Insecticide mother liquor and application thereof

Abstract

The invention discloses an insecticide mother liquor and application thereof. The insecticide mother liquor is prepared by taking efficient pyrethroid as shown in a formula I as an active ingredient; the mother liquor can be processed into mosquito-repellent incense, fly incense, electrothermal mosquito-repellent incense liquid, electrothermal mosquito-repellent incense pieces, aerosol, mothproof tablets or mosquito-repellent nets, and is used for preventing and treating mosquitoes, flies, German cockroaches, American cockroaches, bugs, ants, fleas, bees and other sanitary pests. According to the insecticide mother liquor, the usage amount of an organic solvent can be reduced, the environment is protected, and meanwhile the purposes of increasing efficiency and reducing application are achieved; on the other hand, the mother liquor can be diluted in different proportions by using a solvent and then processed into corresponding dosage forms, so that the use is convenient. # imgabs0 #

Description

[0001] This application is a divisional application of the Chinese invention patent application. The original application date is July 13, 2022, application number 202210823424.2, the name of the invention: A pesticide mother solution and its application, publication number: CN115669677A; the applicant filed a divisional application. Technical Field

[0002] The invention relates to an insecticide mother solution and application thereof. Background Art

[0003] The pyrethroid compound shown in formula I is a novel sanitary insecticide with good basic activity in preventing and controlling sanitary pests; the pyrethroid compound shown in formula I can be prepared according to the following reaction route:

[0004]

[0005] Wherein R is methyl or ethyl, M is sodium or potassium and R1 is hydrogen.

[0006] For example, 3-formyl-2,2-dimethylcyclopropanecarboxylic acid methyl ester (CAS No. 62138-41-4) is used as the starting material, and acetonitrile is reacted with sodium ethoxide at 60°C for 4 hours, dilute hydrochloric acid is added to neutralize the pH to 8, ethyl acetate and water are added to separate, and the oil layer is desolvated to obtain the intermediate 3-(2-cyano-1-vinyl)-2,2-dimethylcyclopropanecarboxylic acid methyl ester.

[0007] 2,3,5,6-tetrafluorobenzyl alcohol, a catalytic amount of tetraisopropyl titanate and a toluene solvent are added to the obtained 3-(2-cyano-1-vinyl)-2,2-dimethylcyclopropanecarboxylic acid methyl ester, and the temperature is slowly raised to reflux to remove the by-product methanol, and the gas phase is controlled. After the raw material is completely converted, the temperature is lowered to 0-5° C., a small amount of water is added dropwise, the liquids are separated, and the solvent is removed to obtain the pyrethroid compound of formula I.

[0008] Using cyclopropanecarboxylates of different single configurations as starting materials, pyrethroid compounds of formula I of corresponding configurations can be obtained. For example, using (1R, 3R)-3-formyl-2,2-dimethylcyclopropanecarboxylic acid methyl ester (CAS No. 27335-33-7) as the starting material for synthesis, the obtained product is the 1R, 3R part of the chrysanthemum acid. After distributed crystallization and separation of the double bond CN group Z, E isomers, a single 2,3,4,5-tetrafluorobenzyl-(1R, 3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate or 2,3,4,5-tetrafluorobenzyl-(1R, 3R)-3-[(1E)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate can be obtained. 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-(-2-cyano-1-vinyl)-2,2-dimethylcyclopropylcarboxylate or 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate or 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1E)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate can be obtained from methyl (1R,3S)-3-(-2-cyano-1-vinyl)-2,2-dimethylcyclopropylcarboxylate.

[0009] However, the preparation of the pyrethroid compound shown in I can be applied to the process of preparing preparations for controlling sanitary pests. If conventional solvents such as xylene and dichloromethane are used, although they have good solubility, these solvents are not environmentally friendly, and because the above solvents have an unpleasant odor, they are also difficult to be accepted by consumers in actual use; on the other hand, in the prior art, odorless kerosene is generally used to dissolve and dilute the sanitary pyrethroid original drug, but since kerosene has a low solubility in the compound of formula I of the present invention, a large amount of kerosene needs to be used, resulting in a problem of solvent waste. In order to solve the above problems, the present invention studies the mother solution of the compound of formula I and its application. Summary of the invention

[0010] The technical problem to be solved by the present invention is to provide an insecticide mother solution and its application in view of the deficiencies in the prior art, wherein the insecticide mother solution is prepared by using the high-efficiency pyrethroid shown in formula I as an active ingredient; the insecticide mother solution of the present invention can be processed into mosquito coils, fly coils, electric mosquito coil liquid, electric mosquito coil tablets, aerosols, moth-proof tablets or mosquito nets, and is used for preventing and controlling mosquitoes, flies, German cockroaches, American cockroaches, bedbugs, ants, fleas, bees and other sanitary pests.

[0011] In order to achieve the above object, the present invention adopts the following technical solution:

[0012] A pesticide mother solution, comprising component A and component B, wherein the total weight of component A and component B accounts for 90%-99.99% of the total weight of the pesticide mother solution, and the remainder is other components; the component A accounts for 0.1%-30% of the total weight of component A and component B;

[0013] The component A is a compound shown in formula I;

[0014] The component B is a solvent;

[0015]

[0016] In the above technical solution, the component A preferably accounts for 5%-20% of the total weight of the components A and B.

[0017] In the above technical scheme, the component A shown is 2,3,4,5-tetrafluorobenzyl-3-[-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, preferably selected from 2,3,4,5-tetrafluorobenzyl-(1R, 3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 2,3,4,5-tetrafluorobenzyl-(1S, 3R)-3-[(1Z)-2-cyano-1-vinyl] Any one of the four isomers of 2,3,4,5-tetrafluorobenzyl-(1R, 3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, or a mixture of two or more of the four isomers in any proportion.

[0018] In the above technical solution, the component A is preferably 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate.

[0019] The component B described in the above technical scheme is selected from C8-18 alkane solvents; deionized water; dodecylbenzene, decanylbenzene; amide solvents such as N,N-dimethyl cinnamamide; γ-butyrolactone; monocarboxylic acid ester solvents such as methyl oleate, isopropyl tridecanoate, isopropyl myristate, isopropyl hexadecanoate, isopropyl phenylacetate, ethyl phenylacetate, and n-butyl myristate; dicarboxylic acid ester solvents such as diisopropyl glutarate, diisopropyl adipate, and diisobutyl adipate; tricarboxylic acid ester solvents such as tributyl citrate and acetylcitrate tributyl; alcohol ether solvents such as triethylene glycol monobutyl ether, diethylene glycol monobutyl ether, and propylene glycol methyl ether; C2-8 alcohol solvents; any one of the compounds shown in formula II and the compounds shown in formula III, or a mixture formed by mixing two or more of them in any proportion;

[0020]

[0021] Wherein R1 and R2 are both C1-C10 alkyl groups.

[0022] The component B described in the above technical solution is preferably N,N-dimethylbutylamine; γ-butyrolactone; diisopropyl adipate, tributyl citrate, acetyl tributyl citrate, and isopropyl myristate.

[0023] In the above technical scheme, the C8-18 alkane solvent is preferably D60 (ExxonMobil Petrochemical Company), D80 (ExxonMobil Petrochemical Company), D100 (ExxonMobil Petrochemical Company), D110 (ExxonMobil Petrochemical Company), Isopar-E (ExxonMobil Petrochemical Company), Isopar-G (ExxonMobil Petrochemical Company), Isopar-H (ExxonMobil Petrochemical Company), Isopar-L (ExxonMobil Petrochemical Company), Isopar-M (ExxonMobil Petrochemical Company), octane, nonane, quinane, undecane, dodecane, tridecane, tetradecane, pentadecane, hexadecane, or any one of them, or a mixture of two or more of them in any proportion.

[0024] In the above technical scheme, the C2-8 alcohol solvent is preferably any one of ethanol, isopropanol, n-propanol, n-butanol, sec-butanol, tert-butanol, n-pentanol and its isomers, n-hexanol and its isomers, n-heptanol and its isomers, n-octanol and its isomers, or a mixture of two or more in any proportion.

[0025] In the above technical solution, the other components are any one of the synergist and the phenol antioxidant, or a mixture of the two in any proportion.

[0026] In the above technical solution, the synergist preferably accounts for 0.01%-8% of the total weight of the insecticide mother solution; the synergist is preferably any one of oxidized piperonyl butoxide, synergistic amine or triphenyl phosphate.

[0027] In the above technical scheme, the phenol antioxidant preferably accounts for 0.05%-2% of the total weight of the insecticide mother solution; the phenol antioxidant is preferably selected from any one of 2,6-di-tert-butyl-4-methylphenol, β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate, butylated hydroxyanisole, and β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate, or a mixture of two or more in any proportion.

[0028] The present invention also provides an application of the above insecticide mother solution in preventing and controlling sanitary pests.

[0029] In the above technical solution, the sanitary pests refer to mosquitoes, flies, German cockroaches, American cockroaches, bedbugs, ants, fleas, bees, etc.

[0030] In the above technical scheme, the sanitary pests are preferably Culex pipiens pallens, Culex pipiens quinquefasciatus, Culex tritaeniorhynchus, Aedes albopictus, Aedes aegypti, Anopheles sinensis, Aedes harassingus, Chironomids, housefly, city fly, Chrysopa longituba, Lucilia sericata, Lucilia cuprina, Lucilia brighten, summer toilet fly, Yuan toilet fly, German cockroach, American cockroach, bedbugs, ants, fleas, bees, wasps, bumblebees, bumblebees, wasps, etc.

[0031] In the above technical scheme, when the insecticide mother liquid is used to control sanitary pests, it is used by diluting it by 1-100 times by weight with odorless kerosene or C8-C18 alkane solvent to prepare mosquito coils, fly coils, electric mosquito coil liquid, electric mosquito coil tablets, aerosols, moth-proof tablets or mosquito nets for use.

[0032] In the above technical scheme, the C8-C18 alkane solvent is selected from D60 (ExxonMobil Petrochemical Company), D80 (ExxonMobil Petrochemical Company), D100 (ExxonMobil Petrochemical Company), D110 (ExxonMobil Petrochemical Company), Isopar-E (ExxonMobil Petrochemical Company), Isopar-G (ExxonMobil Petrochemical Company), Isopar-H (ExxonMobil Petrochemical Company), Isopar-L (ExxonMobil Petrochemical Company), Isopar-M (ExxonMobil Petrochemical Company), octane, nonane, quinane, undecane, dodecane, tridecane, tetradecane, pentadecane, hexadecane, heptadecane, octadecane, any one of them, or a mixture of two or more of them in any proportion.

[0033] The insecticide mother solution of the present invention can reduce the usage of organic solvents, protect the environment, and achieve the purpose of increasing efficiency and reducing application; on the other hand, the mother solution can be diluted with solvents in different proportions and then processed into corresponding dosage forms, which is convenient to use. DETAILED DESCRIPTION

[0034] The specific implementation of the technical solution of the present invention is described in detail below, but the present invention is not limited to the following description:

[0035] The preparation method of the dosage form in each embodiment of the present invention is as follows: the component A, component B and other components are mixed in a certain proportion at room temperature or under heating conditions to prepare a corresponding mother solution.

[0036] The present invention will be described below in conjunction with specific embodiments:

[0037] Formulation Example 1:

[0038] 0.5g 2,3,4,5-tetrafluorobenzyl-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate (the four isomers ((1R, 3S), (1S, 3R), (1R, 3R), and (1S, 3S) each account for 25%), 1g of oxidized piperonyl butoxide, and isopropyl myristate is added to make up to 100g to obtain a 0.5% mother liquor.

[0039] Formulation Example 2:

[0040] 0.5 g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 1 g of piperonyl butoxide, and isopropyl myristate to make up to 100 g to obtain a 0.5% mother liquor.

[0041] Formulation Example 3:

[0042] 0.5 g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 1 g of piperonyl butoxide, and dodecylbenzene are added to make up to 100 g to obtain a 0.5% mother liquor.

[0043] Formulation Example 4:

[0044] 0.5 g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 1 g piperonyl butoxide, and diisopropyl adipate to make up to 100 g to obtain a 0.5% mother liquor.

[0045] Formulation Example 5:

[0046] 5g 2,3,4,5-tetrafluorobenzyl-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate ((1R, 3S): (1S, 3R) = 4:1), 0.5g β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate, 5g N,N-dimethylcaprylamide, and diisobutyl adipate are added to make up to 100g to obtain 5% mother liquor.

[0047] Formulation Example 6:

[0048] 6 g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 0.2 g 2,6-di-tert-butyl-4-methylphenol, and diisopropyl adipate to make up to 100 g to obtain 6% mother liquor.

[0049] Formulation Example 7:

[0050] 5g 2,3,4,5-tetrafluorobenzyl tributyl citrate-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate ((1R, 3S): (1S, 3R) = 5:1), 3g piperonyl butoxide, 20g tributyl citrate, and isopropyl myristate to make up to 100g to obtain a 5% mother liquor.

[0051] Preparation Example 8:

[0052] 5g 2,3,4,5-tetrafluorobenzyl-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate ((1R, 3S): (1S, 3R) = 3:1), 1g of piperonyl butoxide, and the amount of isopropyl myristate is made up to 100g to obtain a 5% mother liquor.

[0053] Formulation Example 9:

[0054] 0.1g 2,3,4,5-tetrafluorobenzyl-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate (the four isomers ((1R, 3S), (1S, 3R), (1R, 3R), and (1S, 3S) each account for 25%), 0.01g synergist amine, 0.1g butylated hydroxyanisole, 10g D110, and tributyl citrate is added to make up to 100g to obtain a 0.1% mother liquor.

[0055] Formulation Example 10:

[0056] 10g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 1g 2,6-di-tert-butyl-4-methylphenol, 20g deionized water, and triethylene glycol monobutyl ether are added to 100g to obtain a 10% mother liquor.

[0057] Formulation Example 11:

[0058] 5g 2,3,4,5-tetrafluorobenzyl-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate ((1R, 3S): (1S, 3R) = 6:1), 0.5g β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester, 10g N,N-dimethylcaprylamide, 10g ethyl phenylacetate, and diisobutyl adipate to 100g to obtain 5% mother liquor.

[0059] Formulation Example 12:

[0060] 27g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 5g synergist amine, 2g 2,6-di-tert-butyl-4-methylphenol, and isopropyl tridecanoate are added to make up to 100g to obtain 27% mother liquor.

[0061] Formulation Example 13:

[0062] 10g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 1g 2,6-di-tert-butyl-4-methylphenol, and isopropyl tridecanoate are added to make up to 100g to obtain a 10% mother liquor.

[0063] Formulation Example 14:

[0064] 10g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 1g 2,6-di-tert-butyl-4-methylphenol, and tributyl citrate are added to make up to 100g to obtain a 10% mother liquor.

[0065] Formulation Example 15:

[0066] 10g 2,3,4,5-tetrafluorobenzyl-(1S,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 1g 2,6-di-tert-butyl-4-methylphenol, and isopropyl tridecanoate are added to make up to 100g to obtain a 10% mother liquor.

[0067] Formulation Example 16:

[0068] 6g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 0.2g β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid isooctyl ester, and diisopropyl adipate is added to make up to 100g to obtain 6% mother liquor.

[0069] Formulation Example 17:

[0070] 6g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 0.2g β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid n-octadecyl ester, and diisopropyl adipate are added to make up to 100g to obtain 6% mother liquor.

[0071] Formulation Example 18:

[0072] 20g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 0.4g β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionic acid n-octadecyl ester, and diisopropyl adipate are added to make up to 100g to obtain a 20% mother liquor.

[0073] Formulation Example 19:

[0074] 16g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 1g 2,6-di-tert-butyl-4-methylphenol, 45g isopropyl tridecanoate, and diisopropyl adipate is added to make up to 100g to obtain 16% mother liquor.

[0075] Formulation Example 20:

[0076] 6g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 0.2g 2,6-di-tert-butyl-4-methylphenol, dodecylbenzene is added to make up to 100g to obtain 6% mother liquor.

[0077] Formulation Example 21:

[0078] 6g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 0.2g 2,6-di-tert-butyl-4-methylphenol, and acetyl tributyl citrate are added to make up to 100g to obtain 6% mother liquor.

[0079] Formulation Example 22:

[0080] 0.5 g of 2,3,4,5-tetrafluorobenzyl-3-[-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 1 g of piperonyl butoxide, and diisopropyl adipate to make up to 100 g to obtain a 0.5% mother liquor.

[0081] Preparation Example 23 (different from the active ingredient of Preparation Example 13):

[0082] 10 g of 2,3,4,5-tetrafluorobenzyl-3-[-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 1 g of 2,6-di-tert-butyl-4-methylphenol, and isopropyl tridecanoate are added to make up to 100 g to obtain a 10% mother liquor.

[0083] Formulation Example 24:

[0084] 6 g of 2,3,4,5-tetrafluorobenzyl-3-[-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 0.2 g of 2,6-di-tert-butyl-4-methylphenol, and diisopropyl adipate to make up to 100 g to obtain a 6% mother liquor.

[0085] Formulation Example 25:

[0086] 16 g of 2,3,4,5-tetrafluorobenzyl-3-[-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 1 g of 2,6-di-tert-butyl-4-methylphenol, 45 g of isopropyl tridecanoate, and diisopropyl adipate is added to make up to 100 g to obtain a 16% mother liquor.

[0087] The test materials in the efficacy examples of the present invention are: Culex pipiens pallens, female adults that have not sucked blood on the 3rd to 5th day after emergence; houseflies, adults on the 3rd to 4th day after emergence, half of which are male and half are female; German cockroaches, adults that are 10-15 days old, half of which are male and half are female.

[0088] Pharmacological Example 1:

[0089] 120 g of water was added to a mixture of 99.96 g of corn starch, carbon powder and wood powder (1:5:4) and kneaded into a shape, and then dried to form a mosquito coil substrate (diameter 12.0 cm, thickness 4 mm, one pair weighing 40 g)

[0090] Spray 4 g of the mother liquor of Formulation Example 1, Formulation Example 2, Formulation Example 4 and Formulation Example 22 onto the above-mentioned mosquito coil substrate to obtain 0.05% disc mosquito coil I, disc mosquito coil II, disc mosquito coil III and disc mosquito coil V, respectively.

[0091] 0.5g 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 1g oxidized piperonyl butoxide, and odorless kerosene to 100g to obtain a 0.5% mother liquor. Take 4g of the above mother liquor and spray it on the above mosquito coil substrate to obtain a disc mosquito coil IV.

[0092] The above-mentioned disc mosquito coils I-IV were compared for efficacy according to "GBT 13917.4-2009 Indoor efficacy test and evaluation of sanitary insecticides for pesticide registration Part 4: Mosquito coils". A cylindrical device was used. 30 test mosquitoes were sucked in and placed in the central circular hole of the original plate (F) below the cylinder, and the rubber plug (H) was plugged in tightly. After the test mosquitoes resumed normal activities, a section of the mosquito coil to be tested was randomly taken, horizontally placed on the mosquito coil rack, pre-ignited for 5 minutes elsewhere, moved to the cylinder for fumigation for 1 minute, and the mosquito coil was immediately removed, plugged with the rubber plug (H), and timed. The number of test insects knocked down was recorded at regular intervals. The observation time limit is 20 minutes. The test should be repeated three times or more, and the mosquito coils used for repeated tests should be randomly taken. After each test, the test device should be cleaned. The test results are shown in the following table:

[0093] Mosquito-repellent coils Concentration w / w Culex pipiens KT50(min) Coil mosquito coil I 0.05％ 3.8 Coil mosquito coil II 0.05％ 2.6 Coil mosquito coil III 0.05％ 2.3 Coil mosquito coil IV 0.05％ 3.4 Coil mosquito coil V 0.05％ 3.1

[0094] Pharmacological Example 2:

[0095] The preparation example, odorless kerosene, propane and butane are mixed in a certain proportion at room temperature and added into a tank equipped with a control valve, and a propellant is added into the tank under pressure through the control valve to obtain the product.

[0096] Aerosol I: 5 g of Formulation Example 13 and 45 g of odorless kerosene were mixed at room temperature and added to a can equipped with a control valve. 50 g of propane propellant was added to the can under pressure through the control valve to prepare 0.5% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate.

[0097] Aerosol II: 5 g of Formulation Example 14 and 45 g of odorless kerosene were mixed at room temperature and added to a can equipped with a control valve. 50 g of propane propellant was added to the can under pressure through the control valve to prepare 0.5% 2,3,4,5-tetrafluorobenzyl-(1R,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate.

[0098] Aerosol III: 5 g of Formulation Example 15 and 45 g of odorless kerosene were mixed at room temperature and added to a can equipped with a control valve. 50 g of propane propellant was added to the can under pressure through the control valve to obtain 0.5% 2,3,4,5-tetrafluorobenzyl-(1S,3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate.

[0099] Aerosol IV: 5 g of Formulation Example 23 and 45 g of odorless kerosene were mixed at room temperature and added to a can equipped with a control valve, and 50 g of propane-butane propellant was added to the can under pressure through the control valve to obtain a 0.5% component A formula.

[0100] Control aerosol: 0.5 g 2,3,4,5-tetrafluorobenzyl-(1R, 3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 0.05 g 2,6-di-tert-butyl-4-methylphenol, odorless kerosene is added to 50 g, heated to dissolve, cooled to room temperature and added to a tank equipped with a control valve, and 50 g of propane propellant is added to the tank under pressure through the control valve to obtain 0.5% 2,3,4,5-tetrafluorobenzyl-(1R, 3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate.

[0101] Test method: Refer to GB / T 13917.2-2009 Indoor efficacy test and evaluation of hygienic insecticides for pesticide registration Part 2: Aerosol method. Mosquitoes and flies: Use a cylinder device. The specific method is to put the test insects (30 houseflies or 30 mosquitoes) into the cylinder. After the test insects resume normal activities, the aerosol cylinder to be tested is horizontal, the nozzle is vertically downward, aimed at the spray hole, and the agent (1.0±0.1g) is sprayed. The round hole is immediately plugged with a rubber plug (G). After 1min, the pull plate (A) is removed, and the time is immediately counted. The number of knocked-down test insects is recorded at regular intervals. After 20min, the knocked-down test insects are moved to a clean insect cage, the feeding standard is restored, and they are fed with 5% sugar water cotton balls. The number of dead insects is checked for 24h, and the unknocked test insects are counted as live insects. The test should be repeated three times or more. The test device should be cleaned at the end of each test.

[0102] Cockroaches: Use a cylindrical device without pulling the board. Place 20 German cockroaches in a cylinder B with a circle of vaseline on the upper inner wall and sealed with a 12-mesh iron screen. After the test insects resume normal activities, place the aerosol cylinder horizontally, aim the nozzle vertically downward at the spray hole on E, spray the agent (1.0±0.1g), immediately plug the round hole with a rubber stopper (G), start timing, and record the number of knocked-down test insects at regular intervals. After 20 minutes, transfer all the test insects to a clean container and resume standard feeding. Feed with mixed feed blocks and soaked cotton balls, and check the number of dead insects for 72 hours. The test should be repeated three times or more. At the end of each test, the test device should be cleaned. The detailed results are shown in the following table:

[0103]

[0104]

[0105] Pharmacological Example 3:

[0106] Electric mosquito-repellent liquid I: 16.7 g of preparation example 6, 40 g of D100 and 43.3 g of D110 were fully mixed, filtered, filled, and equipped with an inner plug and a wood fiber core rod to obtain electric mosquito-repellent liquid I.

[0107] Electric mosquito-repellent liquid II: 10 g of preparation example 18, 20 g of D130 and 70 g of D110 were fully mixed, filtered, filled, and equipped with an inner plug and a ceramic core rod to obtain electric mosquito-repellent liquid II.

[0108] Electric mosquito-repellent liquid III: 16.7 g of preparation example 20, 40 g of D100 and 43.3 g of D110 were fully mixed, filtered, filled, and equipped with an inner plug and a wood fiber core rod to obtain electric mosquito-repellent liquid III.

[0109] Electric mosquito-repellent liquid IV: 16.7 g of preparation example 21, 40 g of D100 and 43.3 g of D110 were fully mixed, filtered, filled, and equipped with an inner plug and a wood fiber core rod to obtain electric mosquito-repellent liquid IV.

[0110] Electric mosquito-repellent liquid V: 16.7 g of preparation example 24, 40 g of D100 and 43.3 g of D110 were fully mixed, filtered, filled, and equipped with an inner plug and a wood fiber core rod to obtain electric mosquito-repellent liquid V.

[0111] Test method: Refer to GBT 13917.6-2009 Indoor efficacy test and evaluation of hygienic insecticides for pesticide registration Part 6: Electric mosquito-repellent liquid and use a cylindrical device: 30 test mosquitoes are sucked in each test, and they are put into the central circular hole of the circular plate (F) and plugged with a rubber plug (H). After the test insects resume normal activities, the heater containing the electric mosquito-repellent liquid to be tested, which is continuously powered on to the corresponding time period, is placed under the central empty space of the circular plate (F), close to the central hole, and fumigated for 1 minute. The rubber plug (H) is immediately plugged in, and the time is counted. The number of test insects knocked down is recorded at regular intervals. The observation time is 20 minutes. The test should be repeated three times or more. The test device should be cleaned after each test.

[0112] Control sample 1: 0.31% tetrafluoromethyl ether electric mosquito-repellent liquid (commercially available)

[0113]

[0114] Pharmacological Example 4:

[0115] Electric mosquito-repellent coil I, 62.5g of formulation example 19 and 37.5g of D110 are fully mixed and filtered, and then 100mg is absorbed and evenly impregnated into a base material (a fiberboard of a compressed mixture of pulp and cotton wool: 2.5cm*1.5cm, thickness 0.3cm) to obtain an electric mosquito-repellent coil.

[0116] Electric mosquito coil II, 62.5g of preparation example 25 and 37.5g of D110 are fully mixed and filtered, and then 100mg is absorbed and evenly impregnated into a base material (a fiberboard of a compressed mixture of pulp and cotton wool: 2.5cm*1.5cm, thickness 0.3cm) to obtain an electric mosquito coil.

[0117] Test method: Refer to GBT 13917.5-2009 Indoor efficacy test and evaluation of hygienic insecticides for pesticide registration Part 5: Electric mosquito coils and use a cylindrical device: 30 test mosquitoes are sucked in each test, and put into the central circular hole of the circular plate (F), and the rubber plug (H) is plugged in tightly. After the test insects resume normal activities, the heater with the electric mosquito coil to be tested (a wire mesh is placed above the heater) is continuously powered on to the corresponding time period and placed under the central empty space of the circular plate (F), and the central circular hole is tightly fastened. Fumigation is carried out for 1 minute, and the rubber plug (H) is immediately plugged in, and the time is counted. The number of test mosquitoes knocked down is recorded at regular intervals. The observation time is 20 minutes. The test should be repeated three times or more. The test device should be cleaned after each test.

[0118] Control sample 2 5mg prallethrin + 5mg tetrafluthrin electric mosquito coil (commercially available)

[0119]

[0120] The above examples are only for illustrating the technical concept and technical features of the present invention, and cannot be used to limit the protection scope of the present invention. Any equivalent transformation or modification made according to the essence of the present invention should be included in the protection scope of the present invention.

Claims

1. A pesticide mother solution, characterized in that: Comprising component A and component B, the total weight of component A and component B accounts for 90%-99.99% of the total weight of the insecticide mother solution, and the remainder is other components; the component A accounts for 0.1%-30% of the total weight of component A and component B; The component A is a compound shown in formula I; The component B is one or more of deionized water, dodecylbenzene, N,N-dimethyl decanoate, isopropyl tridecanoate, isopropyl tetradecanoate, ethyl phenylacetate, diisopropyl adipate, diisobutyl adipate, tributyl citrate, acetyl tributyl citrate or triethylene glycol monobutyl ether; 2. The insecticide mother solution according to claim 1, characterized in that The component A accounts for 5%-20% of the total weight of the components A and B; the component A is 2,3,4,5-tetrafluorobenzyl-3-[-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate.

3. The insecticide mother solution according to claim 1, characterized in that The component A shown is any one of the four isomers of 2,3,4,5-tetrafluorobenzyl-(1R, 3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 2,3,4,5-tetrafluorobenzyl-(1S, 3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, 2,3,4,5-tetrafluorobenzyl-(1R, 3R)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, and 2,3,4,5-tetrafluorobenzyl-(1S, 3S)-3-[(1Z)-2-cyano-1-vinyl]-2,2-dimethylcyclopropylcarboxylate, or a mixture of two or more of them in any proportion.

4. The insecticide mother solution according to claim 1, characterized in that The other components are any one of the synergist and the phenol antioxidant or a mixture of the two in any proportion.

5. The insecticide mother solution according to claim 4, characterized in that The synergist accounts for 0.01%-8% of the total weight of the insecticide mother solution; the synergist is selected from any one of oxidized piperonyl butoxide, synergistic amine or triphenyl phosphate.

6. The insecticide mother solution according to claim 4, characterized in that The phenol antioxidant accounts for 0.05%-2% of the total weight of the insecticide mother solution; the phenol antioxidant is selected from any one of 2,6-di-tert-butyl-4-methylphenol, β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate, butylated hydroxyanisole, and β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate.

7. Use of the insecticide mother solution according to any one of claims 1 to 6 in controlling sanitary pests, characterized in that: The sanitary pests are mosquitoes, flies, German cockroaches, American cockroaches, bed bugs, ants, fleas and bees.

8. The use according to claim 7, characterized in that: When the insecticide mother liquid is used to prevent and control sanitary pests, the mother liquid is diluted 1-100 times by weight with odorless kerosene or C8-C18 alkane solvent to prepare mosquito coils, fly coils, electric mosquito coil liquid, electric mosquito coil tablets, aerosols, moth-proof tablets or mosquito nets.

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