor oil polyoxyethylene ether, 3% calcium dodecylbenzenesulfonate, 1% organic bentonite, and corn oil to make up to 100%.

[0131] Preparation method: According to the formulation ratio in the example, the active ingredients, surfactants and other functional additives are placed in the reaction vessel in sequence, solvent oil is added and mixed evenly, and then subjected to high-speed shearing, wet sand milling and finally homogenization filtration to obtain the dispersible oil suspension product.

[0132] field trials

[0133] Field trials for the control of citrus red spider mites

[0134] Test crop: Citrus;

[0135] Test subject: Citrus red spider mite;

[0136] Test period: Late April 2022;

[0137] Test location: Nanfeng, Jiangxi;

[0138] Pest occurrence: Citrus red spider mite infestation is relatively severe;

[0139] Experimental fields: The soil fertility of the experimental sites was moderate, the terrain was flat, the fertility was uniform, and the irrigation conditions were good. The cultivation conditions (soil type, fertilization, tillage, row spacing, etc.) of all experimental plots were uniform and consistent with local agricultural practices (GAP).

[0140] Experimental design: The formulation treatment, control treatment, and blank control were arranged in a randomized block design, with a plot size of 2 citrus trees and each treatment was replicated 4 times.

[0141] Table 4. Experimental treatments and drug dosages

[0142] Treatment number Pesticide Ingredient Amount g a.i / hm 2 ]] Treatment 1, 2 24% fluensulfone·Acynonapyr suspension concentrate 30、60 Treatment 3, 4 45% fluensulfone·Acynonapyr wettable powder 30、60 Treatment 5, 6 32% fluensulfone·Acynonapyr water dispersible granule 30、60 Control 1 20% Acynonapyr suspension concentrate 60 Control 2 20% fluensulfone suspension concentrate 60 Control 3 Water blank control /

[0143] Spraying method: Spray treatment. The spraying equipment is the WS-16D Guardian electric sprayer with a single fan-shaped mist nozzle. The working pressure is 0.15-0.4 MPa. According to the dosage requirements, the amount of pesticide should be accurately measured according to the area of ​​the plot.

[0144] The weather was good during the experiment. On the day of application, the weather was sunny with an average daily temperature of 22°C, a high of 27°C, a low of 19°C, a level 1 easterly wind, and a relative humidity of 65%.

[0145] Survey method: Mark the tender shoots of each tree in five directions (east, west, south, north, and center) in each plot. For each plot, mark 20 leaves on each tree and conduct the survey. The number of mites before treatment should not be less than 200. The number of live mites should be surveyed 3 days and 14 days after application of the pesticide.

[0146] Methods for calculating drug efficacy:

[0147]

[0148]

[0149] During the experiment, the citrus trees in each treatment plot grew well, and no pesticide damage was observed in any treatment.

[0150] Field trial results:

[0151] Table 5. Results of field trials on citrus red spider mite using different tested pesticides.

[0152]

[0153] Note: The efficacy (%) in the table above is the average of each replicate. Capital letters indicate significant differences at the 1% level.

[0154] Field trial results (Table 5) showed that different tested pesticides had good control effects on citrus red spider mites. Three days after application, the acaricide combination of flufenoxuron and Acynonapyr showed a control efficacy of over 80% against citrus red spider mites, with each combination exhibiting good rapid-acting properties. Fourteen days after application, the acaricide combination of flufenoxuron and Acynonapyr showed a control efficacy of over 85% against citrus red spider mites, with each combination exhibiting good sustained efficacy. The experimental data were processed using the Duncan multiple range method with IBM SPSS data processing software. The analysis of variance results showed that, at 0.01, there were significant differences between each combination group and the control group.

[0155] According to the experimental results, when citrus red spider mites first appear, the use of various compound acaricides can effectively control their damage in a short period of time and reduce the economic losses caused by pests to citrus. It is recommended that the pesticides be sprayed evenly, with a focus on spraying the undersides of the leaves.

[0156] Through indoor toxicity testing and field trials on citrus trees, the acaricidal composition of flufenoxuron and Acynonapyr described in this invention exhibits good control efficacy against phytophagous mites. The acaricidal composition or formulation obtained by this invention demonstrates significant efficacy, superior to single agents in delaying the development of resistance and prolonging its duration of action. Furthermore, no phytotoxicity was observed in the experiments, indicating that the enhanced synergistic effect of the acaricidal composition or formulation reduces production and application costs while ensuring crop safety.

[0157] The exemplary embodiments have been chosen and described in order to explain the specific principles of the invention and its practical application, thereby enabling those skilled in the art to implement and utilize various exemplary embodiments of the invention, as well as various alternatives and modifications. The scope of the invention is intended to be defined by the claims and their equivalents.

Claims

1. A mite-killing composition, characterized in that: It includes active ingredient A, flufenoxuron, and active ingredient B, Acynonapyr, wherein the mass ratio of flufenoxuron to Acynonapyr is 1:20 to 25:

1.

2. The acaricide composition according to claim 1, characterized in that, The mass ratio of flufenoxuron to Acynonapyr is 1:20, 1:15, 1:12, 2:17, 2:15, 1:6, 1:3, 1:2, 3:4, 15:2, 8:1, 12:1, 15:1, and 25:

1.

3. The acaricide composition according to claim 1, characterized in that, Based on a total weight of 100 wt% of the acaricide composition, the sum of the contents of active ingredient A and active ingredient B in the acaricide composition is 1 to 95 wt%.

4. The acaricide composition according to claim 3, characterized in that, Based on a total weight of 100 wt% of the acaricide composition, the sum of the contents of active ingredient A and active ingredient B in the acaricide composition is 5-45 wt%.

5. The acaricide composition according to claim 1, characterized in that, In addition to the active ingredient, the acaricide composition also includes auxiliary ingredients, which are selected from one or more of the following: wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreeze agents, defoamers, solvents, preservatives, stabilizers, synergists, or carriers.

6. The acaricide composition according to claim 5, characterized in that, The formulations prepared from the acaricidal composition are wettable powders, water-dispersible granules, emulsifiable concentrates, water-emulsions, microemulsions, suspensions, suspension emulsions, and dispersible oil suspensions.

7. The use of the acaricidal composition according to any one of claims 1-6 in the control of harmful mites, characterized in that, The pest mentioned is the citrus red spider mite.

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