Acaricidal composition and application thereof

Abstract

The invention belongs to the field of pesticide acaricides, and relates to an acaricidal composition, the active components of the acaricidal composition comprise an active component A and an active component B, the active component A is a compound represented by a formula (I), the active component B is any one of two spirodiclofen, spiromesifen, spirodiclofen diester and bromopropylate, and the mass ratio of the active component A to the active component B is 1: 50-42: 1. The acaricidal composition has good acaricidal activity, has a remarkable synergistic effect under a certain mass ratio, and has the characteristics that the dosage of pesticides is reduced, the residues of the pesticides on crops are reduced, the environmental pollution is alleviated, the acaricidal composition is safe to human and livestock, the environmental compatibility is good, pest mites are not easy to generate drug resistance, and the like.

Description

Technical Field

[0001] The invention belongs to the technical field of pesticide acaricides, and in particular relates to application of a miticide composition to agricultural and forestry harmful mites and sanitary harmful mites. Background Art

[0002] The control of phytophagous mites still mainly relies on chemical control. Due to the rapid reproduction rate of phytophagous mites and the increase in the types and amounts of pesticides used in the field, phytophagous mites have developed varying degrees of resistance to a variety of pesticides, and cross-resistance has occurred, making the field control effectiveness of a variety of miticides increasingly poor, which has brought great difficulties to control.

[0003] By mixing two or more agents with different mechanisms of action, different pests can be controlled simultaneously, the efficacy of the agents can be improved, and the development of pest resistance can be reduced. The compound of formula (I) and any one of dispiracid, spiromesifen, spirobudiclib or bromofen have a significant synergistic effect on the control of herbivorous spider mites, and the compounded miticide composition of the compound of formula (I) and any one of dispiracid, spiromesifen, spirobudiclib or bromofen and its application have not been reported so far. Summary of the invention

[0004] Based on the above situation, the purpose of the present invention is to provide a miticide composition, which is mainly used for controlling pest mites in the crop industry, especially phytophagous pest mites. The miticide 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.

[0005] To achieve the above object, the technical solution adopted by the present invention is: an acaricidal composition, the active ingredients of the acaricidal composition include active ingredient A and active ingredient B, wherein active ingredient A is a compound of formula (I):

[0006] The active ingredient B is any one of dispiracil, spiromesifen, spiroclofen or bromocyclopentyl.

[0007] Furthermore, the mass ratio of the active ingredient A to the active ingredient B is 1:50 to 42:1;

[0008] Furthermore, the mass ratio of the active ingredient A to the active ingredient B is 1:45 to 40:1;

[0009] Furthermore, the mass ratio of the compound of formula (I) to Dispira is 1:20 to 40:1;

[0010] Furthermore, the mass ratio of the compound of formula (I) to Dispira is 1:20 to 22:1;

[0011] Furthermore, the mass ratio of the compound of formula (I) to Dispira is 1:20, 1:4, 4:1, 10:1, 22:1;

[0012] Furthermore, the mass ratio of the compound of formula (I) to spiromesifen is 1:45 to 36:1;

[0013] Furthermore, the mass ratio of the compound of formula (I) to spiromesifen is 1:32 to 36:1;

[0014] Furthermore, the mass ratio of the compound of formula (I) to spiromesifen is 1:32, 1:18, 4:7, 7:4, 6:1, 18:1, 36:1;

[0015] Furthermore, the mass ratio of the compound of formula (I) to spirobudiclib is 1:30 to 35:1;

[0016] Furthermore, the mass ratio of the compound of formula (I) to spirobudiclib is 1:30 to 24:1;

[0017] Furthermore, the mass ratio of the compound of formula (I) to spirobudiclib is 1:30, 1:25, 1:15, 4:9, 7:2, 15:1, 24:1;

[0018] Furthermore, the mass ratio of the compound of formula (I) to bromofen is 1:32 to 17:1;

[0019] Furthermore, the mass ratio of the compound of formula (I) to bromofen is 1:17 to 17:1;

[0020] Furthermore, the mass ratio of the compound of formula (I) to bromofen is 1:17, 1:8, 4:3, 4:1, 17:1;

[0021] Furthermore, 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 1 to 80 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 2 to 50 wt%;

[0023] Further, based on the total mass of the acaricidal composition as 100wt%, the sum of the contents of the active ingredient A and the active ingredient B in the acaricidal composition is 5wt%, 6.5wt%, 8wt%, 10wt%, 12wt%, 15wt%, 20wt%, 24wt%, 28wt%, 36wt%, 42wt%, 45wt%, 50wt%;

[0024] Furthermore, the acaricide composition includes agriculturally acceptable auxiliary ingredients in addition to the active ingredients, and the auxiliary ingredients are selected from one or more of wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreeze agents, defoamers, solvents, preservatives, stabilizers, synergists or carriers;

[0025] Further, the wetting agent is selected from one or more of alkylbenzene sulfonate, alkylnaphthalene sulfonate, lignin sulfonate, sodium dodecyl sulfate, sodium dioctyl succinate sulfonate, α-olefin sulfonate, alkylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, ethylene glycol polyoxyethylene polyoxypropylene ether, fatty alcohol ethoxylate, isomeric alcohol polyoxyethylene ether, fatty alcohol polyoxyethylene ether sodium sulfate, silkworm feces, saponin powder, soapberry powder, SOPA, detergent, emulsifier 2000 series and wetting penetrant F; and / or

[0026] Further, the dispersant is selected from one or more of lignin sulfonate, alkylnaphthalene sulfonate formaldehyde condensate, naphthalene sulfonate, tristyrylphenol ethoxylate phosphate, block polyether phosphate, arylphenol polyoxyethylene ether sulfate, 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 acid, phosphates, EO-PO block copolymers and EO-PO graft copolymers; and / or

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

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

[0029] Further, 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] Further, the antifreeze agent is selected from one or more of alcohols, alcohol ethers, chlorinated hydrocarbons and inorganic salts; and / or

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

[0032] Further, the solvent is selected from one or more of benzene, toluene, xylene, trimethylolbenzene, durene, methanol, ethanol, isopropanol, n-butanol, isooctyl alcohol, dimethyl sulfoxide, N,N-dimethylformamide, N,N-dimethylacetamide, N,N-dimethyldecylamide, N-methylpyrrolidone, cyclohexanone, propylene carbonate, alkylene carbonate, diesel, solvent oil, vegetable oil, vegetable oil derivatives and water; and / or

[0033] Further, 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, ethyl p-hydroxybenzoate, propyl p-hydroxybenzoate, butyl p-hydroxybenzoate, isothiazolinones, benzimidazoles, iodopropargyls, pyridinethiones, kasone and 1,2-benzisothiazolin-3-one; and / or

[0034] Further, 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] Further, the synergist is selected from synergistic phosphorus, synergistic ether, synergistic amine; and / or

[0036] Further, 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] Furthermore, the acaricide composition can be prepared into a formulation form permitted in agriculture, and the formulation form is selected from a solid formulation and / or a liquid formulation;

[0038] Furthermore, the solid preparation includes powders, granules, pellets, tablets, strips, wettable powders, oil-dispersible powders, emulsion powders, water-dispersible granules, emulsion granules, water-dispersible tablets, soluble powders, soluble tablets or soluble granules;

[0039] Further, the liquid preparation includes a soluble solution, a soluble gel, an oil, a film-spreading oil, an emulsifiable concentrate, a latex, a dispersible liquid, an ointment, an aqueous emulsion, an oil emulsion, a microemulsion, a fat, a suspension, a microcapsule suspension, an oil suspension, a dispersible oil suspension, a suspoemulsion, a microcapsule suspension-suspension, a microcapsule suspension-water emulsion or a microcapsule suspension-suspoemulsion;

[0040] Furthermore, 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;

[0041] Furthermore, the solid preparation is selected from wettable powders and water dispersible granules;

[0042] Furthermore, the liquid preparation is selected from emulsifiable concentrates, aqueous emulsions, suspensions, suspoemulsions, and microemulsions;

[0043] Furthermore, when the acaricide composition is a wettable powder, the mass proportions of the components are: 1 to 40 parts of active ingredient A, 1 to 40 parts of active ingredient B, 3 to 10 parts of dispersant, 1 to 5 parts of wetting agent, and the balance is made up of fillers;

[0044] The wettable powder preparation method comprises the following steps: pre-grinding and mixing the active ingredients and other auxiliary agents uniformly, and then grinding them by a jet mill until the fineness meets the requirement that at least 98 wt % passes through a 45 μm test sieve, thereby obtaining a wettable powder product.

[0045] Furthermore, when the acaricide composition is a water dispersible granule, the mass proportions of the components are: 1-40 parts of active ingredient A, 1-40 parts of active ingredient B, 3-20 parts of dispersant, 1-10 parts of wetting agent, 1-5 parts of disintegrant, and the balance is made up of filler;

[0046] The preparation method of the water dispersible granules is as follows: according to the formula ratio, the active ingredients are added into the carrier, and the surfactant and other functional additives are added thereto, mixed, air flow pulverized, 10-25% of water is added, and then the water dispersible granule product is obtained by kneading, granulating, drying and screening.

[0047] Furthermore, when the acaricide composition is an emulsifiable concentrate preparation, the weight percentages of the components are: 1-40 parts of active ingredient A, 1-40 parts of active ingredient B, 5-30 parts of emulsifier, 0-5 parts of synergist, and the balance is made up of solvent;

[0048] The emulsifiable concentrate preparation method comprises the following steps: adding the active ingredients into a solvent according to the formula ratio of the embodiment, adding a surfactant and other functional additives thereto, and stirring and mixing the mixture in a stirring mixing kettle to obtain an emulsifiable concentrate product.

[0049] Furthermore, when the acaricide composition is an aqueous emulsion, the mass fractions of the components are: 1-40 parts of active ingredient A, 1-40 parts of active ingredient B, 3-30 parts of emulsifier, 5-50 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 makes up the balance;

[0050] The preparation method of the aqueous emulsion is as follows: according to the formula ratio of the embodiment, the active ingredient is dissolved in the solvent and an emulsifier is added to dissolve it into a uniform oil phase; deionized water and antifreeze are mixed together to form a uniform water phase; the water phase is added to the oil phase, and after stirring evenly, a defoaming agent is added and subjected to high-speed shearing to form a well-dispersed aqueous emulsion product.

[0051] Furthermore, when the acaricide composition is a suspension, the mass fractions of the components are: 1-40 parts of active ingredient A, 1-40 parts of active ingredient B, 1-15 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, 0-10 parts of solvent, 0-5 parts of stabilizer, and deionized water makes up the balance;

[0052] The preparation method of the suspension concentrate comprises the following steps: placing active ingredients, surfactants and other functional additives in a reaction kettle in sequence according to the formula ratio, adding water to mix evenly, subjecting the mixture to high-speed shearing, wet sand grinding and finally homogenizing filtration to obtain the suspension concentrate product.

[0053] Furthermore, when the acaricide composition is a suspoemulsion, the mass fractions of the components are: 1-40 parts of active ingredient A, 1-40 parts of active ingredient B, 1-10 parts of emulsifier, 1-10 parts of dispersant, 1-5 parts of antifreeze, 0.1-2 parts of thickener, 0.1-0.8 parts of defoamer, 1-40 parts of solvent, 0-5 parts of stabilizer, and deionized water makes up the balance;

[0054] The preparation method of the suspoemulsion is as follows: according to the formula ratio, the active ingredient A is completely dissolved in a solvent, and an emulsifier is added to prepare an oil phase; the active ingredient B 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 mixing 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] Furthermore, when the acaricide composition is a microemulsion, the mass fractions of the components are: 1-40 parts of active ingredient A, 1-40 parts of active ingredient B, 8-30 parts of emulsifier, 5-15 parts of solvent, 2-15 parts of stabilizer, 1-5 parts of antifreeze, 0.1-8 parts of defoamer, and the balance is made up of deionized water;

[0056] The microemulsion preparation method comprises the following steps: dissolving the active ingredient in a solvent according to the formula ratio of the embodiment, adding an emulsifier to dissolve the active ingredient into a uniform oil phase, mixing deionized water and an antifreeze agent together to form a uniform water phase; adding the water phase into the oil phase, or the oil phase into the water phase, and stirring the mixture to form a microemulsion product.

[0057] The invention also discloses the use of the acaricidal composition as described above in preventing and controlling harmful mites.

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

[0059] Furthermore, the phytophagous pest mites are Panonychus citri McGregor, Eotetranychus kankitus (Ehara), Phyllocoptes oleivora, Tetranychus cinnabarinus (Boisduval), and Tetranychus urticae Koch.

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

[0061] The acaricidal composition of the present invention has the following advantages:

[0062] 1) The acaricidal composition of the present invention exhibits a synergistic effect within a certain ratio range and can effectively control a variety of vegetative pest mites;

[0063] 2) The two active ingredients in the acaricidal composition of the present invention have different action mechanisms, which effectively delay the development of drug resistance in harmful mites and extend the service life of the product;

[0064] 3) The acaricide composition of the present invention is environmentally friendly, safe and efficient, and its popularization and application has huge economic and social benefits. DETAILED DESCRIPTION

[0065] The present invention is further described below in conjunction with the examples, in which the percentages are all weight percentages, but the present invention is not limited thereto. The content of the active ingredient in the composition of the present invention depends on the dosage when used alone, and also depends on the mixing ratio and the degree of synergistic effect. The optimal range of the active ingredient content varies according to the formulation type of the composition.

[0066] Preparation Example:

[0067] Preparation Example 1

[0068] 1.1% formula (Ⅰ) compound·Eubacterium spp. emulsion (1:0.1)

[0069] Formula composition: 1% compound of formula (I), 0.1% dispiracil, 12.5% ​​cyclohexanone, 5% EO / PO block polyether, 0.5% phenylphenol polyoxyethylene ether phosphate, 0.5% fatty alcohol polyoxyethylene ether phosphate, 5% propylene glycol, 0.1% organosilicon defoamer, and deionized water to make up the balance;

[0070] Preparation method: After the active ingredients are completely dissolved in the solvent according to the formula ratio, an emulsifier is added to prepare an oil phase; a dispersant, an antifreeze agent, deionized water, etc. are stirred evenly to prepare an aqueous phase; the oil phase is added to the aqueous phase and stirred evenly, and high-speed shearing is performed until the particle size meets the requirements, and a defoaming agent is added and stirred evenly to obtain an aqueous emulsion product.

[0071] Preparation Example 2

[0072] 1.2% formula (Ⅰ) compound·spirobudic acid diester water emulsion (0.9:0.3)

[0073] Formula composition: 0.9% compound of formula (I), 0.3% spirobudic acid diester, 13% cyclohexanone, 4.5% castor oil polyoxyethylene ether, 1% fatty alcohol polyoxyethylene ether phosphate, 5% propylene glycol, 0.1% organosilicon defoamer, and deionized water to make up the balance;

[0074] Preparation method: Same as Preparation Example 1.

[0075] Preparation Example 3

[0076] 1% compound of formula (I)·bromofen emulsion in water (0.8:0.2)

[0077] Formula composition: 0.8% compound of formula (I), 0.2% bromofen, 15% cyclohexanone, 4.5% castor oil polyoxyethylene ether, 1% fatty alcohol polyoxyethylene ether phosphate, 5% propylene glycol, 0.1% silicone oil, and deionized water to make up the balance;

[0078] Preparation method: Same as Preparation Example 1.

[0079] Preparation Example 4

[0080] 25% formula (Ⅰ) compound·Eubacterium suspension (20:5)

[0081] Formula composition: 20% compound of formula (I), 5% dispiracil, 2% alkylnaphthalene sulfonate formaldehyde condensate, 2.5% tristyrylphenol ethoxylate phosphate, 0.5% organosilicon defoamer, 0.25% xanthan gum, 1% magnesium aluminum silicate, 5% ethylene glycol, 0.5% sodium benzoate, and deionized water to make up the balance;

[0082] Preparation method: Add wetting dispersant and defoamer to the measured deionized water and stir evenly, then add active ingredients and stir evenly, use zirconium oxide beads and sand mill to wet grind 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 evenly at a high speed to obtain a suspension.

[0083] Preparation Example 5

[0084] 25% formula (Ⅰ) compound·spiromesifen suspension (16:9)

[0085] Formula composition: 16% compound of formula (I), 9% spiromesifen, 1.5% sodium alkylnaphthalene sulfonate, 2% EO-PO block copolymer, 2.5% tristyrylphenol ethoxylate phosphate, 3% EO-PO block copolymer, 0.5% silicone defoamer, 0.25% xanthan gum, 1% magnesium aluminum silicate, 5% glycerol, 0.5% sodium benzoate, and deionized water to make up the balance;

[0086] Preparation method: Same as Preparation Example 4.

[0087] Preparation Example 6

[0088] 27% formula (Ⅰ) compound·spirobudiclib suspension (21:6)

[0089] Formula composition: 21% compound of formula (I), 6% spirobudic acid diester, 2% alkylnaphthalene sulfonate formaldehyde condensate, 1.5% lignin sulfonate, 2.5% tristyrylphenol ethoxylate phosphate, 0.5% silicone oil, 0.2% xanthan gum, 1% magnesium aluminum silicate, 5% glycerol, 0.5% sodium benzoate, and deionized water to make up the balance;

[0090] Preparation method: Same as Preparation Example 4.

[0091] Preparation Example 7

[0092] 42% Formula (Ⅰ) compound·Dispirillum wettable powder (38:4)

[0093] Formula composition: 38% compound of formula (I), 4% dispiracil, 5% naphthalene sulfonate, 4.5% sodium lignin sulfonate, 7.2% alkylphenol polyoxyethylene ether methyl ether condensate sulfate, 2.5% sodium dodecyl sulfate, 2% white carbon black, 8% bentonite, and kaolin makes up the balance;

[0094] Preparation method: pre-crush and mix evenly, then grind by air flow mill to a fineness that satisfies the requirement that at least 98wt% passes through a 45μm test sieve to obtain a wettable powder.

[0095] Preparation Example 8

[0096] 40% formula (Ⅰ) compound·spiromesifen water dispersible granules (32:8)

[0097] Formula composition: 32% compound of formula (I), 8% spiromesifen, 8% lignin sulfonate, 2% α-olefin sulfonate, 10% alkylnaphthalene sulfonate formaldehyde condensate, 2% sodium dodecyl sulfate, 1% ammonium chloride, 1.5% sodium carbonate, 18% attapulgite, and bentonite makes up the balance;

[0098] Preparation method: first mix evenly, then crush 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, and prepare water dispersible granules.

[0099] Preparation Example 9

[0100] 28% formula (Ⅰ) compound·bromofen water dispersible granules (22:6)

[0101] Formula composition: 22% compound of formula (I), 6% bromofen, 10% lignin sulfonate, 1.5% α-olefin sulfonate, 8% alkylnaphthalene sulfonate formaldehyde condensate, 2.5% sodium dodecyl sulfate, 1% ammonium chloride, 1.5% sodium carbonate, 15% attapulgite, and bentonite makes up the balance;

[0102] Preparation method: Same as Preparation Example 8.

[0103] Preparation Example 10

[0104] 2.5% formula (Ⅰ) compound·bromofen emulsifiable concentrate (2:0.5)

[0105] Formula composition: 2% compound of formula (I), 0.5% bromofen, 12% propylene carbonate, 3% calcium dodecylbenzenesulfonate, 8% castor oil polyoxyethylene ether, 15% N,N-dimethylformamide, 2% corn oil, 18% cyclohexanone, and methyl oleate makes up the balance;

[0106] Preparation method: first add the active ingredient into the solvent and completely dissolve it, then add the emulsifier and stir evenly to form a uniform and transparent oily liquid, fill it, and prepare the emulsifiable concentrate preparation.

[0107] Indoor biological activity assay

[0108] Indoor activity test 1

[0109] Test insect source: Panonychus citri;

[0110] Test agents: technical of the compound of formula (I), dispiracloprid technical, spiromesifen technical, spiroclofen technical, bromofen technical, all of which are provided by the Group's R&D Center;

[0111] Test material preparation: Select 2-year-old nymphs or female adult mites that are reared indoors and have the same physiological state. Cut the double-sided tape into 2 cm long pieces and stick them on one end of the slide. Then select healthy mites and stick their backs on the double-sided tape. Put 20 mites per slide into a container padded with a wet sponge, cover it, and place it at (25±1)℃. After 2 hours, examine under a microscope, remove dead and injured individuals, and make up 15 mites per slide, with 2 slides per treatment.

[0112] Preparation of drugs: The original drug was prepared into a mother solution with solvent, and the mother solution was prepared into test drugs in different proportions with 0.1% Tween 80 aqueous solution.

[0113] Chemical treatment: Immerse the glass slide in the chemical solution and shake it gently for 5 seconds, then take it out and absorb the excess chemical solution with absorbent paper. Place it on a white porcelain plate lined with a wet sponge, cover it with a light-transmitting plastic film, and place it at (25±1)℃ for observation.

[0114] Experimental repetition: Each treatment was repeated 4 times, and a treatment without drug was set as a blank control.

[0115] Test investigation: 48 hours after treatment, check the death of test insects, record the total number of mites and the number of dead mites, and calculate the mortality rate:

[0116]

[0117] Where:

[0118] P——mortality rate, in percentage (%);

[0119] K——indicates the number of dead mites, the unit is head;

[0120] N——represents the total number of mites treated, in heads.

[0121] Where:

[0122] P1——adjusted mortality rate, in percentage (%);

[0123] P t ——Treatment mortality rate, expressed as percentage (%);

[0124] P0——blank control mortality rate, in percentage (%).

[0125] 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.

[0126] The LC of each drug was calculated by linear regression analysis between the probability value of mortality and the logarithmic value of the series concentration (DPS data processing system). 50 value.

[0127] 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:

[0128]

[0129] Where:

[0130] ATI——Actual Toxicity Index of Mixture;

[0131] S——LC of standard acaricide 50 , the unit is milligrams per liter (mg / L);

[0132] M——LC of the mixture 50 , the unit is milligrams per liter (mg / L).

[0133] TTI=TI A *P A +TI B *P B

[0134] Where:

[0135] TTI – Theoretical Toxicity Index of Mixtures;

[0136] TI A ——A: toxicity index of the agent;

[0137] P A ——The percentage of agent A in the mixture, in percentage (%);

[0138] TI B ——Toxicity index of agent B;

[0139] P B ——The percentage of agent B in the mixture, in percentage (%).

[0140]

[0141] Where:

[0142] CTC – Co-toxicity coefficient;

[0143] ATI——Actual Toxicity Index of Mixture;

[0144] TTI - Theoretical Toxicity Index of Mixture.

[0145] According to the classification standard of combined 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 < CTC < 120 indicates an additive effect.

[0146] Test results:

[0147] The results in Table 1 show that the compound of formula (I) has an activity against Panonychus citri (female adult mite) LC 50 The value is 20.559 mg / L, and the LC value of Diplococcus spp. to Panonychus citri (female adult mite) 50 The value is 1.038mg / L.

[0148] The mass ratio of the compound of formula (I) to the two-spiral worm in the range of 1:50 to 40:1 shows an additive or synergistic effect on the control of citrus Panonychus mite (female adult mites). The mass ratio of the compound of formula (I) to the two-spiral worm in the range of 1:20 to 40:1 shows a synergistic effect on the control of citrus Panonychus mite (female adult mites). When the mass ratio of the compound of formula (I) to the two-spiral worm is 10:1, its LC 50 The value is 2.520 mg / L, and the co-toxicity coefficient is 301.082. The co-toxicity coefficient is relatively high, and the synergistic effect is significant.

[0149] Table 1 Indoor activity test results of compound of formula (I) and Diplocoriella against Panonychus citri (female adult mite)

[0150]

[0151] The results in Table 2 show that the LC of spiromesifen against Panonychus citri (female adult mites) 50 The value is 8.834 mg / L. The mass ratio of the compound of formula (I) to spiromesifen is in the range of 1:45 to 36:1, and the control effect on citrus panonychus mites (female adult mites) is synergistic. When the mass ratio of the compound of formula (I) to spiromesifen is 7:4, its LC 50 The value is 4.029 mg / L, and the co-toxicity coefficient is 344.167. The co-toxicity coefficient is relatively high, and the synergistic effect is significant.

[0152] Table 2 Indoor activity test results of the compound of formula (I) and spiromesifen against Panonychus citri (female adult mites)

[0153]

[0154] The results in Table 3 show that the LC of spiroclocarp against Panonychus citri (female adult mites) 50 The value is 5.160 mg / L. The mass ratio of the compound of formula (I) to spirobudiclib is in the range of 1:30 to 35:1, and the control effect on Panonychus citri (female adult mites) is synergistic. When the mass ratio of the compound of formula (I) to spirobudiclib is 7:2, its LC 50 The value is 4.300 mg / L, and the co-toxicity coefficient is 287.471. The co-toxicity coefficient is relatively high, and the synergistic effect is significant.

[0155] Table 3 Indoor activity test results of the compound of formula (I) combined with spiroclofenac against Panonychus citri (female adult mites)

[0156]

[0157] The results in Table 4 show that the compound of formula (I) has an activity against Panonychus citri (nymph) LC 50 The value is 23.298mg / L, and the LC value of bromofen against Panonychus citri (nymph) 50The value is 31.683 mg / L.

[0158] The mass ratio of the compound of formula (I) to bromofen is in the range of 1:32 to 42:1, and the control effect on citrus panonychus mites (nymphs) is additive or synergistic. The mass ratio of the compound of formula (I) to bromofen is in the range of 1:32 to 17:1, and the control effect on citrus panonychus mites (nymphs) is synergistic. When the mass ratio of the compound of formula (I) to bromofen is 4:1, its LC 50 The value is 11.561 mg / L, and the co-toxicity coefficient is 212.785. The co-toxicity coefficient is relatively high, and the synergistic effect is significant.

[0159] Table 4 Indoor activity test results of compound of formula (I) combined with bromofen against Panonychus citri (nymph)

[0160]

[0161] Field efficacy examples

[0162] Field test on the efficacy of pesticides against citrus red spider mites

[0163] Test crops: Citrus (Wogan);

[0164] Test subjects: Citrus spider mite;

[0165] Experimental design: a total of 10 treatments, 3 replications, 30 plots, 2 trees per plot, randomized block arrangement, with one row of fruit trees between each plot.

[0166] Table 5 Test agents and dosage

[0167]

[0168] Test location: Citrus orchard in Shuangqiao Town, Wuming District, Nanning City, Guangxi Zhuang Autonomous Region. The growth of citrus trees in the test area is basically the same, and citrus red spider mites have occurred more severely in recent years. The soil fertility of the test site is high, the cultivation and management conditions are good, and it is planted all year round.

[0169] In September 2022, it was sunny on the day of spraying, with a maximum temperature of 32°C, a minimum temperature of 21°C, and a north wind of level 1. It was cloudy during the test.

[0170] Application method, time and frequency: Use a motorized sprayer (WL-ABSC model) and manually spray the whole tree evenly. According to the actual field conditions and farmers' water consumption habits, the water consumption per citrus tree is determined to be 1.8L, and the amount of application is determined to be evenly applied to the leaves with a little dripping. Apply once.

[0171] Survey method: Randomly select one point from the east, west, south, north and center of each citrus tree, mark a branch at each point, and record the number of all living citrus red spider mites on the leaves on the marked branches (starting from the top leaf, with no less than 5 leaves). Mainly investigate adult mites and female adult mites (can be observed with a magnifying glass).

[0172] Investigation time and frequency: once before medication and once at 3d and 10d after medication.

[0173] The efficacy is calculated as follows:

[0174]

[0175] Safety survey:

[0176] A safety survey was conducted each time the control effect was investigated after the application of the pesticides to investigate whether each test agent caused any damage to citrus. If so, the extent of the damage was recorded.

[0177] Field test results:

[0178] Observation of the growth of citrus trees showed that during the entire test, each pesticide treatment was safe and had no harm to the citrus trees.

[0179] As can be seen from Table 6, the compound of formula (I) mixed with dispiracil, spiromesifen, spiroclofen or bromofen has a good control effect on citrus red spider mites, showing good quick-acting property.

[0180] 3 days after treatment, the protective effects of 25% compound of formula (I)·dispirilla suspension (20:5), 25% compound of formula (I)·spiromesifen suspension (16:9), 27% compound of formula (I)·spiromesifen suspension (21:6), and 28% compound of formula (I)·bromofen water dispersible granules (22:6) against citrus red spider mites were 82.36%, 81.13%, 81.21%, and 80.57%, respectively. At the 0.05 level, through difference analysis, the mixed preparations of compound of formula (I) and dispirilla, spiromesifen, spiromesifen or bromofen were significantly higher than the control single agent.

[0181] Table 6 Control effect of each treatment on citrus red spider mites 3 days after application

[0182]

[0183] Note: The protective effect (%) in the table is the average value of each replicate, and the difference is at the 5% level. The same applies to the following tables.

[0184] As can be seen from Table 7, 10 days after application, the protective effects of 25% compound of formula (I)·dispirilla suspension (20:5), 25% compound of formula (I)·spiromesifen suspension (16:9), 27% compound of formula (I)·spiromesifen suspension (21:6), and 28% compound of formula (I)·bromofen water dispersible granules (22:6) against citrus red spider mites were 92.70%, 91.12%, 91.07%, and 87.38%, respectively. At the 0.05 level, through difference analysis, the mixed preparations of compound of formula (I) and dispirilla, spiromesifen, spiromesifen or bromofen were significantly higher than the control single agent.

[0185] The compound of formula (I) mixed with dispiracil, spiromesifen, spiroclofen or bromofen has a good persistent effect on citrus red spider mites.

[0186] Table 7 Control effect of each treatment on citrus red spider mites 10 days after application

[0187]

[0188] Through indoor toxicity determination and tests on citrus in the field, the acaricidal composition prepared by compounding the compound of formula (I) of the present invention with any one of dispiracid, spiromesifen, spirocyclopentyl or bromocyclopentyl showed good control effect on phytophagous mites, especially citrus red spider mites.

[0189] The compounded acaricidal composition or the preparation thereof of the present invention has significant control effect, and is superior to a single agent in delaying the generation of drug resistance and prolonging the lasting effect. In addition, no compound agent was found to cause phytotoxicity to crops in the test, indicating that the acaricidal composition or preparation obtained can reduce production costs and use costs and is safe for crops when the acaricidal synergistic synergy is improved.

[0190] Although the present invention has been described in detail above with general instructions and specific implementation schemes, it is obvious to those skilled in the art that some modifications or improvements can be made on the basis of the present invention. Therefore, these modifications or improvements made without departing from the spirit of the present invention are within the scope of protection claimed by the present invention.

Claims

1. A mite-killing composition, characterized in that: The active ingredients of the acaricide composition include active ingredient A and active ingredient B, wherein active ingredient A is a compound of formula (I): The active ingredient B is any one of dispiracil, spiromesifen, spiroclofen or bromocyclopentyl.

2. The acaricidal composition according to claim 1, characterized in that The mass ratio of the active ingredient A to the active ingredient B is 1:50 to 42:1; Preferably, the mass ratio of the active ingredient A to the active ingredient B is 1:45 to 40:

1.

3. The acaricidal composition according to claim 1, characterized in that: The mass ratio of the compound of formula (I) to Dispira is 1:20 to 40:1; The mass ratio of the compound of formula (I) to spiromesifen is 1:45 to 36:1; The mass ratio of the compound of formula (I) to spirobudiclib is 1:30 to 35:1; The mass ratio of the compound of formula (I) to bromofen is 1:32 to 17:

1.

4. 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 1 to 80 wt %.

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

6. The acaricidal composition according to claim 5, characterized in that: The acaricidal composition is prepared into a formulation form permitted in agriculture, and the formulation form 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.

9. The use according to claim 8, characterized in that: The harmful mites are herbivorous harmful mites; Preferably, the phytophagous pest mites are Panonychus citri, Tetranychus citri, Tetranychus cinnabarinus, and Tetranychus urticae.

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

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