A mite-killing composition

Abstract

The present invention belongs to the field of pesticide technology and relates to a mite-killing composition. The active ingredients of the mite-killing composition include active ingredient A and active ingredient B. Active ingredient A is a compound of formula (I), and active ingredient B is selected from any one of flupentiofenox, aceynonapyr, or bisulflufen. The mass ratio of active ingredient A to active ingredient B is 1:30 to 56:1. The mite-killing composition or its formulation of the present invention can enhance efficacy, expand the mite-killing spectrum, reduce usage costs, reduce dosage, extend the duration of effect, and delay the development of drug resistance.

Description

Technical Field

[0001] The present invention relates to the technical field of pesticide compounding, in particular to an acaricidal composition. The acaricidal composition or its preparation can enhance drug efficacy, reduce drug dosage, and at the same time improve quick-acting property, prolong the duration of effect and delay the development of drug resistance. Background Art

[0002] Flupentiofenox was developed by Kumihiko Chemical Industries, Ltd., Japan, under the development code KⅡ-9396. (RS)-[5-[4-chloro-2-fluoro-5-[(2,2,2-trifluoroethyl)sulfinyl]phenoxy]pentyl]trifluoromethyl sulfide; CAS registration number: 1472050-04-6; molecular formula: C 14 H 14 ClF7O2S2.

[0003] Acynonapyr, a novel acaricide with a cyclic amine backbone developed by Japan Soda Co., Ltd., acts on inhibitory glutamate receptors (IGluRs), interfering with neurotransmission in mites. This deprives muscle cells of their ability to move, resulting in a paralysis-like state. This in turn affects feeding and movement, ultimately killing the mites. It has excellent control effects on mites in fruit trees, vegetables, and tea plants.

[0004] Bisulflufen was first discovered in 2014 by Shenyang Sinochem Pesticide Chemical Research and Development Co., Ltd., a subsidiary of Yangnong Chemical. It is a systemic acaricide of the trifluoroethyl sulfide class with a novel structure, unique mechanism of action, and is safe and highly effective.

[0005] In the agricultural production process, chemical agents are the most effective means of preventing and controlling pests and diseases. The long-term continuous high-dose use of a single chemical agent can easily lead to a series of problems such as the development of resistance in pest mites and environmental pollution. Reasonable compounding or mixing of chemical agents has the positive characteristics of expanding the acaricide spectrum, improving the control effect, extending the appropriate period for application, reducing the dosage, reducing drug damage, reducing residues, and delaying the occurrence of pest tolerance and resistance. The applicant was surprised to find through indoor toxicity tests and field efficacy tests that the combination of the compound of formula (I) with Flupentiofenox, Acynonapyr or Bisulflufen has a significant synergistic effect, and the above-mentioned compounded acaricide composition and its application have not been reported so far. Summary of the Invention

[0006] Based on the above situation, the purpose of the present invention is to provide a mite-killing composition and its preparation, which are mainly used to control herbivorous mites. The mite-killing composition or its preparation can enhance the efficacy, reduce the dosage, and at the same time prolong the lasting effect and delay the development of drug resistance.

[0007] In order to achieve the above object, the present invention provides the following technical solution: an acaricidal composition comprising an active ingredient A and an active ingredient B, wherein the active ingredient A is a compound of formula (I): Active ingredient B is any one of Flupentiofenox, Acynonapyr or Bisulflufen;

[0008] Furthermore, the mass ratio of the active ingredient A to the active ingredient B is 1:30 to 56:1;

[0009] Furthermore, the mass ratio of the compound of formula (I) to Flupentiofenox is 1:30 to 56:1;

[0010] Furthermore, the mass ratio of the compound of formula (I) to Flupentiofenox is 1:20 to 28:1;

[0011] Furthermore, the mass ratio of the compound of formula (I) to Flupentiofenox is 1:30, 1:20, 1:15, 1:7, 2:1, 7:1, 14:1, 28:1, and 56:1;

[0012] Furthermore, the mass ratio of the compound of formula (I) to Flupentiofenox is 1:20, 1:15, 1:7, 2:1, 7:1, 14:1, and 28:1;

[0013] Furthermore, the mass ratio of the compound of formula (I) to Acynonapyr is 1:25 to 50:1;

[0014] Furthermore, the mass ratio of the compound of formula (I) to Acynonapyr is 1:25 to 20:1;

[0015] Furthermore, the mass ratio of the compound of formula (I) to Acynonapyr is 1:25, 1:10, 1:5, 2:1, 5:1, 10:1, 20:1, 50:1;

[0016] Furthermore, the mass ratio of the compound of formula (I) to Acynonapyr is 1:10, 1:5, 2:1, 5:1, 10:1, 20:1;

[0017] Furthermore, the mass ratio of the compound of formula (I) to Bisulflufen is 1:20 to 35:1;

[0018] Furthermore, the mass ratio of the compound of formula (I) to Bisulflufen is 1:20 to 17:1;

[0019] Furthermore, the mass ratio of the compound of formula (I) to Bisulflufen is 1:20, 1:15, 1:3, 1:1, 3:1, 8:1, 17:1, and 35:1;

[0020] Furthermore, the mass ratio of the compound of formula (I) to Bisulflufen is 1:15, 1:3, 1:1, 3:1, 8:1, and 17:1;

[0021] A mite-killing composition, wherein the total weight of the mite-killing composition is 100 wt%, and the sum of the active ingredient A and the active ingredient B in the mite-killing composition is 1 to 95 wt%;

[0022] Furthermore, based on the total mass of the acaricidal composition being 100 wt%, the sum of the contents of the active ingredient A and the active ingredient B in the acaricidal composition is 5 to 50 wt%;

[0023] Furthermore, based on the total mass of the acaricidal composition as 100 wt%, the sum of the contents of the active ingredient A and the active ingredient B in the acaricidal composition is 20 wt%, 24 wt%, 30 wt%, 34 wt%, 36 wt%, 48 wt%, 50 wt%, and 54 wt%;

[0024] Furthermore, the acaricidal composition further comprises an adjuvant, which is selected from one or more of a wetting agent, a dispersant, an emulsifier, a thickener, a disintegrant, an antifreeze agent, a defoaming agent, a solvent, a preservative, a stabilizer, a synergist and a carrier;

[0025] The wetting agent is selected from one or more of alkylbenzene sulfonate, alkylnaphthalene sulfonate, lignin sulfonate, sodium lauryl sulfate, sodium dioctyl sulfosuccinate, α-olefin sulfonate, alkylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, alkylphenol ethoxylate, fatty alcohol ethoxylate, fatty alcohol polyoxyethylene ether sodium sulfate, silkworm feces, soapberry powder, soapberry powder, SOPA, detergent, emulsifier 2000 series and wetting penetrant F; and / or

[0026] The dispersant is selected from one or more of lignin sulfonate, alkylnaphthalene sulfonate formaldehyde condensate, naphthalene sulfonate, tristyrylphenol ethoxylate phosphate, fatty alcohol ethoxylate, alkylphenol polyoxyethylene ether, alkylphenol polyoxyethylene ether methyl ether condensate sulfate, fatty amine polyoxyethylene ether, glycerol fatty acid ester polyoxyethylene ether, polycarboxylates, polyacrylic acids, phosphates, EO-PO block copolymers and EO-PO graft copolymers; and / or

[0027] The emulsifier is selected from one or more of calcium dodecylbenzenesulfonate, alkylphenol formaldehyde resin polyoxyethylene ether, phenylethylphenol polyoxyethylene polyoxypropylene ether, fatty alcohol ethylene oxide-propylene oxide copolymer, styrylphenol polyoxyethylene ether, castor oil polyoxyethylene ether and alkylphenol ether phosphate; and / or

[0028] The thickener is selected from one or more of xanthan gum, organobentonite, gum arabic, sodium alginate, magnesium aluminum silicate, carboxymethyl cellulose and white carbon black; and / or

[0029] 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

[0030] The antifreeze agent is selected from one or more of alcohols, alcohol ethers, chlorinated hydrocarbons and inorganic salts; and / or

[0031] Defoaming agent selected from C 10 -C 20 Saturated fatty acid compounds, silicone oil, silicone compounds, C8-C 10 One or more of fatty alcohols; and / or

[0032] The solvent is selected from one or more of benzene, toluene, xylene, durene, methanol, ethanol, isopropanol, n-butanol, dimethyl sulfoxide, dimethylformamide, cyclohexanone, alkylene carbonate, diesel, solvent oil, vegetable oil, vegetable oil derivatives and water; and / or

[0033] The preservative is selected from one or more of propionic acid, sodium propionic acid, sorbic acid, sodium sorbic acid, potassium sorbic acid, benzoic acid, sodium benzoic acid, sodium p-hydroxybenzoic acid, methyl p-hydroxybenzoate, kasone and 1,2-benzisothiazolin-3-one; and / or

[0034] The stabilizer is selected from one or more of 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, white carbon black, talc, montmorillonite and starch; and / or

[0035] Synergists are selected from synergist, piperonyl butoxide; and / or

[0036] The carrier is selected from one or more of ammonium salts, ground natural minerals, ground artificial minerals, silicates, resins, waxes, solid fertilizers, water, organic solvents, mineral oils, vegetable oils and vegetable oil derivatives.

[0037] The present invention optimizes the content of active ingredients and adjuvants in the acaricidal composition to achieve a better balance between toxicity and residue, thereby enhancing efficacy, reducing dosage and lowering costs.

[0038] Furthermore, the pesticide composition can be prepared into an agriculturally acceptable formulation, wherein the formulation is selected from a solid formulation and / or a liquid formulation;

[0039] Furthermore, the solid preparation is selected from wettable powders and water-dispersible granules; the liquid preparation is selected from emulsifiable concentrates, aqueous emulsions, microemulsions, suspensions, suspoemulsions, and dispersible oil suspensions.

[0040] The specific embodiments of the pesticide formulation prepared by the acaricidal composition of the present invention are as follows:

[0041] When the acaricide composition is a wettable powder, the components by mass are: 1-40 parts of active ingredient A; 1-40 parts of active ingredient B; 3-10 parts of dispersant; 1-5 parts of wetting agent; and the balance is made up of fillers.

[0042] The specific production steps of the wettable powder are: mixing the active ingredients, dispersant, wetting agent and filler according to the above formula, stirring them uniformly in a mixer, and mixing them uniformly after air flow crushing to prepare the wettable powder of the composition of the present invention.

[0043] When the acaricide composition is a water-dispersible granule, the components by mass are 1-40 parts of active ingredient A; 1-40 parts of active ingredient B; 3-10 parts of dispersant; 1-10 parts of wetting agent; 1-5 parts of disintegrant; and the balance is made up of filler.

[0044] The specific production steps of the water-dispersible granules are as follows: the active ingredients and the dispersant, wetting agent, disintegrant and filler are uniformly mixed according to the above formula, crushed with an ultra-fine airflow mill, kneaded, and then added to a fluidized bed granulation dryer for granulation, drying, screening, and sampling and analysis, thereby producing the water-dispersible granules of the composition of the present invention.

[0045] When the acaricide composition is an emulsifiable concentrate preparation, the components by weight are: 1-40 parts of active ingredient A; 1-40 parts of active ingredient B; 10-30 parts of conventional emulsifier; 20-50 parts of conventional solvent; and 1-5 parts of conventional synergist.

[0046] The specific production steps of the emulsifiable concentrate preparation are: firstly, adding the active ingredient into a solvent and completely dissolving it, then adding an emulsifier and a synergist, stirring evenly to form a uniform and transparent oily liquid, and filling it to prepare the emulsifiable concentrate preparation of the composition of the present invention.

[0047] When the acaricide composition is an aqueous emulsion, the components by mass are: 1-40 parts of active ingredient A; 1-40 parts of active ingredient B; 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 defoaming agent; 0.2-2 parts of thickener; and deionized water makes up the balance.

[0048] The specific production steps of the aqueous emulsion are as follows: first, active ingredients, solvent, emulsifier and cosolvent are added together to dissolve into a uniform oil phase; deionized water, antifreeze agent, antimicrobial agent and other pesticide adjuvants are mixed together to form a uniform aqueous phase; while stirring at high speed in a reactor, 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 aqueous emulsion, thereby preparing the aqueous emulsion of the composition of the present invention.

[0049] When the acaricide composition is a microemulsion, the components by mass are: 1-40 parts of active ingredient A; 1-40 parts of active ingredient B; 10-30 parts of emulsifier; 1-8 parts of antifreeze; 0.5-10 parts of stabilizer; and 20-50 parts of conventional solvent cosolvent.

[0050] The specific production steps of the microemulsion are: completely dissolving the active ingredient with a cosolvent, then adding other ingredients such as an emulsifier and an antifreeze stabilizer, mixing them evenly, and finally adding water and stirring thoroughly to prepare the microemulsion.

[0051] When the acaricide composition is a suspension concentrate, the components in parts by mass are: 1 to 40 parts of active ingredient A; 1 to 40 parts of active ingredient B; 1 to 10 parts of wetting and dispersing agent; 1 to 5 parts of antifreeze agent; 0.1 to 2 parts of thickener; 0.1 to 0.8 parts of defoaming agent; 0 to 10 parts of solvent; 1 to 5 parts of stabilizer; and deionized water makes up the balance.

[0052] The specific production steps of the suspension are: using zirconium beads, wet grinding with a sand mill to D 90 (90% of the particle size) <5 μm, the suspension preparation of the composition of the present invention can be prepared.

[0053] When the insecticide composition is a suspoemulsion, the components by mass are: 1-40 parts of active ingredient A; 1-40 parts of active ingredient B; 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 defoaming agent; 1-40 parts of solvent; 1-5 parts of stabilizer; and deionized water makes up the balance.

[0054] The specific production steps of the suspoemulsion are as follows: the active ingredient B is completely dissolved with a solvent to prepare an oil phase; the active ingredient A is mixed with a wetting dispersant, an antifreeze agent, a defoaming agent, deionized water, etc. by wet sand grinding until D 90 The suspension mother liquid is prepared by adding the oil phase into the suspension mother liquid and stirring evenly, and then adding the thickener and stirring and shearing evenly to prepare the suspoemulsion preparation of the composition of the present invention.

[0055] When the insecticide composition is a dispersible oil suspension, the components by mass are: 1-40 parts of active ingredient A; 1-40 parts of active ingredient B; 1-10 parts of wetting and dispersing agent; 0.1-2 parts of thickener; 0.1-0.8 parts of defoaming agent; 0-10 parts of solvent; 1-5 parts of stabilizer; and the balance is made up of vegetable oil.

[0056] The specific production steps of the dispersible oil suspension are: using zirconium beads, wet grinding with a sand mill to D 90 (90% of the particles have a particle size) < 5 μm, the dispersible oil suspension preparation of the composition of the present invention can be prepared.

[0057] Use of the acaricidal composition of the present invention in preventing and controlling harmful mites;

[0058] Furthermore, the pest mites are herbivorous pest mites;

[0059] Furthermore, the herbivorous pest mites are Tetranychus cinnabarinus, Tetranychus truncatus, Tetranychus two-spotted, and Citrus red spider;

[0060] Furthermore, the acaricidal composition and / or its preparation is applied in an effective dose to the harmful mites to be controlled and / or the medium where they grow.

[0061] Compared with the prior art, the beneficial effects of the technical solution of the present invention are as follows:

[0062] (1) The compound acaricide of the present invention has a significant synergistic effect compared to a single agent, thereby improving the control effect;

[0063] (2) The compound acaricide of the present invention improves the control effect while reducing the dosage, cost and residue;

[0064] (3) The compound acaricide of the present invention is a compound of two agents with different mechanisms of action, has no cross-resistance, and is beneficial for delaying the development of drug resistance in mites. DETAILED DESCRIPTION

[0065] In order to make the technical solutions, objectives and advantages of the present invention more clearly understood, 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.

[0066] Indoor toxicity assay

[0067] Test insect source: Tetranychus cinnabarinnum Boisduval;

[0068] Test drugs: technical drug of the compound of formula (I), Flupentiofenox technical drug, Acynonapyr technical drug, Bisulflufen technical drug, all provided by the Group's R&D Center;

[0069] Material Preparation: Select female adult mites raised indoors and in consistent physiological condition. Cut double-sided tape into 2 cm lengths and attach to one end of a glass slide. Select healthy mites and attach their backs to the tape, 30 per slide. Place mites in a container lined with a damp sponge, cover, and store at (25 ± 1)°C. After 2 hours, examine under a microscope, remove dead and injured individuals, and replenish the remaining mites per slide.

[0070] Preparation of drugs: The original drug was prepared into a mother solution with acetone, and the mother solution was prepared into test drugs with different proportions using 0.1% Tween-80 aqueous solution;

[0071] Chemical treatment: Immerse the glass slide in the drug solution and shake it gently for 5 seconds, then take it out and absorb the excess drug solution with absorbent paper. Place it on a white porcelain plate with a wet sponge, cover it with a plastic film with good light transmittance, and place it at (25±1)℃ for observation.

[0072] Each treatment was repeated 4 times, and a treatment without drug was set as a blank control.

[0073] Test investigation: 48 hours after treatment, check the mortality of test insects, record the total number of insects and the number of dead insects, and calculate the mortality rate:

[0074]

[0075] Where:

[0076] P——mortality rate, in percentage (%);

[0077] K——indicates the number of dead insects, the unit is head;

[0078] N——represents the total number of insects processed, in heads.

[0079]

[0080] Where:

[0081] P1——adjusted mortality rate, in percentage (%);

[0082] P t ——Treatment mortality rate, expressed in percentage (%);

[0083] P0 - blank control mortality rate, in percentage (%).

[0084] If the control mortality rate is less than 5%, no correction is required; if the control mortality rate is between 5% and 20%, correction should be made according to the above formula; if the control mortality rate is greater than 20%, the test needs to be repeated.

[0085] The LC value of each drug was calculated by linear regression analysis (DPS) between the probability value of mortality and the logarithm of the serial concentration. 50 The co-toxicity coefficient (CTC) of the mixture was calculated using the Sun Yunpei method to evaluate the activity of the test agents against the test insects. The specific calculation formula is as follows:

[0086]

[0087] Where:

[0088] ATI - measured toxicity index of mixture;

[0089] S——LC of standard acaricide 50 , the unit is milligrams per liter (mg / L);

[0090] M——LC of the mixture 50 , the unit is milligrams per liter (mg / L).

[0091] TTI=TI A *P A +TI B *P B

[0092] Where:

[0093] TTI – Theoretical Toxicity Index of Mixtures;

[0094] TI A ——Agent toxicity index;

[0095] P A ——The percentage of agent A in the mixture, in percentage (%);

[0096] TI B ——Toxicity index of agent B;

[0097] P B ——The percentage of agent B in the mixture, in percentage (%).

[0098]

[0099] Where:

[0100] CTC – Co-toxicity coefficient;

[0101] ATI - measured toxicity index of mixture;

[0102] TTI - Theoretical Toxicity Index of Mixture.

[0103] According to the classification standard of joint effects: a co-toxicity coefficient (CTC) ≥ 120 indicates a synergistic effect, a co-toxicity coefficient (CTC) ≤ 80 indicates an antagonistic effect, and a co-toxicity coefficient (CTC) 80 < 120 indicates an additive effect.

[0104] Test results:

[0105] The compound of formula (I) has an LC activity against Tetranychus cinnabarinus (female adult mite). 50 The toxicity test results of different ratios of the compound of formula (I) and Flupentiofenox on Tetranychus cinnabarinus (female adult mites) are shown in Table 1. The LC value of Flupentiofenox on Tetranychus cinnabarinus is 17.7079 mg / L. 50 The value is 1.2464 mg / L. The control effect of the compound of formula (I) and Flupentiofenox on Tetranychus cinnabarinus in the range of 1:30 to 56:1 showed an additive or synergistic effect. The mass ratio of the compound of formula (I) to Flupentiofenox was 1:20 to 28:1, and the co-toxicity coefficient was greater than 130, with a significant synergistic effect. When the mass ratio of the compound of formula (I) to Flupentiofenox was 7:1, the co-toxicity coefficient was the highest, which was 217.22. 50 The value is 3.0752 mg / L.

[0106] Table 1 Toxicity test results of different ratios of compound of formula (I) and Flupentiofenox against Tetranychus cinnabarinus (female adult mites)

[0107]

[0108] The results of the toxicity test of different ratios of the compound of formula (I) and Acynonapyr on Tetranychus cinnabarinus (female adult mites) are shown in Table 2. 50 The value is 1.6811 mg / L. The compound of formula (I) and Acynonapyr show a synergistic effect on the control of Tetranychus cinnabarinus in the range of 1:25 to 50:1. The mass ratio of the compound of formula (I) to Acynonapyr is 1:10 to 50:1, and the co-toxicity coefficient is greater than 130, with a significant synergistic effect. When the mass ratio of the compound of formula (I) to Acynonapyr is 5:1, the co-toxicity coefficient is the highest, which is 251.89. LC 50 The value is 2.7154 mg / L.

[0109] Table 2 Toxicity test results of different ratios of the compound of formula (I) and Acynonapyr against Tetranychus cinnabarinus (female adult mites)

[0110]

[0111]

[0112] The results of the toxicity test of different ratios of the compound of formula (I) and Bisulflufen on Tetranychus cinnabarinus (female adult mites) are shown in Table 3. 50 The value is 1.0571 mg / L. The compound of formula (I) and Bisulflufen show a synergistic effect on the control of spider mites in the range of 1:20 to 35:1. The mass ratio of the compound of formula (I) to Bisulflufen is 1:15 to 17:1, and the co-toxicity coefficient is greater than 130, with a significant synergistic effect. When the mass ratio of the compound of formula (I) to Bisulflufen is 3:1, the co-toxicity coefficient is the highest, which is 262.32. LC 50 The value is 1.3671 mg / L.

[0113] Table 3 Toxicity test results of different ratios of compound of formula (I) and Bisulflufen to Tetranychus cinnabarinus (female adult mites)

[0114]

[0115] Formulation Examples

[0116] Preparation Example 1:

[0117] 24% formula (I) compound flupentiofenox suspension (7:1)

[0118] Preparation formula: 21% of compound of formula (I), 3% of flupentiofenox, 2% of sodium dioctyl sulfosuccinate, 2% of EO-PO block copolymer, 2.5% of styrylphenol polyoxyethylene ether phosphate, 1% of sodium polycarboxylate, 0.5% of organosilicon defoamer, 0.2% of xanthan gum, 1% of magnesium aluminum silicate, 5% of ethylene glycol, 0.5% of sodium benzoate, and the balance is made up of deionized water;

[0119] Preparation method: Add active ingredients to the wetting dispersant and defoamer, stir evenly, use zirconium beads, and wet grind with a sand mill to D 90 (90% of the particle size) <5 μm, to obtain a crushed slurry; add a thickener, an antifreeze agent, and a preservative to the crushed slurry and mix them evenly, add deionized water to 100%, and shear at high speed to obtain a suspension.

[0120] Preparation Example 2:

[0121] 30% formula (I) compound·acynonapyr suspension (5:1)

[0122] Preparation formula: 25% of compound of formula (I), 5% of acynonapyr, 2% of sodium dioctyl sulfosuccinate, 2.5% of sodium lignin sulfonate, 2.5% of styrylphenol polyoxyethylene ether phosphate, 1% of sodium polycarboxylate, 0.5% of organosilicon defoamer, 0.2% of xanthan gum, 1% of magnesium aluminum silicate, 5% of glycerol, 0.5% of sodium benzoate, and deionized water to make up the balance;

[0123] Preparation method: Add active ingredients to the wetting dispersant and defoamer, stir evenly, use zirconium beads, and wet grind with a sand mill to D 90 (90% of the particle size) <5 μm, to obtain a crushed slurry; add a thickener, an antifreeze agent, and a preservative to the crushed slurry and mix them evenly, add deionized water to 100%, and shear at high speed to obtain a suspension.

[0124] Preparation Example 3:

[0125] 20% formula (I) compound·bisulflufen suspension (3:1)

[0126] Preparation formula: 15% of the compound of formula (I), 5% of bisulflufen, 2% of EO-PO block copolymer, 3% of styrylphenol polyoxyethylene ether phosphate salt, 1% of sodium polycarboxylate, 0.5% of organosilicon defoamer, 0.25% of xanthan gum, 1% of magnesium aluminum silicate, 5% of ethylene glycol, 0.5% of sodium benzoate, and the balance made up with deionized water;

[0127] Preparation method: Add active ingredients to the wetting dispersant and defoamer, stir evenly, use zirconium beads, and wet grind with a sand mill to D 90 (90% of the particle size) <5 μm, to obtain a crushed slurry; add a thickener, an antifreeze agent, and a preservative to the crushed slurry and mix them evenly, add deionized water to 100%, and shear at high speed to obtain a suspension.

[0128] Preparation Example 4:

[0129] 50% compound of formula (I)·flupentiofenox water dispersible granules (4:1)

[0130] Preparation formula: 40% of the compound of formula (I), 10% of flupentiofenox, 6% of sodium lignin sulfonate, 10% of naphthalene sulfonate formaldehyde condensate, 2% of α-olefin sulfonate, 2% of ammonium sulfate, 20% of kaolin, and the balance of bentonite;

[0131] Preparation method: First mix evenly, then grind to less than 15μm by air flow mill, mix evenly with water, granulate by extrusion granulator, dry to a moisture content of ≤3%, select 20 mesh and 60 mesh test sieves for sieving, discard the large particles on the top and the dust filtered at the bottom to prepare water dispersible granules.

[0132] Preparation Example 5:

[0133] 36% formula (Ⅰ) compound·acynonapyr water dispersible granules (7:2)

[0134] Preparation formula: 28% of compound of formula (I), 8% of acynonapyr, 5% of sodium lignin sulfonate, 10% of naphthalene sulfonate formaldehyde condensate, 2% of sodium polycarboxylate, 2% of sodium lauryl sulfate, 2% of ammonium sulfate, 20% of kaolin, and the balance of bentonite;

[0135] Preparation method: First mix evenly, then grind to less than 15μm by air flow mill, mix evenly with water, granulate by extrusion granulator, dry to a moisture content of ≤3%, select 20 mesh and 60 mesh test sieves for sieving, discard the large particles on the top and the dust filtered at the bottom to prepare water dispersible granules.

[0136] Preparation Example 6:

[0137] 48% Formula (I) compound·bisulflufen water dispersible granules (5:1)

[0138] Preparation formula: 30% of the compound of formula (I), 18% of bisulflufen, 8% of calcium lignin sulfonate, 10% of naphthalene sulfonate formaldehyde condensate, 2% of sodium lauryl sulfate, 2% of ammonium sulfate, 20% of kaolin, and the balance of bentonite;

[0139] Preparation method: First mix evenly, then grind to less than 15μm by air flow mill, mix evenly with water, granulate by extrusion granulator, dry to a moisture content of ≤3%, select 20 mesh and 60 mesh test sieves for sieving, discard the large particles on the top and the dust filtered at the bottom to prepare water dispersible granules.

[0140] Preparation Example 7:

[0141] 34% formula (I) compound flupentiofenox wettable powder (15:2)

[0142] Preparation formula: 30% of the compound of formula (I), 4% of flupentiofenox, 10% of sodium lignin sulfonate, 5% of naphthalene sulfonate formaldehyde condensate, 3% of sodium lauryl sulfate, 6% of bentonite, and kaolin to make up the balance;

[0143] Preparation method: pre-crush and mix evenly, then grind by air flow mill to a fineness that satisfies the requirement that at least 98 wt% passes through a 45 μm test sieve to obtain a wettable powder.

[0144] Preparation Example 8:

[0145] 54% formula (Ⅰ) compound acynonapyr wettable powder (5:1)

[0146] Preparation formula: 45% of the compound of formula (I), 9% of acynonapyr, 10% of sodium lignin sulfonate, 5% of naphthalene sulfonate formaldehyde condensate, 3% of sodium lauryl sulfate, 4% of bentonite, 3% of starch, and kaolin to make up the balance;

[0147] Preparation method: pre-crush and mix evenly, then grind by air flow mill to a fineness that satisfies the requirement that at least 98 wt% passes through a 45 μm test sieve to obtain a wettable powder.

[0148] Field trials

[0149] Field trials for controlling Tetranychus cinnabarinus

[0150] Test crops: Eggplant;

[0151] Test subjects: Tetranychus cinnabarinus;

[0152] Trial time: late June 2023;

[0153] Experimental location: Eggplant planting field in Xiazhuang, Chengyang District, Qingdao City;

[0154] Pest occurrence: The damage caused by spider mites is relatively high;

[0155] Experimental plots: The soil fertility of the experimental plots is moderate, the terrain is flat, the fertility is uniform, and the irrigation conditions are good. The cultivation conditions (soil type, fertilization, tillage, row spacing, etc.) of all experimental plots are uniform and consistent with local agricultural cultivation practices (GAP).

[0156] Experimental design: Preparation treatment, control treatment and blank control were arranged in random blocks with a plot area of ​​20m 2 , each treatment was repeated 4 times.

[0157] Table 4 Experimental treatment and dosage

[0158]

[0159] Spraying method: spray treatment, the spraying equipment is WS-16D Guardian electric sprayer, the nozzle is a single fan-shaped mist nozzle, the working pressure is 0.15-0.4Mpa, according to the dosage requirements of the pesticide and the area of ​​the plot, accurately measure the dosage.

[0160] The weather was good during the test period. On the day of application, the weather was sunny, with a force 1 east wind and a relative humidity of 65%.

[0161] Survey method: 10 eggplant plants were selected from each plot, and 10 leaves were surveyed from each plant. The base number of spider mites was surveyed before the application of pesticides, and the number of surviving mites was surveyed 1 and 7 days after the application of pesticides.

[0162] Calculation method of drug efficacy:

[0163]

[0164]

[0165] During the experiment, eggplants in each treatment plot grew well and no phytotoxicity was observed in any treatment.

[0166] Field trial results:

[0167] Table 5 Field test results of different test agents on Tetranychus cinnabarinus on eggplant

[0168]

[0169]

[0170] Note: The control efficacy (%) in the above table is the average of each replicate. Lowercase letters indicate significant differences at the 5% level.

[0171] The results of the field test showed (Table 5) that the different test agents had good control effects on eggplant spider mites. Three days after application, the control efficacy of 24% formula (I) compound·flupentiofenox suspension concentrate (7:1), 30% formula (I) compound·acynonapyr suspension concentrate (5:1), and 48% formula (I) compound·bisulflufen water dispersible granules (5:1) against spider mites was above 80%, and each combination showed good rapid effect. Seven days after application, the control efficacy of 24% formula (I) compound·flupentiofenox suspension concentrate (7:1), 30% formula (I) compound·acynonapyr suspension concentrate (5:1), and 48% formula (I) compound·bisulflufen water dispersible granules (5:1) against spider mites was 95.07%, 97.18%, and 96.07%, respectively. Each combination showed good long-term effect. SPSS data processing software was used to process the experimental data using Duncan's new multiple range method. The results of variance analysis showed that at the 0.05 level, there were significant differences between each compound group and the control group.

[0172] According to the test results, during the initial outbreak of Tetranychus cinnabarinus, the use of various compound acaricides can effectively control its damage in a short period of time and reduce the economic losses caused by pests to crops. It is recommended to spray evenly and focus on spraying the back of leaves.

[0173] Indoor toxicity assays and field trials have shown that the acaricidal compositions of the present invention, formulated with the compound of formula (I) and flupentiofenox, aceynonapyr, or bisulflufen, demonstrate excellent control efficacy against phytophagous mites. The resulting acaricidal compositions or formulations exhibit significant control efficacy, outperforming single agents in delaying the development of resistance and prolonging their effectiveness. Furthermore, no crop damage was observed with the combined formulations, demonstrating that the enhanced synergistic acaricidal effects of the resulting acaricidal compositions or formulations can reduce production and use costs and are safe for crops.

[0174] The purpose of selecting and describing the exemplary embodiments is to explain the specific principles of the present invention and its practical application, so that those skilled in the art can realize and utilize various exemplary embodiments and various choices and changes of the present invention. The scope of the present invention is intended to be defined by the claims and their equivalents.

Claims

1. A mite-killing composition, characterized in that: The acaricidal composition comprises an active ingredient A and an active ingredient B, wherein the active ingredient A is a compound of formula (I): (I), active ingredient B is flupentiofenox, and the mass ratio of the compound of formula (I) to flupentiofenox is 1:20~28:

1.

2. The acaricidal composition according to claim 1, characterized in that The mass ratio of the compound of formula (I) to Flupentiofenox is 1:20, 1:15, 1:7, 2:1, 7:1, 14:1, and 28:

1.

3. The acaricidal composition according to claim 1, characterized in that Based on the total weight of the acaricidal composition being 100 wt %, the sum of the contents of the active ingredient A and the active ingredient B in the acaricidal composition is 0.5 to 95 wt %.

4. The acaricidal composition according to claim 1, characterized in that The total content of the active ingredient A and the active ingredient B in the acaricidal composition is 1 to 80 wt %.

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

6. The acaricidal composition according to claim 5, characterized in that The acaricidal composition can be prepared into an agriculturally acceptable formulation, which is selected from a solid formulation and / or a liquid formulation.

7. The acaricidal composition according to claim 6, characterized in that The solid preparation is selected from wettable powders and water-dispersible granules; the liquid preparation is selected from soluble solutions, emulsifiable concentrates, aqueous emulsions, suspensions, suspoemulsions, microemulsions, and dispersible oil suspensions.

8. Use of the acaricidal composition according to any one of claims 1 to 7 for controlling harmful mites, characterized in that: The harmful mite is Tetranychus cinnabarinus.

9. The use according to claim 8, characterized in that The acaricidal composition is applied at an effective dose to the harmful mites to be controlled or the medium where they grow.

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