Acaricide containing organic tin compound and application thereof

By combining the compound of formula I with triazole tin or benzyl tin, the acaricide formed significantly enhances the prevention and control effect of the spider mite family and the glanid family, solves the problems of poor control effects and rapid resistance development in the existing technology, and achieves more efficient and environmentally friendly prevention and control of the spider mite family.

CN119856721AActive Publication Date: 2025-04-22HAILIR PESTICIDES & CHEM GRP
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Patent Information

Application Number
CN202311357029.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2023-10-19
Publication Date
2025-04-22
Estimated Expiration
2043-10-19

AI Technical Summary

Technical Problem

The existing organic tin acaricides have limited effect on the prevention and control of harmful mites, especially the prevention and control of harmful mites in the Spider Mite family and the Gall Mite family, and the resistance develops rapidly.

Method used

By reasonably combining the compound of formula I with triazole tin or benzyl tin, acaricides of different mass ratios are formed, which are used for agricultural prevention and control of harmful mites.

Benefits of technology

It significantly enhances the prevention and control effect of spider mites and gall mites, effectively controls the harm of spider mites to crops, delays the development of resistance of spider mites, and reduces the use of pesticides.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention belongs to the technical field of pesticide mite killing, and discloses an acaricide containing organic tin compounds and application thereof.The acaricide comprises an active ingredient A and an active ingredient B. The active ingredient A is a compound shown in the formula I: # imgabs0, the active ingredient B is the organic tin compounds, the organic tin compounds are azocyclotin or fenbutatin oxide, and the active ingredient A is a compound shown in the formula II. The mass ratio of the active component A to the active component B is (1: 50)-(45: 1). According to the acaricide disclosed by the invention, different active components are reasonably compounded, so that the acaricide has an obvious synergistic effect on agricultural common pest mites, and particularly has an obvious control effect on tetranychidae pest mites and acaridae pest mites.
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Description

Technical Field

[0001] The invention belongs to the technical field of pesticide acaricide and discloses an acaricide containing an organic tin compound and application thereof. Background Art

[0002] Azotin, CAS registration number 41083-11-8, chemical name tricyclohexyl (1,2,4-triazol-1-yl) stannane, is widely used to control mites on fruit trees, flowers and vegetables. Its structural formula is as follows:

[0003]

[0004] Phenylbutatin, CAS registration number 13356-08-6, chemical name bis[tri(2-methyl-2-phenylpropyl)tin] oxide, can be used in fruit trees, tea trees, flowers and other crops to prevent and control various plant mites in their active stages. Its structural formula is as follows:

[0005]

[0006] The compound of formula I, chemical name: (4'-chloro-6-fluoro-4-methyl-[1,1'-biphenyl]-3-yl)(2,2,2-trifluoroethyl) sulfide, has the following chemical structure:

[0007]

[0008] Azolin and fenbutatin belong to the same class of organotin acaricides, and are both inhibitors of oxidative phosphorylation. Both of them mainly act on contact, and are weak in killing eggs. However, the compound of formula I has a completely different chemical structure and mechanism of action from the organotin acaricides. Studies have found that compounding the compound of formula I with azolin or fenbutatin exhibits a significant synergistic effect on harmful mites within a certain mass ratio range. Summary of the invention

[0009] Based on the above situation, the purpose of the present invention is to provide an acaricide containing an organotin compound and its application. The acaricide has an obvious synergistic effect on the control of common agricultural pest mites by rationally compounding different active ingredients, especially the control effect on the pest mites of the Tetranychus family and the Gall Mite family. The use of the acaricide of the present invention in the field can effectively control the harm of the pest mites to crops and control the spread of the pest mites; and the acaricide reduces the dosage of pesticides and has a significant effect on delaying the resistance of the pest mites.

[0010] In order to achieve the above object, the present invention adopts the following technical scheme: an acaricide containing an organotin compound, wherein the acaricide comprises an active ingredient A and an active ingredient B, wherein the active ingredient A is a compound of formula I: The active ingredient B is an organic tin compound, the organic tin compound is triazotin or fenbutatin, and the mass ratio of the active ingredient A to the active ingredient B is 1:50 to 45:1;

[0011] Furthermore, the mass ratio of the active ingredient A to the active ingredient B is 1:48 to 42:1;

[0012] Furthermore, the active ingredient B is triazotin, and the mass ratio of the active ingredient A to the active ingredient B is 1:32 to 30:1;

[0013] Furthermore, the active ingredient B is triazotin, and the mass ratio of the active ingredient A to the active ingredient B is 1:26 to 32:1.

[0014] Furthermore, the active ingredient B is fenbutatin, and the mass ratio of the active ingredient A to the active ingredient B is 1:40 to 30:1;

[0015] Furthermore, the active ingredient B is fenbutatin, and the mass ratio of the active ingredient A to the active ingredient B is 1:30 to 30:1;

[0016] Furthermore, the total weight of the acaricide is 100 wt%, and the total weight of the active ingredient A and the active ingredient B accounts for 2% to 70% of the total weight of the acaricide;

[0017] Furthermore, the acaricide comprises auxiliary ingredients in addition to the active ingredients, and the auxiliary ingredients are 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 or a carrier;

[0018] 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, alkylphenol ethoxylate, fatty alcohol ethoxylate, fatty alcohol polyoxyethylene ether sodium sulfate, silkworm feces, saponin powder, soapberry powder, SOPA, detergent, emulsifier 2000 series and wetting penetrant F; and / or

[0019] 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 acid, phosphates, EO-PO block copolymers and EO-PO graft copolymers; and / or

[0020] The thickener is selected from one or more of xanthan gum, polyvinyl alcohol, organic bentonite, magnesium aluminum silicate, and carboxymethyl cellulose; and / or

[0021] 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

[0022] The emulsifier is selected from one or more of fatty alcohol polyoxyethylene ether, fatty alcohol ethylene oxide-propylene oxide copolymer, phenylethylphenol polyoxyethylene polyoxypropylene ether, alkylphenol polyoxyethylene ether, fatty amine polyoxyethylene ether, alkylbenzene sulfonate, styrylphenol polyoxyethylene ether, fatty acid polyoxyethylene ester; and / or

[0023] The defoaming agent is selected from silicone oil, C 10 ~C 20 Saturated fatty acid compounds, C8~C 10 One or more of fatty alcohol compounds or silicone compounds; and / or

[0024] The preservative is selected from one or more of sorbic acid, sodium sorbate, potassium sorbate, benzoic acid, sodium benzoate, sodium p-hydroxybenzoate, and methyl p-hydroxybenzoate; and / or

[0025] 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, epoxidized vegetable oil, and / or

[0026] The synergist is selected from synergist phosphite and synergist ether; and / or

[0027] The carrier is selected from one or more of kaolin, bentonite, attapulgite, light calcium carbonate, diatomaceous earth, and white carbon black; and / or

[0028] The solvent is selected from one or more of benzene, toluene, xylene, methanol, ethanol, isopropanol, n-butanol, diesel, N,N-dimethylformamide, cyclohexanone, ethyl acetate, N-methylpyrrolidone, propanol, butanol, ethylene glycol, diethylene glycol, ethylene glycol methyl ether, butyl ether, solvent oil, vegetable oil, vegetable oil derivatives and deionized water; and / or

[0029] The above auxiliary ingredients are all commercially available.

[0030] Furthermore, the acaricide can be prepared into a formulation form permitted by pesticides, and the formulation form is a solid formulation and / or a liquid formulation;

[0031] Furthermore, the solid preparation is a water-dispersible granule, a wettable powder, a granule, a soluble powder or an emulsion; the liquid preparation is a soluble solution, a soluble gel, an emulsifiable concentrate, an aqueous emulsion, an oil emulsion, a microemulsion, a suspension, a microcapsule suspension, an oil suspension, a dispersible oil suspension or a suspoemulsion.

[0032] The invention also discloses the use of the acaricide for preventing and controlling harmful mites.

[0033] Furthermore, the harmful mites are pest mites of the Tetranychidae family and / or the Gall Mite family, the pest mites of the Tetranychidae family are Tetranychus cinnabarinus, Tetranychus urticae or Panonychus citri, and the harmful mites of the Gall Mite family are Citrus rust mite or Lycium barbarum gall mite.

[0034] Furthermore, the harmful mite is Tetranychus cinnabarinus, Panonychus citri or Lycium barbarum gall mite.

[0035] The beneficial effects of the present invention are as follows:

[0036] 1) The acaricide of the present invention rationally compounds active ingredients with different action mechanisms, has a significant synergistic effect on common Tetranychus and Gall Mites, and effectively controls the damage and spread of the pests;

[0037] 2) The acaricide of the present invention reduces the amount of pesticides used, thereby reducing agricultural production costs and is environmentally safe;

[0038] 3) The acaricide of the present invention effectively delays the development of drug resistance of harmful mites, does not cause drug damage to crops, and is safe to non-target organisms. DETAILED DESCRIPTION

[0039] In order to make the purpose, technical scheme and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the embodiments. It should be understood that the specific embodiments and preparation examples described herein are only used to explain the present invention and are not used to limit the present invention.

[0040] Related preparation examples:

[0041] Preparation Example 1: 24% Formula I compound·Triazolidine water dispersible granules (1:1)

[0042] Formula composition: 12% compound of formula I, 12% triazotin, 3% sodium dodecyl sulfate, 10% naphthalenesulfonate formaldehyde condensate, 5% sodium salt of polycarboxylate, 5% white sugar, and kaolin makes up the balance.

[0043] Preparation method: according to the formula ratio of the preparation example, the active ingredient is added to the carrier, and the surfactant and other functional additives are added thereto, mixed, and after air flow grinding, 10-25% of water is added, and then kneading, granulation, drying and sieving are carried out to obtain a water-dispersible granule product; or the ground powder is sprayed with water in a boiling granulator, granulated, dried, and then sieved to obtain the product.

[0044] Preparation Example 2: 25% Formula I compound·Triazolidine emulsifiable concentrate (3:2)

[0045] Formula composition: 15% of the compound of formula I, 10% of triazotin, 18% of EO / PO block copolymer, 12% of acetophenone, 10% of N-octylpyrrolidone, 1% of calcium dodecylbenzenesulfonate, 15% of dichloromethane, and xylene makes up the balance.

[0046] Preparation method: according to the formula ratio of the preparation example, the measured active ingredients, solvents and co-solvents are added into a mixing kettle and stirred to dissolve, then an emulsifier is added, and the balance is supplemented with the remaining solvent, and the mixture is stirred evenly in a stirring kettle, and the desired emulsifiable concentrate of the present invention is obtained after filtering.

[0047] Preparation Example 3: 16% Formula I compound·Triazolopyrimidine dispersible oil suspension (7:1)

[0048] Formula composition: 14% compound of formula I, 2% triazotin, 2% lignin sulfonate, 12% phenethylphenol polyoxyethylene polyoxypropylene ether, 3% Guerbet alcohol polyoxyethylene ether, 2% calcium dodecylbenzene sulfonate, 0.5% silicon dioxide, 0.5% organic bentonite, 15% 200# solvent oil, and methyl oleate makes up the balance;

[0049] Preparation method: According to the formula ratio, the active ingredients, surfactants and other functional additives are placed in a reactor in sequence, oil is added and mixed evenly, and the dispersible oil suspension product is obtained by high-speed shearing, wet sand grinding, and finally homogenization filtration.

[0050] Preparation Example 4: 18% Formula I compound·Triazolidine suspension (1:5)

[0051] Formula composition: 3% compound of formula I, 15% triazotin, 1% sodium lignin sulfonate, 1% naphthalene sulfonate formaldehyde condensate, 3% fatty alcohol polyoxyethylene ether, 3% alkyl phosphate ester salt, 0.3% xanthan gum, 1% magnesium aluminum silicate, 4% propylene glycol, 0.01% potassium benzisothiazolinone, 0.5% silicone oil, and deionized water to make up the balance;

[0052] Preparation method: According to the formula ratio of the preparation example, the active ingredient, surfactant and other functional additives are placed in a reaction kettle in sequence, water is added to mix evenly, and the suspension product is obtained by high-speed shearing, wet sand grinding, and finally homogenization filtration.

[0053] Preparation Example 5: 21% Formula I compound·Triazolidine sulfoxide emulsion (5:2)

[0054] Formula composition: 15% compound of formula I, 6% triazotin, 1% calcium dodecylbenzene sulfonate, 1% alkylphenol polyoxyethylene ether, 1% sodium salt of polycarboxylic acid, 4% alkylphenol polyoxyethylene ether phosphate, 2% styrylphenol polyoxyethylene polyoxypropylene ether, 0.1% hydroxyethyl cellulose, 1% magnesium aluminum silicate, 0.1% kason, 0.5% silicone defoamer, 5% ethylene glycol, 8% dichloromethane, 6% cyclohexanone, and deionized water to make up the balance;

[0055] Preparation method: According to the formula ratio of the embodiment, the active ingredient B is completely dissolved with a solvent to prepare an oil phase; the compound of formula I and a wetting dispersant, an antifreeze agent, a defoaming agent, deionized water, etc. are wet-grinded to a D90 of less than 5 μm to prepare a suspension mother liquid; the oil phase is added to the suspension mother liquid and stirred evenly, and then a thickener is added and stirred and sheared evenly to prepare a suspoemulsion preparation of the composition of the present invention.

[0056] Preparation Example 6: 40% Formula I compound·fenbutatin water dispersible granules (1:7)

[0057] Formula composition: 5% compound of formula I, 35% fenbutatin, 5% sodium polycarboxylate, 10% sodium lignin sulfonate, 3% sodium lauryl sulfate, 10% ammonium sulfate, and starch makes up the balance;

[0058] Preparation method: Same as Preparation Example 1.

[0059] Preparation Example 7: 20% Formula I compound·fenbutatin emulsifiable concentrate (3:1)

[0060] Formula composition: 15% compound of formula I, 5% fenbutatin, 12% DMF, 5% octylphenol polyoxyethylene ether phosphate, 0.5% glacial acetic acid, 10% tristyrylphenol polyoxyethylene ether, 2% calcium dodecylbenzene sulfonate, 15% propylene carbonate, and xylene makes up the balance;

[0061] Preparation method: Same as Preparation Example 2.

[0062] Preparation Example 8: 18% Formula I compound·fenbutatin dispersible oil suspension (1:8)

[0063] Formula composition: 2% compound of formula I, 16% fenbutatin, 4% alkylphenol polyoxyethylene ether, 8% glycerol fatty acid ester polyoxyethylene ether, 2% calcium dodecylbenzene sulfonate, 1% sodium salt of polycarboxylic acid, 1% sodium alkyl polyoxyethylene ether sulfonate, 0.5% organic bentonite, and soybean oil makes up the balance;

[0064] Preparation method: Same as Preparation Example 3.

[0065] Preparation Example 9: 20% Formula I compound·fenbutatin suspension (1:3)

[0066] Formula composition: 5% compound of formula I, 15% fenbutatin, 2% castor oil polyoxyethylene ether, 1% alkyl aryl polyoxyethylene ether polyoxypropylene ether, 2% castor oil polyoxyethylene ether phosphate, 2% polycarboxylic acid sodium salt, 1.5% magnesium aluminum silicate, 0.1% carboxyethyl cellulose, 1% sodium benzoate, 5% ethylene glycol, 0.5% silicone oil, and deionized water to make up the balance;

[0067] Preparation method: Same as Preparation Example 4.

[0068] Preparation Example 10: 24% Formula I compound·fenbutatin suspoemulsion (5:1)

[0069] Formula composition: 20% compound of formula I, 4% phenylbutanol, 5% dichloromethane, 5% cyclohexanone, 0.2% glacial acetic acid, 2% castor oil polyoxyethylene ether, 3% fatty alcohol polyoxyethylene ether phosphate, 1% polycarboxylic acid sodium salt, 2% styrylphenol polyoxyethylene polyoxypropylene ether, 1% fatty alcohol polyoxyethylene ether sulfate, 4% glycerol, 0.1% hydroxyethyl cellulose, 1% magnesium aluminum silicate, 0.5% sodium diacetate, 0.5% organosilicon defoamer, and deionized water to make up the balance;

[0070] Preparation method: Same as Preparation Example 5.

[0071] The preparation examples prepared above have been tested and found to meet the quality and technical indicators required for the corresponding preparations, and the preparations prepared are qualified preparations recognized in the art.

[0072] Example 1: Indoor biological activity test of compound acaricide against Tetranychus mites

[0073] Test basis: The test refers to NY / T 1154.12-2008 "Guidelines for Indoor Biological Activity Determination of Pesticides Insecticides Part 12: Spider Mite Slide Dipping Method".

[0074] Test targets: female adult mites of Panonychus citri and female adult mites of Tetranychus cinnabarinus.

[0075] Test method: Select female adult mites with the same physiological state. Cut a 2 cm long double-sided tape and stick it to one end of the slide. Pick healthy female adult mites and stick them on the double-sided tape. 30 mites per slide. After treatment, put the harmful mites into a container with a wet sponge, cover it, and place it at (25±1)℃. After 2 hours, conduct microscopic examination, remove dead, injured and inactive individuals, and make up 30 mites per slide.

[0076] Preparation of the drug: Dissolve the technical drug of the compound of formula I, the technical drug of fenbutatin and the technical drug of triazotin with a solvent to prepare a mother liquor, and then use a 0.1% Tween-80 aqueous solution to prepare 5 series of mass concentration gradients according to the equal ratio method.

[0077] Test method: Immerse the glass slide in the above reagents and shake gently for 5 seconds, then take it out, absorb the excess liquid with absorbent paper, place it in a white porcelain plate padded with a wet sponge, and cover it with a plastic film with good light transmittance. Repeat each treatment 4 times, and set a treatment without reagents (containing all organic solvents and emulsifiers) as a blank control.

[0078] Feeding and observation: The treated mites were placed in (25±1)℃, light cycle L:D=(16:8)h for feeding and observation. After 48h of treatment, the mites were checked for death, and the total number of mites and the number of dead mites were recorded.

[0079] Data statistics and analysis:

[0080] Based on the survey data, the adjusted mortality rate of each treatment was calculated according to the following formula, and the calculation results were retained to two decimal places.

[0081]

[0082] Where:

[0083] P——mortality rate, in percentage (%);

[0084] K——indicates the number of dead insects, in units of heads;

[0085] N——represents the total number of insects treated, in heads.

[0086]

[0087] Where:

[0088] P1——adjusted mortality rate, in percentage (%);

[0089] P t ——Treatment mortality rate, expressed as percentage (%);

[0090] P0——blank control mortality rate, in percentage (%).

[0091] 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 correction mortality formula; if the control mortality rate is greater than 20%, the test needs to be repeated.

[0092] Analyze using the DPS statistical analysis system to find the LC 50Value, to evaluate the activity of the test agent on the biological test material.

[0093] The co-toxicity coefficient (CTC value) of the mixture is calculated as follows:

[0094]

[0095] Where:

[0096] ATI——Actual Toxicity Index of Mixture;

[0097] S——LC of standard acaricide 50 , the unit is milligrams per liter (mg / L);

[0098] M——LC of the mixture 50 , the unit is milligrams per liter (mg / L).

[0099] TTI=TI A ×P A +TI B ×P B

[0100] Where:

[0101] TTI – Theoretical Toxicity Index of Mixtures;

[0102] TI A ——A: toxicity index of the agent;

[0103] P A ——The percentage of agent A in the mixture, in percentage (%);

[0104] TI B ——Toxicity index of agent B;

[0105] P B ——The percentage of agent B in the mixture, in percentage (%).

[0106]

[0107] Where:

[0108] CTC – Co-toxicity coefficient;

[0109] ATI——Actual Toxicity Index of Mixture;

[0110] TTI - Theoretical Toxicity Index of Mixture.

[0111] The co-toxicity coefficient of the combination CTC≥120 shows a synergistic effect; CTC≤80 shows an antagonistic effect; 80<CTC<120 shows an additive effect.

[0112] Indoor activity test is shown in the following table:

[0113] Table 1 Results of indoor biological activity test on compound of formula I and triazotin against Panonychus citri

[0114] Test drug <![CDATA[LC 50 (mg / L)]]> ATI TTI Co-toxicity coefficient (CTC) Compound (A) of formula I 3.1977 100.000 / / Triazotin(B) 15.4767 20.661 / / A:B(1:32) 10.2566 31.177 23.066 135.167 A:B(1:23) 9.1429 34.975 23.967 145.928 A:B(1:15) 8.0327 39.809 25.620 155.380 A:B(1:10) 6.8922 46.396 27.874 166.449 A:B(1:5) 4.9791 64.222 33.884 189.534 A:B(1:1) 2.8993 110.292 60.331 182.813 A:B(5:1) 2.1298 150.141 86.777 173.019 A:B(12:1) 2.2070 144.889 93.897 154.306 A:B(25:1) 2.3024 138.886 96.949 143.257 A:B(30:1) 2.5663 124.604 97.441 127.876 A:B(40:1) 3.2023 99.856 98.065 101.827

[0115] The indoor test results in Table 1 show that the compound of formula I and triazotin have good activity against citrus mites, the mass ratio of the two is 1:32 to 30:1, the co-toxicity coefficient against citrus mites is greater than 120, and the synergistic effect is significant.

[0116] Table 2 Results of indoor biological activity test on compound of formula I and fenbutatin against Panonychus citri

[0117] Test drug <![CDATA[LC 50 (mg / L)]]> ATI TTI Co-toxicity coefficient (CTC) Compound (A) of formula I 3.1977 100.000 / / Phenbutyltin(B) 29.9939 10.661 / / A:B(1:48) 19.4115 16.473 12.484 131.950 A:B(1:32) 16.7223 19.122 13.368 143.042 A:B(1:21) 13.8448 23.097 14.722 156.886 A:B(1:12) 11.3893 28.076 17.533 160.131 A:B(1:7) 7.6238 41.944 21.829 192.151 A:B(3:1) 2.2749 140.564 77.665 180.987 A:B(7:1) 2.1095 151.586 88.833 170.642 A:B(14:1) 2.3217 137.731 94.044 146.454 A:B(21:1) 2.4228 131.984 95.939 137.570 A:B(33:1) 2.6182 122.134 97.372 125.429 A:B(42:1) 2.6755 119.518 97.922 122.054

[0118] The indoor test results in Table 2 show that the compound of formula I and fenbutatin have good activity against Panonychus citri, the mass ratio of the two is 1:48 to 42:1, the co-toxicity coefficient against Panonychus citri is greater than 120, and the synergistic effect is significant.

[0119] Table 3 Results of indoor biological activity test on compound of formula I and triazotin against Tetranychus cinnabarinus

[0120] Test drug <![CDATA[LC 50 (mg / L)]]> ATI TTI Co-toxicity coefficient (CTC) Compound (A) of formula I 0.3087 100.000 / / Triazotin(B) 35.3544 0.873 / / A:B(1:46) 11.242 2.746 2.982 92.077 A:B(1:32) 6.3315 4.876 3.877 125.758 A:B(1:28) 4.9664 6.216 4.291 144.845 A:B(1:14) 2.5428 12.140 7.482 162.267 A:B(1:7) 1.1997 25.731 13.264 193.994 A:B(3:2) 0.2762 111.767 60.349 185.200 A:B(7:1) 0.2252 137.078 87.609 156.466 A:B(10:1) 0.2359 130.861 90.988 143.821 A:B(20:1) 0.2367 130.418 95.280 136.879 A:B(30:1) 0.2520 122.500 96.802 126.547 A:B(45:1) 0.2697 114.461 97.845 116.981

[0121] The indoor test results in Table 3 show that the compound of formula I and triazotin have good activity against Tetranychus cinnabarinus, the mass ratio of the two is 1:32 to 20:1, the co-toxicity coefficient against Tetranychus cinnabarinus is greater than 120, and the synergistic effect is significant.

[0122] Table 4 Results of indoor biological activity test on compound of formula I and fenbutatin against Tetranychus cinnabarinus

[0123]

[0124]

[0125] The indoor test results in Table 4 show that the compound of formula I and fenbutatin have good activity against Tetranychus cinnabarinus, with a mass ratio of 5.5, and a co-toxicity coefficient of more than 120 for Tetranychus cinnabarinus, showing a significant synergistic effect.

[0126] Example 2: Indoor biological activity test of compound miticide on wolfberry gall mite

[0127] Test basis: The test refers to the "Guidelines for Indoor Bioassay Tests of Pesticides - Insecticides Part 13: Leaf Disk Spray Method".

[0128] Test target: Lycium barbarum gall mite (Aceri macrodonis Keifer).

[0129] Test material preparation: Select adult mites with consistent physiological status and wolfberry leaves with consistent growth.

[0130] Preparation of the drug: Dissolve the technical drug of the compound of formula I, the technical drug of fenbutatin and the technical drug of triazotin with a solvent to prepare a mother liquor, and then use a 0.1% Tween-80 aqueous solution to prepare 5 series of mass concentration gradients according to the equal ratio method.

[0131] Test method: Use a pointed brush to pick up healthy, newly emerged adult mites and place them on the front of fresh wolfberry leaves wrapped with wet cotton wool. Pick 15 mites per leaf. After the mites are stable, observe the survival of the mites, remove the dead mites, and add new adult mites. Repeat 4 times for each treatment, with 2 leaves for each treatment, for a total of 30 mites. Use a Potter spray tower to evenly spray different concentrations of liquid medicine on the front of wolfberry leaves. The initial spray volume is 1mL and the spray time is 1min as the standard parameters. Wrap a layer of cotton wool around the treated wolfberry leaves and place them in an incubator with a temperature of 25±1℃, a relative humidity of 70% to 80%, and a photoperiod of L:D=14:10h.

[0132] After 48 hours of treatment, the mortality of mites was checked and the total number of mites and the number of dead mites were recorded respectively.

[0133] Data statistics and analysis:

[0134] Based on the survey data, the adjusted mortality rate of each treatment was calculated according to the following formula, and the calculation results were retained to two decimal places.

[0135]

[0136] Where:

[0137] P——mortality rate, in percentage (%);

[0138] K——indicates the number of dead insects, in units of heads;

[0139] N——represents the total number of insects treated, in heads.

[0140]

[0141] Where:

[0142] P1——adjusted mortality rate, in percentage (%);

[0143] P t ——Treatment mortality rate, expressed as percentage (%);

[0144] P0——blank control mortality rate, in percentage (%).

[0145] 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 correction mortality formula; if the control mortality rate is greater than 20%, the test needs to be repeated.

[0146] Analyze using the DPS statistical analysis system to find the LC 50 Value, to evaluate the activity of the test agent on the biological test material.

[0147] The co-toxicity coefficient (CTC value) of the mixture is calculated as follows:

[0148]

[0149] Where:

[0150] ATI——Actual Toxicity Index of Mixture;

[0151] S——LC of standard acaricide 50 , the unit is milligrams per liter (mg / L);

[0152] M——LC of the mixture 50 , the unit is milligrams per liter (mg / L).

[0153] TTI=TI A ×P A +TI B ×P B

[0154] Where:

[0155] TTI – Theoretical Toxicity Index of Mixtures;

[0156] TI A ——A: toxicity index of the agent;

[0157] P A ——The percentage of agent A in the mixture, in percentage (%);

[0158] TI B ——Toxicity index of agent B;

[0159] P B ——The percentage of agent B in the mixture, in percentage (%).

[0160]

[0161] Where:

[0162] CTC – Co-toxicity coefficient;

[0163] ATI——Actual Toxicity Index of Mixture;

[0164] TTI - Theoretical Toxicity Index of Mixture.

[0165] The co-toxicity coefficient of the combination CTC ≥ 120 shows a synergistic effect; CTC ≤ 80 shows an antagonistic effect; 80 < CTC < 120 shows an additive effect.

[0166] Indoor activity test is shown in the following table:

[0167] Table 5 Results of indoor biological activity test on wolfberry gall mites with compound of formula I and triazotin

[0168]

[0169]

[0170] The indoor test results in Table 5 show that the compound of formula I and triazotin have good activity against wolfberry gall mites, the mass ratio of the two is 1:26 to 32:1, the co-toxicity coefficient to wolfberry gall mites is greater than 120, and the synergistic effect is significant.

[0171] Table 6 Results of indoor biological activity test on wolfberry gall mites with compound of formula I and fenbutatin

[0172] Test drug <![CDATA[LC 50 (mg / L)]]> ATI TTI Co-toxicity coefficient (CTC) Compound (A) of formula I 6.6087 100.000 / / Phenbutyltin(B) 24.3524 27.138 / / A:B(1:30) 17.6691 37.403 29.488 126.839 A:B(1:20) 16.1809 40.843 30.607 133.440 A:B(1:10) 12.3670 53.438 33.762 158.281 A:B(1:5) 10.0148 65.989 39.281 167.991 A:B(1:3) 7.9577 83.048 45.353 183.113 A:B(2:1) 4.9816 132.662 75.713 175.218 A:B(5:1) 4.514 146.405 87.856 166.641 A:B(10:1) 4.9737 132.873 93.376 142.299 A:B(15:1) 5.0658 130.457 95.446 136.682 A:B(20:1) 5.2943 124.827 96.530 129.313 A:B(30:1) 5.4116 122.121 97.650 125.060

[0173] The indoor test results in Table 6 show that the compound of formula I and fenbutatin have good activity against wolfberry gall mites, the mass ratio of the two is 1:30 to 30:1, the co-toxicity coefficient to wolfberry gall mites is greater than 120, and the synergistic effect is significant.

[0174] Field efficacy test:

[0175] Example 3: Field trial to control citrus spider mites

[0176] Test crops: citrus trees, the variety is sugar orange.

[0177] Test target: Panonychus citri.

[0178] Test location: The test was conducted in the citrus orchard in Gugan Village, Dahua Town, Dahua County, Hechi City, Guangxi Zhuang Autonomous Region. The trees in the test site were two years old, and the fertilizer and water management was consistent, and the citrus grew uniformly. The fertility conditions were moderate, which was in line with local scientific agricultural practices.

[0179] Test drugs: See Table 7 for test and control drugs and dosage.

[0180] Experimental arrangement: 2 fruit trees per plot, each treatment was repeated 4 times, and all experimental plots were arranged in random blocks.

[0181] Experimental method: This experiment only applied the pesticide once, on July 22, 2023. The diluted pesticide was evenly sprayed on the citrus leaves, and the blank control was sprayed with an equal amount of clean water.

[0182] Survey time and frequency: mite population density surveys were conducted before application and on the 3rd and 15th days after application. Tender shoots were marked in the east, west, south, north and center of the tree in each plot. The number of active mites on 25 leaves was surveyed and the number of live mites was counted.

[0183] Calculation method of drug efficacy:

[0184]

[0185]

[0186] Results and Analysis:

[0187] Table 7 Results of field trials for controlling citrus spider mites

[0188]

[0189] The results of the field efficacy test for controlling citrus spider mites show that compounding the compound of formula I with either triazotin or fenbutatin has a good control effect on controlling citrus spider mites in the field.

[0190] Example 4: Field trial to control wolfberry gall mites

[0191] Test crops: wolfberry (Ningqi No. 1), with a tree age of about 5 years.

[0192] Test subject: Lycium barbarum gall mite (Aceri macrodonis Keifer).

[0193] Test and control drugs: See Table 8 for test and control drugs and dosage.

[0194] Test location: The test was conducted in a wolfberry plantation in Jingyuan County, Baiyin City, Gansu Province. The wolfberry trees in the test site were about 5 years old, and the tree vigor was consistent. The soil fertility of the test site was medium, the ground was flat, and the irrigation conditions were good.

[0195] Experimental arrangement: Each experimental plot has an area of ​​30m 2 Each treatment was repeated 4 times, and the plots were arranged in random blocks. Protective rows or isolation belts were set between the plots. In the early stage of the occurrence of wolfberry gall mites, the whole wolfberry tree was sprayed with a Gongnong-16 backpack electric sprayer. The front and back of each leaf were evenly sprayed with the liquid, and the leaves were moistened and no droplets fell. The test was conducted twice, with an interval of 7 days.

[0196] Survey method: 7 days and 14 days after the second application of pesticides, the gall mite damage in each plot was investigated. Two wolfberry plants were investigated in each plot, and one branch of the current year was investigated in the east, south, west, north and center of each tree and marked with a sign. 25 leaves at the top of each branch were investigated, and the total number of leaves and the number of damaged leaves at each level were recorded. The mite index was investigated and the control effect was calculated.

[0197] Grading Standard:

[0198] Level 0: leaves are not damaged;

[0199] Level 1: There are only 1 to 2 gall spots smaller than 1 mm on the leaves;

[0200] Level 3: There are 2 to 3 gall spots on the leaves that are larger than 1 mm and smaller than 2 mm;

[0201] Level 5: There are more than 3 gall spots smaller than 2 mm on the leaves;

[0202] Level 7: Gall spots larger than 2 mm on leaves;

[0203] Level 9: Deformed leaves or twigs appear due to severe infestation by gall mites.

[0204] Calculation method of drug efficacy:

[0205]

[0206]

[0207] Results and Analysis:

[0208] Table 8 Field test results for the control of wolfberry gall mites

[0209]

[0210] It can be seen from the field efficacy experiment that the acaricide of the present invention has significant control effect on wolfberry gall mites. The test was applied twice in total, and the control effect was investigated 7 days after the second application. The overall control effect of the compound preparation on wolfberry gall mites was above 84%; 14 days after the second application, the control effect of 18% formula I compound·triazoxan suspension (1:5) was as high as 94.17%.

[0211] Although the present invention has been described in detail above with general descriptions 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. An acaricide containing an organotin compound, characterized in that: The acaricide comprises active ingredient A and active ingredient B, wherein the active ingredient A is a compound of formula I: The active ingredient B is an organic tin compound, the organic tin compound is triazotin or fenbutatin, and the mass ratio of the active ingredient A to the active ingredient B is 1:50 to 45:

1.

2. The acaricide according to claim 1, characterized in that The mass ratio of the active ingredient A to the active ingredient B is 1:48 to 42:

1.

3. The acaricide according to claim 1, characterized in that The active ingredient B is triazotin, and the mass ratio of the active ingredient A to the active ingredient B is 1:32 to 30:1; Preferably, the active ingredient B is triazotin, and the mass ratio of the active ingredient A to the active ingredient B is 1:26 to 32:

1.

4. The acaricide according to claim 1, characterized in that The active ingredient B is fenbutatin, and the mass ratio of the active ingredient A to the active ingredient B is 1:40 to 30:1; Preferably, the active ingredient B is fenbutatin, and the mass ratio of the active ingredient A to the active ingredient B is 1:30 to 30:

1.

5. The acaricide according to claim 1, characterized in that The total weight of the acaricide is 100 wt %, and the total weight of the active ingredient A and the active ingredient B accounts for 2% to 70% of the total weight of the acaricide.

6. The acaricide according to claim 1, characterized in that The acaricide comprises 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, defoaming agents, solvents, preservatives, stabilizers, synergists or carriers.

7. The acaricide according to claim 1, characterized in that The acaricide can be prepared into a formulation form permitted by pesticides, and the formulation form is a solid formulation and / or a liquid formulation.

8. The acaricide according to claim 7, characterized in that The solid preparation is a water-dispersible granule, a wettable powder, a granule, a soluble powder or an emulsion; the liquid preparation is a soluble solution, a soluble gel, an emulsifiable concentrate, an aqueous emulsion, an oil emulsion, a microemulsion, a suspension, a microcapsule suspension, an oil suspension, a dispersible oil suspension or a suspoemulsion.

9. Use of the acaricide according to any one of claims 1 to 8 for controlling harmful mites.

10. The use according to claim 9, characterized in that: The harmful mites are pest mites of the Tetranychidae family and / or the Gall Mite family. The pest mites of the Tetranychidae family are Tetranychus cinnabarinus, Tetranychus urticae or Panonychus citri, and the harmful mites of the Gall Mite family are Citrus rust mite or Lycium barbarum gall mite.

Citation Information

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