A soluble liquid containing broflanpyr and a method for preparing the same

Abstract

The application discloses a kind of bromide chlorfenapyr bisamide-containing soluble liquid and preparation method thereof, belong to the technical field of pesticide.The soluble liquid of the application, with mass percentage content, its composition is as follows: bromide chlorfenapyr bisamide 1%~10%, active component B 1%~10%, amide solvent 25%~45%, alcohol solvent 5%~15%, phosphate emulsifier 5%~15%, stabilizer 0%~1% and the rest water of water content.The raw material of the preparation is safe and environment-friendly, formula process is simple, storage stability is good, active ingredient is in molecular or ionic state after dilution with water, and has the characteristics of good drug efficacy, small dosage etc., can effectively reduce the amount of pesticide, to achieve the purpose of reducing amount and increasing efficiency.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of pesticides, in particular to a soluble concentrate containing broflanpyrduim and a preparation method thereof. BACKGROUND

[0002] Broflanpyrduim belongs to the class of diamide insecticides, and is a GABA-gated chloride channel (also known as ionotropic GABA receptor) allosteric modulator. It mainly acts on a unique binding site of the ion channel, inhibits the transmission of chloride ions into cells, and leads to excessive excitement or spasm of insects, thereby showing rapid insecticidal activity. IRAC classifies this type of compound into group 30. Broflanpyrduim has good insecticidal activity on Lepidoptera and Coleoptera insects, and especially shows high larvicidal activity on Lepidoptera pests.

[0003] Although the mechanism of action of broflanpyrduim is unique, with the extensive application of broflanpyrduim, the problem of resistance is increasingly prominent. At the present stage, one of the most effective methods to solve the above problems is to compound different types of insecticides to delay or reduce the occurrence of pest resistance. In addition, due to the high cost and long cycle of developing new insecticides, compared with this, the development and research of high-efficiency, low-toxicity and low-residue compound insecticide combinations have attracted attention at home and abroad, and various enterprises have increased the development and research efforts.

[0004] At present, there are many complex varieties of broflanvalerate, and the development of dosage forms mainly focuses on water dispersible granules, suspensions, dispersible oil suspensions, wettable powders, emulsifiable concentrates, suspoemulsions, aqueous emulsions or microemulsions. For example, the patent with publication number CN110959615A discloses an insecticidal composition containing broflanvalerate, wherein the weight ratio of broflanvalerate and emamectin benzoate or abamectin is 1:20 20:1, and the dosage form is wettable powder, water dispersible granule and suspension; the patent with publication number CN110199995A discloses a pesticide composition containing broflanvalerate and teflubenzuron, wherein the active ingredients are broflanvalerate and teflubenzuron, and the dosage form is emulsifiable concentrate, suspension, wettable powder, water dispersible granule, aqueous emulsion or microemulsion; the patent with publication number CN110063331A discloses a synergistic pesticide composition of broflanvalerate and neonicotinoid insecticide, wherein the active ingredients are broflanvalerate and neonicotinoid insecticide, and the dosage form is water dispersible granule, wettable powder, suspension, emulsifiable concentrate, microemulsion or aqueous emulsion; the patent with publication number CN109258651A discloses an insecticidal composition containing broflanvalerate and chlorfenapyr, wherein the active ingredients are broflanvalerate and chlorfenapyr, and the dosage form is wettable powder, granule, water dispersible granule, suspension or emulsifiable concentrate; the patent with publication number CN109221127A discloses an insecticidal composition containing broflanvalerate and neonicotinoids, wherein the active ingredient A is broflanvalerate, the active ingredient B is any one of thiamethoxam, imidacloprid, acetamiprid, nitenpyram, dinotefuran and clothianidin, and the dosage form can be wettable powder, water dispersible granule, suspension, suspoemulsion, aqueous emulsion or microemulsion. The patent with publication number CN108077264A discloses an insecticidal composition containing ethyl spinosyn and broflanvalerate, and the dosage form is wettable powder, water dispersible granule, suspension, suspoemulsion, aqueous emulsion or microemulsion. The above patents do not involve soluble concentrates.

[0005] The emulsifiable concentrate type of the above patent needs to use a large amount of aromatic hydrocarbon organic solvents such as toluene and xylene in the processing process. The use of aromatic hydrocarbon solvents increases the residue of toxic substances in crops, and reduces the quality of agricultural products. The microemulsion has certain advantages for liquid technical materials, but for the preparation development of high content or difficultly soluble solid drugs, a large amount of harmful solvents such as N,N-dimethylformamide, N-methyl pyrrolidone, cyclohexanone and methanol still needs to be used, which has high reproductive toxicity to humans and animals and easily pollutes the environment. The emulsion and suspension are environmentally friendly pesticides with water as the base, but the physical stability of the storage is poor and the drug efficacy is relatively poor, which increases the use amount of the effective components of the pesticide, is not conducive to environmental protection, and may enhance the pest resistance. In addition, the particle size of the suspension or emulsion formed after the above patent related dosage forms are diluted with water is relatively large, the spreading and penetration performance is poor, and the drug efficacy is generally not high. It is well known that for the same pesticide technical material, the drug efficacy of the pesticide preparation depends on the type of the dosage form and the dispersion state and size of the pesticide particles. Scientific common sense tells us that when other conditions are the same, the smaller the particle size of the pesticide technical material, the larger the surface area, the wider the contact area with the plant leaves and pests, the more sufficient the drug efficacy, and the corresponding use amount of the pesticide will be reduced. Therefore, it is necessary to develop a new dosage form to improve the drug efficacy of broflanalcymide. SUMMARY

[0006] The present application provides a soluble liquid containing broflanalcymide and a preparation method thereof. The soluble liquid containing broflanalcymide of the present application selects phosphate ester surfactants as emulsifiers, overcomes the defects of traditional dosage forms, and improves the physical and chemical properties and application performance of the preparation. After being diluted with water, the active ingredients are in a molecular or ionic state, which is more conducive to spreading and penetrating on the plant surface, is beneficial to the full play of the drug efficacy, and can reduce the use amount of the pesticide, thereby achieving the purpose of reducing the amount and increasing the efficiency.

[0007] In order to achieve the above-mentioned application purposes, the present application adopts the following technical solutions:

[0008] A soluble liquid containing broflanalcymide, which comprises, by mass percentage, 1-10% of broflanalcymide, 1-10% of active component B, 25-45% of amide solvent, 5-15% of alcohol solvent, 5-15% of phosphate emulsifier, 0-1% of stabilizer, and the balance of water.

[0009] In the above soluble liquid, the active component B is selected from at least one of emamectin benzoate, abamectin, lambda-cyhalothrin, thiamethoxam, acetamiprid, hydroprene, tolfenpyrad, and chlorfenapyr.

[0010] The amide solvent in the above-mentioned dissoluble solution is selected from at least one of N,N-dimethyl octanedecanoic amide and N,N-dimethyl decanoic amide.

[0011] The amide solvent in the above-mentioned dissoluble solution is selected from at least one of N,N-dimethyl octanedecanoic amide and N,N-dimethyl decanoic amide.

[0012] 1) N,N-dimethyl octanedecanoic amide and N,N-dimethyl decanoic amide;

[0013] 2) N,N-dimethyl lactamide and N,N-dimethyl decanoic amide;

[0014] 3) N,N-dimethyl lactamide and N,N-dimethyl octanedecanoic amide.

[0015] The amide solvent in the above-mentioned dissoluble solution is selected from at least one of N,N-dimethyl octanedecanoic amide and N,N-dimethyl decanoic amide.

[0016] 1) N,N-dimethyl octanedecanoic amide and N,N-dimethyl decanoic amide;

[0017] 2) N,N-dimethyl lactamide and N,N-dimethyl decanoic amide;

[0018] 3) N,N-dimethyl lactamide and N,N-dimethyl octanedecanoic amide.

[0019] The alcohol solvent in the above-mentioned dissoluble solution is selected from at least one of tetrahydrofurfuryl alcohol, diacetone alcohol, 3-methoxy-3-methyl-1-butanol and isohexide.

[0020] The phosphate emulsifier in the above-mentioned dissoluble solution is selected from at least one of tristyrylphenol ethoxylate phosphate, fatty alcohol ethoxylate phosphate, polyethylene glycol 400 monooleate phosphate, oleyl ethoxylate phosphate and alkoxylated phosphate.

[0021] The stabilizer in the above-mentioned dissoluble solution is selected from at least one of octanedecanoic acid, 2,6-di-tert-butyl-p-cresol (BHT) and 2-hydroxy-4-n-octyloxybenzophenone (UV-531).

[0022] Further, the present application provides a preparation method of the above-mentioned dissoluble solution, comprising the following steps:

[0023] (1) Mix the amide solvent, alcohol solvent, chlorfenapyr, active component B and stabilizer, and stir until transparent and uniform;

[0024] (2) Add the phosphate ester emulsifier to the solution in (1), and stir until transparent and uniform;

[0025] (3) Add water to the solution in (2), and stir until transparent and uniform.

[0026] In the above preparation method, the stirring time in step (1) is 5-15 min;

[0027] In steps (2) and (3), the stirring time is 5-10 min.

[0028] Compared with the prior art, the present application has the following beneficial effects:

[0029] (1) The present application successfully disperses and dissolves the solid active ingredient, which is originally insoluble in water, in water to form a true solution state, thereby improving the drug efficacy and maintaining the normal physical and chemical stability of the preparation;

[0030] (2) The phosphate ester surfactant is selected as the emulsifier in the formula, which has both wetting and synergistic functions, so that the diluted pesticide solution is more easily spread and penetrated on the target, thereby reducing the pesticide dosage and meeting the national industrial policy. BRIEF DESCRIPTION OF DRAWINGS

[0031] Figure 1 It is the appearance of 5% chlorfenapyr + 4% emamectin benzoate diluted 20 times in different dosage forms. Note: left 1 is SC, left 2 is EC, left 3 is ME, and left 4 is SL.

[0032] Figure 2 It is the wetting and spreading of 5% chlorfenapyr + 4% emamectin benzoate diluted 1500 times on a canvas sheet. Note: the sample amount is 0.05 mL, left 1 is SC, left 2 is EC, left 3 is ME, and left 4 is SL. DETAILED DESCRIPTION

[0033] The present application will be further described in detail below in conjunction with specific embodiments, and the examples given are only for illustrating the present application, rather than limiting the scope of the present application.

[0034] In the following examples, the experimental methods are conventional methods, unless otherwise specified.

[0035] In the quantitative test in the following examples, three repeated experiments are set up, and the average value is taken.

[0036] In the following examples, the materials and reagents used, unless otherwise specified, can be obtained from commercial channels.

[0037] The percentage in the following examples refers to mass percentage unless otherwise specified.

[0038] The mass technical index testing method of the soluble liquid containing bromofluorfenisulam in the following examples is as follows:

[0039] 1. Active ingredient mass fraction: bromofluorfenisulam is determined by high performance liquid chromatography; active ingredient B is determined by high performance liquid chromatography;

[0040] 2. pH value range: determined according to the method of CIPAC MT 75.3;

[0041] 3. Solution stability: determined according to the method of CIPAC MT 41.1; standard hard water is diluted by 20 times, and is placed at 20℃ for 18h.

[0042] 4. Persistent foaming property: determined according to CIPAC MT 47.3;

[0043] 5. Thermal storage stability: determined according to CIPAC MT 46.4, and is placed at 54℃ for 14 days;

[0044] 6. Low temperature stability: determined according to CIPAC MT 39.3, and is placed at 0℃ for 7 days.

[0045] Example 1, 5% bromofluorfenisulam + 4% emamectin benzoate soluble liquid

[0046] 1. The content of each component is as follows:

[0047] Bromofluorfenisulam (active ingredient, Mitsui Chemicals, Inc.) 5%

[0048] Emamectin benzoate (active ingredient, Shandong Jingbo Agricultural Chemical Technology Co., Ltd.) 4%

[0049] N,N-dimethyl lactamide AGNIQUE AMD 3L (amide solvent, BASF) 25%

[0050] Tetrahydrofurfuryl alcohol (alcohol solvent, Luxi Chemical Group Co., Ltd.) 10%

[0051] N,N-dimethyl octanamide (amide solvent, Nantong Zhukai Chemical Co., Ltd.) 15%

[0052] Tristyrylphenol ethoxylate phosphoric ester Dispersogen LFH (phosphoric ester emulsifier, Clariant) 15%

[0053] BHT (stabilizer, Jiangsu Maidaxin Material Co., Ltd.) 1%

[0054] Water make up 100%

[0055] 2. The preparation process according to the above formula is as follows:

[0056] (1) Prepare various raw materials according to the mass ratio of the formula;

[0057] (2) Add AGNIQUE AMD 3L, tetrahydrofurfuryl alcohol and N,N-dimethyl octyl decanamide measured into the kettle, then add bromofenoximate, emamectin benzoate and BHT, mix thoroughly under stirring for about 10 min until transparent and uniform;

[0058] (3) Add Dispersogen LFH into the solution of (2) above, stir for 10 min until transparent and uniform;

[0059] (4) Add the remaining water into the solution of (3) above, stir for 5 min until transparent and uniform, stand, filter, and obtain the product.

[0060] The quality technical indicators of 9% bromofenoximate·emamectin benzoate soluble concentrate prepared in this example are shown in Table 1.

[0061] Table 1 Quality technical indicators of 9% bromofenoximate·emamectin benzoate soluble concentrate

[0062]

[0063] The appearance of 5% bromofenoximate + 4% emamectin benzoate different dosage forms diluted 20 times is shown in Figure 1 , and the left 4SL is the sample prepared in this example.

[0064] The wetting and spreading of 5% bromofenoximate + 4% emamectin benzoate different dosage forms diluted 1500 times on canvas is shown in Figure 2 , and the left 4SL is the sample prepared in this example.

[0065] Figure 1 and Figure 2 , the preparation method of the left 1 suspension concentrate (SC) is as follows:

[0066] Take bromofenoxy 5%, emamectin benzoate 4%, dispersant Supragil MNS / 90 (alkyl naphthalene formaldehyde condensate sulfonate, Solvay) 3%, wetting agent Tergitol W-600 (isomeric alcohol polyoxyethylene ether, DOW) 1%, 1,2-propanediol (antifreeze, Shandong Guohua Chemical Co., Ltd.) 5%, stabilizer BHT (Jiangsu Maidaxin Material Co., Ltd.) 0.5%, xanthan gum (thickening agent, Hebei Pengyu Biological Technology Co., Ltd.) 0.1%, kathon (preservative, Beijing Guangyuan Yinan Chemical Co., Ltd.) 0.1%, SAG 1522 (silicone defoamer, Maitian High-tech Material Group) 0.5%, and deionized water (self-made) to make up 100% by mass percentage. The above raw materials are mixed and sand ground to a particle size of less than 5 μm, and then filtered to obtain 5% bromofenoxy + 4% emamectin benzoate suspension concentrate.

[0067] The preparation method of left 2 emulsifiable concentrate (EC) is as follows:

[0068] Take bromofenoxy 5%, emamectin benzoate 4%, emulsifier EL-40 (castor oil polyoxyethylene ether, Nantong Deyi Chemical Co., Ltd.) 7%, emulsifier 505# (calcium dodecylbenzenesulfonate, Nantong Deyi Chemical Co., Ltd.) 3%, solvent N,N-dimethylacetamide (Nantong Zhukai Chemical Co., Ltd.) 15%, stabilizer BHT (Jiangsu Maidaxin Material Co., Ltd.) 0.5%, and solvent oil S-150 (Jiangsu Hualun Chemical Co., Ltd.) to make up 100% by mass percentage. The above raw materials are mixed and stirred to be transparent, and then filtered to obtain 5% bromofenoxy + 4% emamectin benzoate emulsifiable concentrate.

[0069] The preparation method of left 3 microemulsion (ME) is as follows:

[0070] Take bromofenoxy 5%, emamectin benzoate 4%, emulsifier 602 (triphenyl ethenyl phenol polyoxyethylene ether, Nantong Deyi Chemical Co., Ltd.) 20%, solvent dimethyl sulfoxide (Hubei Xingfa Chemical Group Co., Ltd.) 20%, solvent cyclohexanone (Liaoyang Petrochemical Fiber Company of China Petroleum) 30%, stabilizer BHT (Jiangsu Maidaxin Material Co., Ltd.) 0.5%, and water (self-made) to make up 100% by mass percentage. The above bromofenoxy technical material and emamectin benzoate technical material are dissolved in an organic solvent, and then the emulsifier is added and stirred to be transparent. Finally, water is added and stirred to be transparent, and then filtered to obtain 5% bromofenoxy + 4% emamectin benzoate microemulsion.

[0071] At the same mass, the area of the pesticide solution contacting with the pests will be larger. It can more widely cover the plant leaf surface or the pest body surface, and more easily enter the pest body to play a toxic effect. Figure 1As shown in the table, the suspension concentrate (SC) is a suspension in dilute state with particle size between 1-10 microns; the emulsifiable concentrate (EC) is an emulsion in dilute state with particle size between 1-5 microns; the microemulsion (ME) is a translucent emulsion in dilute state with particle size between 0.01-0.1 microns; the soluble concentrate (SL) is a true solution in dilute state with particle size generally less than 1 nanometer. As can be seen from the particle size, the active ingredient in the soluble concentrate (SL) is generally uniformly dispersed in the solvent in molecular or ionic state with extremely small particle size, which can efficiently contact and act on the target, and thus the drug efficacy is excellent. The microemulsion (ME) also has relatively small droplet size, and has certain advantages in dispersion and penetration, and the drug efficacy is second. The emulsifiable concentrate (EC) has relatively large particle size, and is slightly inferior to the former two in terms of dispersion uniformity and contact efficiency with the target. The suspension concentrate (SC) is a dispersion system formed by solid particles dispersed in liquid, and has relatively large particle size, and is relatively low in deposition, adhesion and penetration into the target organism, and thus the drug efficacy is relatively the worst.

[0072] 3. Comparison of biological efficacy

[0073] In order to determine the difference in control effect of 9% chlorantraniliprole·emamectin benzoate soluble concentrate and 9% chlorantraniliprole·emamectin benzoate suspension concentrate and microemulsion on cabbage diamondback moth, a field plot efficacy test was conducted.

[0074] The experimental method is as follows:

[0075] In this test, the test agent, control agent and blank control plot treatment were arranged randomly according to GB / T 17980.13-2000 Pesticide Field Efficacy Test Guidelines (I) Insecticides for Controlling Lepidoptera Larvae in Cruciferous Vegetables, and the plot area was 50 m 2 . A 3WBD-20 type backpack electric sprayer was used for uniform spraying, and each plot was sprayed with 30 kg of water per 667 m 2 . No other agents were used during the test, and each treatment was repeated 4 times.

[0076] Investigation and statistical method: 10 plants were selected for investigation at 5 points on the diagonal line of each plot before treatment, and the number of diamondback moth larvae was recorded. The number of live diamondback moth larvae was investigated on the 3rd, 7th and 14th day after treatment. The diamondback moth larva reduction rate and control effect were calculated according to the following formula:

[0077] Larva reduction rate (%) = {(number of larvae before treatment-number of larvae after treatment) / number of larvae before treatment} x 100;

[0078] Control effect (%) = {(larva reduction rate in agent treatment plot-larva reduction rate in blank control plot) / (100-larva reduction rate in blank control plot)} x 100

[0079] Safety investigation and effects on other organisms: The effects of each treatment on the growth of cabbage and on other organisms were observed on the first day after each spray and on several days after spraying.

[0080] The preparation method of 9% flubendiamide·emamectin benzoate suspension used is as follows:

[0081] Take flubendiamide 5%, emamectin benzoate 4%, dispersant Soprophor SC (phosphoric acid triethanolamine salt, Solvay) 3%, wetting agent YUS-EP60P (sulfosuccinic acid sodium, TAKEMOTO) 2%, 1,2-propanediol (antifreeze, Shandong Guohua Chemical Co., Ltd.) 5%, xanthan gum (thickening agent, Hebei Pengyu Biological Technology Co., Ltd.) 0.1%, kathon (preservative, Beijing Guangyuyinong Chemical Co., Ltd.) 0.1%, SAG 1522 (silicone antifoaming agent, Momentive High-tech Materials Group) 0.5%, BHT (stabilizer, Jiangsu Maidan New Material Co., Ltd.) 0.5%, and deionized water (self-made) to make up 100% by mass fraction. The above raw materials are mixed and sand-milled to a particle size of less than 5 μm, and then filtered to obtain 9% flubendiamide·emamectin benzoate suspension.

[0082] The preparation method of 9% flubendiamide·emamectin benzoate suspension used is as follows:

[0083] Take flubendiamide 5%, emamectin benzoate 4%, N,N-dimethylformamide (solvent, Changzhou Juyuan Chemical Co., Ltd.) 15%, cyclohexanone (solvent, Hunan Dongwei Chemical New Material Co., Ltd.) 15%, methanol (solvent, Qilu Petrochemical Company) 5%, 602# (emulsifier, Nanjing Taihua Chemical Co., Ltd.) 20%, BHT (stabilizer, Jiangsu Maidan New Material Co., Ltd.) 0.5%, and deionized water (self-made) to make up 100% by mass fraction. Flubendiamide, emamectin benzoate and stabilizer are dissolved in organic solvent, the emulsifier is added and stirred uniformly, and then water is added and stirred uniformly to obtain 9% flubendiamide·emamectin benzoate microemulsion.

[0084] Medicament 1: 9% flubendiamide·emamectin benzoate soluble liquid diluted 1500 times with water;

[0085] Medicament 2: 9% flubendiamide·emamectin benzoate soluble liquid diluted 2000 times with water;

[0086] Medicament 3: 9% flubendiamide·emamectin benzoate suspension diluted 1500 times with water;

[0087] Medicament 4: 9% flubendiamide·emamectin benzoate microemulsion diluted 1500 times with water;

[0088] Table 2 Data of flubendiamide·emamectin benzoate mixture efficacy test

[0089]

[0090] As shown in Table 2, at the same dilution ratio, the control effect of the chlorfenapyr·emamectin soluble solution on cabbage diamondback moth is obviously higher than that of other formulations with the same content, and it has obvious advantages in reducing amount and increasing efficiency. No phytotoxicity was found during application, and it is safe to cabbage growth.

[0091] Example 2, 8% chlorfenapyr + 2% abamectin soluble solution

[0092] 1. The content of each component is as follows:

[0093]

[0094] 2. The preparation process according to the above formula is as follows:

[0095] (1) Prepare various raw materials according to the weight ratio of the formula;

[0096] (2) Add the weighed AGNIQUE AMD 3L, 3-methoxy-3-methyl-1-butanol and N,N-dimethyl decanamide into the kettle, and then add chlorfenapyr, abamectin and octyl decanoate. Stir well and mix for about 10 min until transparent and uniform;

[0097] (3) Add phosphonate emulsifier MOA-9P to the solution in (2) above, and stir for 5 min until transparent and uniform;

[0098] (4) Add the remaining water to the solution in (3) above, and stir for 5 min until transparent and uniform. Let stand, filter, and obtain the product.

[0099] The quality technical indicators of the 10% chlorfenapyr·abamectin soluble solution prepared in this example are shown in Table 3.

[0100] Table 3 Quality technical indicators of 10% chlorfenapyr·abamectin soluble solution

[0101]

[0102] After the sample in this example is diluted 20 times with standard hard water, it presents a true solution state, and its appearance is similar to that shown in Fig. 4A, which is more easily wetted, spread and absorbed on the target surface, thereby improving the efficacy. Figure 1

[0103] 3. Biological efficacy comparison

[0104] ​In order to clarify the difference of control effect of 10% broflanilide·abamectin soluble concentrate and 10% broflanilide·abamectin suspension concentrate and microemulsion on Chilo irridans, field plot efficacy test was carried out.

[0105] The experimental method is as follows:

[0106] In this test, the test agent, control agent and blank control plot treatment were arranged randomly according to GB / T 17980.1-2000 Pesticide Field Efficacy Test Guidelines (I) Insecticide Control of Lepidoptera Borer Pests in Rice. The plot area was 50 m 2 , and 3WBD-20 type backpack electric sprayer was used for uniform spraying. Each plot was sprayed with 30 kg of water per 667 m 2 according to the amount of each agent treatment. No other agent was used during the test, and each treatment was repeated 4 times.

[0107] Investigation and statistical method: parallel jumping sampling, 50 clusters of rice were investigated in each plot, and the rate of dead heart or the number of white spikes was counted. The rate of dead heart and mortality were investigated on the 5th, 14th and 27th day after treatment, respectively. The rate of dead heart (white spike) and control effect were calculated according to the following formula:

[0108] Rate of dead heart (white spike) (%) = {(number of investigated dead heart white spike) / (total number of investigated spike)} x 100;

[0109] Control effect (%) = {(rate of dead heart (white spike) of blank control after treatment - rate of dead heart (white spike) of agent treatment area after treatment) / rate of dead heart (white spike) of blank control after treatment} x 100

[0110] Safety investigation and effect on other organisms: the effect of each agent treatment on rice growth and other organisms was observed on the first day after each spraying and several days after treatment.

[0111] The preparation method of 10% broflanilide·abamectin suspension concentrate used is as follows:

[0112] Take bromofene 8%, avermectin 2%, dispersant Morwet D-425 (alkyl naphthalene sulfonate, Nouryon) 3%, wetting agent YUS-EP60P (sulfonated succinic acid sodium, TAKEMOTO) 2%, 1,2-propanediol (antifreeze, Shandong Guohua Chemical Co., Ltd.) 5%, xanthan gum (thickening agent, Hebei Pengyu Biological Technology Co., Ltd.) 0.1%, Kathon (preservative, Beijing Guangyuyinong Chemical Co., Ltd.) 0.1%, SAG 1522 (organic silicon defoaming agent, Mayite High-tech Materials Group) 0.5%, BHT (stabilizer, Jiangsu Maidan New Material Co., Ltd.) 0.5%, and deionized water (self-made) to make up 100% by mass fraction. The above raw materials are mixed and sand ground to a particle size of less than 5 μm, and then filtered to obtain 10% bromofene·avermectin suspension concentrate.

[0113] The preparation method of 10% bromofene·avermectin microemulsion is as follows:

[0114] Take bromofene 8%, avermectin 2%, N,N-dimethylformamide (solvent, Changzhou Polyfeng Chemical Co., Ltd.) 20%, cyclohexanone (solvent, Hunan Dongwei Chemical New Material Co., Ltd.) 17%, methanol (solvent, Qilu Petrochemical Company) 5%, 602# (emulsifier, Nanjing Taihua Chemical Co., Ltd.) 20%, BHT (stabilizer, Jiangsu Maidan New Material Co., Ltd.) 0.5%, and deionized water (self-made) to make up 100% by mass fraction. Dissolve bromofene, avermectin and stabilizer in organic solvent, add emulsifier and stir uniformly, and finally add water and stir uniformly to obtain 10% bromofene·avermectin microemulsion.

[0115] Medicine 1: 10% bromofene·avermectin soluble concentrate diluted 1500 times with water;

[0116] Medicine 2: 10% bromofene·avermectin soluble concentrate diluted 2000 times with water;

[0117] Medicine 3: 10% bromofene·avermectin suspension concentrate diluted 1500 times with water;

[0118] Medicine 4: 10% bromofene·avermectin microemulsion diluted 1500 times with water;

[0119] Table 4: Data of bromofene·avermectin mixture efficacy test

[0120]

[0121] From Table 4, it can be seen that at the same dilution ratio, the control effect of the chlorfenapyr·abamectin soluble solution on Chilo irridans is obviously higher than that of other formulations with the same content, and it has obvious advantages in reducing amount and increasing efficiency. No phytotoxicity was found during application, and it is safe for rice growth.

[0122] Example 3, 6% chlorfenapyr + 4% lambda-cyhalothrin soluble solution

[0123] 1. The content of each component is as follows:

[0124]

[0125] 2. The preparation process according to the above formula is as follows:

[0126] (1) Prepare various raw materials according to the weight ratio of the formula;

[0127] (2) Add the measured N,N-dimethylformamide, tetrahydrofurfuryl alcohol and N,N-dimethyl octyldecylamide into the kettle, then add chlorfenapyr and lambda-cyhalothrin, and mix thoroughly for about 10 min until transparent and uniform;

[0128] (3) Add the phosphonate emulsifier polyethylene glycol 400 monooctadecyl phosphate to the solution in (2) above, and stir for 10 min until transparent and uniform;

[0129] (4) Add the remaining water to the solution in (3) above, stir for 5 min until transparent and uniform, stand, and filter to obtain the product.

[0130] The quality technical indicators of the 10% chlorfenapyr·lambda-cyhalothrin soluble solution prepared in this example are shown in Table 5.

[0131] Table 5 Quality technical indicators of 10% chlorfenapyr·lambda-cyhalothrin soluble solution

[0132]

[0133] After the sample in this example is diluted 20 times with standard hard water, it presents a true solution state, and its appearance is similar to that shown in Fig. 4, which is more easily wetted, spread and absorbed on the target surface, thereby improving the efficacy. Figure 1

[0134] 3. Biological efficacy comparison

[0135] In order to clarify the difference in control effect of 10% chlorfenapyr·lambda-cyhalothrin soluble solution, 10% chlorfenapyr·lambda-cyhalothrin suspension concentrate and 10% chlorfenapyr·lambda-cyhalothrin microemulsion on Spodoptera exigua, a field plot efficacy test was conducted.

[0136] The experimental method is as follows: ​

[0137] The test refers to "GB / T 23392.4-2009 Technical Specifications for Forecasting Diseases and Pests of Cruciferae Part 4: Spodoptera exigua", and the test agent, control agent and blank control plot treatment are randomly arranged. The plot area is 50m 2 , and 3WBD-20 type backpack electric sprayer is used for uniform spraying. Each plot is uniformly sprayed with 30kg of water per 667m 2 , and no other agent is used during the test. Each treatment is repeated 4 times.

[0138] Investigation and statistical method: 5 larger areas are selected, 2 plots are investigated in each area, and the investigation is carried out at the peak of egg. Before and after spraying, 5-point sampling method is used, 2 plants are determined at each point, the number of live larvae on the whole leaf of the plant is observed, and the data is statistically processed and analyzed by using DPS data processing system, and variance analysis is carried out by using Duncan new multiple range method. The larva reduction rate of spodoptera exigua and the control effect are calculated according to the following formula:

[0139] Larva reduction rate (%) = {(number of larvae before spraying-number of larvae after spraying) / number of larvae before spraying} x 100;

[0140] Control effect (%) = {(larva reduction rate of agent treatment area-larva reduction rate of blank control area) / (100-larva reduction rate of blank control area)} x 100

[0141] Safety investigation and influence on other organisms: the influence of each treatment of the agent on the growth of lettuce and on other organisms is observed on the first day after spraying and on several days after spraying.

[0142] The preparation method of 10% broflanpyrimestrofloclorfenapate suspension concentrate is as follows:

[0143] Take 6% broflanpyrimestro, 4% high-efficiency chloroflocorfenapate, 3% dispersant ATLOX4913 (polyacrylate, CRODA), 2% wetting agent Genapol X 080 (isomeric alcohol polyoxyethylene ether, Clariant), 5% 1,2-propanediol (antifreeze, Shandong Guohua Chemical Co., Ltd.), 0.1% xanthan gum (thickening agent, Hebei Pengyu Biological Technology Co., Ltd.), 0.1% kathon (preservative, Beijing Guangyuan Yinan Chemical Co., Ltd.), 0.5% SAG 1522 (organic silicon defoaming agent, Maitu High-tech Material Group), and deionized water (self-made) to make up 100% by mass fraction. The above raw materials are mixed and sand milled to a particle size of less than 5μm, and then filtered to obtain 10% broflanpyrimestrofloclorfenapate suspension concentrate.

[0144] The preparation method of 10% broflanpyrimestrofloclorfenapate microemulsion is as follows:

[0145] Take bromofenprox 6%, lambda cyhalothrin 4%, N,N-dimethylformamide (solvent, Changzhou Jufeng Chemical Co., Ltd.) 15%, cyclohexanone (solvent, Hunan Dongwei New Material Co., Ltd.) 17%, methanol (solvent, Qilu Petrochemical Company) 5%, 602# (emulsifier, Nanjing Taihua Chemical Co., Ltd.) 20%, and deionized water (self-made) to make up 100% by mass fraction. Dissolve bromofenprox and lambda cyhalothrin in the organic solvent, add the emulsifier and stir uniformly, and finally add water and stir uniformly to obtain 10% bromofenprox·lambda cyhalothrin microemulsion.

[0146] Medicine 1: 10% bromofenprox·lambda cyhalothrin soluble concentrate diluted 1500 times with water;

[0147] Medicine 2: 10% bromofenprox·lambda cyhalothrin soluble concentrate diluted 2000 times with water;

[0148] Medicine 3: 10% bromofenprox·lambda cyhalothrin suspension diluted 1500 times with water;

[0149] Medicine 4: 10% bromofenprox·lambda cyhalothrin microemulsion diluted 1500 times with water;

[0150] Table 6: Data of bromofenprox·lambda cyhalothrin mixture efficacy test

[0151]

[0152] As can be seen from Table 6, under the same dilution multiple, the control effect of bromofenprox·lambda cyhalothrin soluble concentrate on beet armyworm is obviously higher than that of other formulations with the same content, and it has obvious advantages in reducing amount and increasing efficiency. No phytotoxicity was found during application, and it is safe to lettuce growth.

[0153] Example 4: 5% bromofenprox + 5% thiamethoxam soluble concentrate

[0154] 1. The content of each component is as follows:

[0155]

[0156] 2. The preparation process according to the above formula is as follows:

[0157] (1) Prepare various raw materials according to the weight ratio of the formula;

[0158] (2) Add the weighed N,N-dimethylformamide, diacetone alcohol and N,N-dimethyl octylamide into the kettle, then add bromofenprox and thiamethoxam, and stir thoroughly for about 10 min until transparent and uniform;

[0159] (3) Add the phosphate emulsifier O-5P to the solution in (2) above and stir for 10 minutes until it is transparent and homogeneous;

[0160] (4) Add the remaining water to the solution in (3) above, stir for 5 minutes until it is transparent and uniform, let it stand, filter, and you will get the solution.

[0161] The quality technical indicators of the 10% bromoxynil diamide·thiamethoxam soluble concentrate prepared in this embodiment are shown in Table 7.

[0162] Table 7 Quality Technical Specifications of 10% Brombutamide·Thiamethoxam Soluble Solution

[0163]

[0164] The sample in this embodiment, after being diluted 20 times with standard hard water, exhibited a true solution state, and its appearance was similar to that of the attached sample. Figure 1 Similar to the one shown in left 4, it is easier to wet, spread, and penetrate the target surface, thus improving efficacy.

[0165] 3. Comparison of biological efficacy

[0166] To clarify the differences in the control efficacy of 10% bromfenoxam·thiamethoxam soluble concentrate, 10% bromfenoxam·thiamethoxam suspension concentrate, and microemulsion against western flower thrips on peppers, a field plot efficacy test was conducted.

[0167] The experimental method is as follows:

[0168] This experiment followed the guidelines in "NY / T 1464.6-2007 Field Efficacy Test Guidelines for Pesticides Part 6: Insecticides for the Control of Thrips in Vegetables". The experimental pesticide, control pesticide, and blank control were randomly assigned to plots of 40 m². 2 Use a 3WBD-20 backpack electric sprayer to spray evenly, applying the pesticide at a rate of 1:1 per 667m². 2 30 kg of water was used to spray evenly on each plot. No other agents were used during the experiment, and each treatment was repeated 4 times.

[0169] Survey and statistical methods: For each plot, 30 leaves were selected from the middle and upper parts of the pepper plant to investigate the number of live nymphs. The initial insect population (number of live nymphs before application) was investigated, and the number of residual insects (number of live nymphs after application) was investigated on days 1, 3, 7, and 10 after application. The control effect was calculated using the following formula, and statistical analysis was performed using the DMRT method.

[0170] Control effect (%) = {1 - (number of live insects in the blank control area before application x number of live insects in the pesticide treatment area after application) / number of live insects in the blank control area after application x number of live insects in the pesticide treatment area before application) x 100

[0171] Safety investigation and impact on other organisms: On the first day after each spraying and on several days after spraying, the impact of each treatment of the pesticide on the growth of peppers and on other organisms was observed.

[0172] The preparation method of the 10% broflanpyrium·thiamethoxam suspension used is as follows:

[0173] In mass percentage, 5% of broflanpyrime, 5% of thiamethoxam, 3% of Suparex K powder (naphthalene formaldehyde condensate sulfonate dispersant, Switzerland OnGuard Chemical Co.), 2% of Tergitol W-600 (isomeric alcohol polyoxyethylene ether, DOW), 5% of 1,2-propanediol (antifreeze, Shandong Guohua Chemical Co., Ltd.), 0.1% of xanthan gum (thickening agent, Hebei Pengyu Biological Technology Co., Ltd.), 0.1% of Kathon (preservative, Beijing Guangyuan Yinan Chemical Co., Ltd.), 0.5% of SAG 1522 (organic silicon defoaming agent, Mayite High-tech Materials Group), and deionized water (self-made) are weighed to make up 100%. The above raw materials are mixed and sand-milled to a particle size of less than 5 μm, and then filtered to obtain 10% broflanpyrime·thiamethoxam suspension.

[0174] The preparation method of 10% broflanpyrime·thiamethoxam microemulsion is as follows:

[0175] In mass percentage, 5% of broflanpyrime, 5% of thiamethoxam, 15% of N-methyl pyrrolidone (solvent, Xingmai Chemical Co., Ltd.), 15% of cyclohexanone (solvent, Hunan Dongwei Chemical New Material Co., Ltd.), 5% of methanol (solvent, Qilu Petrochemical Co.), 20% of 602# (emulsifier, Nanjing Taihua Chemical Co., Ltd.), and deionized water (self-made) are weighed to make up 100%. Broflanpyrime and thiamethoxam are dissolved in organic solvents, the emulsifier is added and stirred uniformly, and then water is added and stirred uniformly to obtain 10% broflanpyrime·thiamethoxam microemulsion.

[0176] Pesticide 1: 10% broflanpyrime·thiamethoxam soluble concentrate diluted 1000 times with water;

[0177] Pesticide 2: 10% broflanpyrime·thiamethoxam soluble concentrate diluted 1500 times with water;

[0178] Pesticide 3: 10% broflanpyrime·thiamethoxam suspension diluted 1000 times with water;

[0179] Formulation 4: 10% broflanilide + thiamethoxam ME diluted 1000 times with water;

[0180] Table 8: Data of efficacy test of broflanilide + thiamethoxam mixture

[0181]

[0182] As shown in Table 8, at the same dilution ratio, the control effect of the broflanilide + thiamethoxam soluble solution on the pepper thrips is obviously higher than that of other formulations with the same content, and it has obvious advantages in reducing the amount of increase in efficiency. No phytotoxicity was found during the application, and it was safe for the growth of peppers.

[0183] Example 5, 2% broflanilide + 8% acetamiprid soluble solution

[0184] 1. The content of each component is as follows:

[0185]

[0186] 2. The preparation process according to the above formulation is as follows:

[0187] (1) Prepare various raw materials according to the weight ratio of the formulation;

[0188] (2) Add the weighed AGNIQUE AMD 3L, isohexyl alcohol and N,N-dimethyl decanamide into the kettle, then add broflanilide and acetamiprid, and mix thoroughly for about 10 min until transparent and uniform;

[0189] (3) Add phosphonate emulsifier E1310P to the solution in (2) above, and stir for 10 min until transparent and uniform;

[0190] (3) Add the remaining water to the solution in (3) above, and stir for 5 min until transparent and uniform, then stand, filter, and obtain the product.

[0191] The quality technical indicators of the 10% broflanilide + acetamiprid soluble solution prepared in this example are shown in Table 9.

[0192] Table 9: Quality technical indicators of 10% broflanilide + acetamiprid soluble solution

[0193]

[0194] After the sample of this example is diluted 20 times with standard hard water, it presents a true solution state, and its appearance is similar to that shown in Fig. 4, which is more easily wetted, spread and absorbed on the target surface, thereby improving the efficacy. Figure 1

[0195] 3. Biological efficacy comparison

[0196] ​To clarify the differences in the control efficacy of 10% bromutrin dimethyl sulfadiazine·acetamiprid soluble concentrate, 10% bromutrin dimethyl sulfadiazine·acetamiprid suspension concentrate, and microemulsion against flea beetle in cabbage, a field plot efficacy trial was conducted.

[0197] The experimental method is as follows:

[0198] This experiment followed the guidelines in GB / T 17980.18-2000 "Field Efficacy Testing Criteria for Pesticides (I) - Control of Yellow-striped Flea Beetles in Cruciferous Vegetables". The experimental pesticide, control pesticide, and blank control were randomly assigned to plots of 40 m². 2 Use a 3WBD-20 backpack electric sprayer to spray evenly, applying the pesticide at a rate of 1:1 per 667m². 2 30 kg of water was used to spray evenly on each plot. No other agents were used during the experiment, and each treatment was repeated 4 times.

[0199] Survey and statistical methods:

[0200] Adult insect survey: At least 20 cabbage plants were randomly selected from each plot to investigate the number of live adults.

[0201] Larval survey: During the last survey after the pesticide application, at least three fixed points should be set up in each plot, and two plants should be surveyed at each point. The soil around the plant roots should be dug up and rinsed with clean water to count the number of live larvae in the soil.

[0202] A baseline survey was conducted before application. The second survey was conducted 2 days after application. The third survey was conducted 7 days after application.

[0203] Insect population reduction rate (%) = {(number of insects before application - number of insects after application) / number of insects before application} × 100;

[0204] Adult insect control efficacy (%) = {(insect population reduction rate in the pesticide-treated area - insect population reduction rate in the blank control area) / (100 - insect population reduction rate in the blank control area)} × 100;

[0205] Larval control efficacy (%) = {(Number of larvae in the blank control area - Number of larvae in the pesticide-treated area) / Number of larvae in the blank control area} × 100

[0206] Safety investigation and effects on other organisms: The effects of each pesticide treatment on cabbage growth and other organisms were observed on the first day after each spraying and several days after the spraying.

[0207] The preparation method of the 10% bromfenac-methyl·acetamiprid suspension used is as follows:

[0208] Weigh out the following ingredients by weight percentage: 2% brofenoxam, 8% acetamiprid, 3% dispersant Dispersogen LFS (alkylphenol polyoxyethylene phosphate, Solvay), 2% wetting agent TERGITOL W-600 (isomeric alcohol polyoxyethylene ether, DOW), 5% 1,2-propanediol (antifreeze, Shandong Guohua Chemical Co., Ltd.), 0.1% xanthan gum (thickener, Hebei Pengyu Biotechnology Co., Ltd.), 0.1% Kathon (preservative, Beijing Guangyuan Yinong Chemical Co., Ltd.), 0.5% SAG 1522 (silicone defoamer, Momentive Advanced Materials Group), and make up to 100% with deionized water (self-made). Mix the above ingredients, mill them using a sand mill until the particle size is less than 5 μm, and filter to obtain a 10% brofenoxam·acetamiprid suspension.

[0209] The preparation method of 10% bromfenoxam·acetamiprid microemulsion is as follows:

[0210] Weigh out the following ingredients by mass percentage: 2% brofenoxam, 8% acetamiprid, 12% N-methylpyrrolidone (solvent, Xinmaiqi Materials Co., Ltd.), 10% cyclohexanone (solvent, Hunan Dongwei Chemical New Materials Co., Ltd.), 5% methanol (solvent, Qilu Petrochemical Co., Ltd.), 20% 602# (emulsifier, Nanjing Taihua Chemical Co., Ltd.), and make up to 100% with deionized water (self-made). Dissolve brofenoxam and acetamiprid in the organic solvent, add the emulsifier and stir until homogeneous, and finally add water and stir until homogeneous to obtain a 10% brofenoxam·acetamiprid microemulsion.

[0211] Agent 1: 10% bromofenopram·acetamiprid soluble solution diluted 1500 times with water;

[0212] Agent 2: 10% bromofenopram·acetamiprid soluble solution diluted 2000 times with water;

[0213] Agent 3: 10% bromofenopram·acetamiprid suspension diluted 1500 times with water;

[0214] Agent 4: 10% bromofenopram·acetamiprid microemulsion diluted 1500 times with water;

[0215] Table 10. Efficacy test data of bromofenopram·acetamiprid mixture

[0216]

[0217] As shown in Table 10, at the same dilution ratio, the bromufenprox·acetamiprid soluble concentrate is significantly more effective against flea beetles on cabbage than other formulations at the same concentration, demonstrating a clear advantage in reducing dosage while increasing efficacy. No phytotoxicity was observed during application, indicating safety for cabbage growth.

[0218] Example 6, 8% chlorfenapyr + 8% lufenuron soluble solution

[0219] 1. The content of each component is as follows:

[0220]

[0221] 2. The preparation process according to the above formulation is as follows:

[0222] (1) Prepare various raw materials according to the weight ratio of the formulation;

[0223] (2) Add the measured N,N-dimethylformamide, tetrahydrofurfuryl alcohol and N,N-dimethyl octyl decanamide into the kettle, then add chlorfenapyr and lufenuron, and mix thoroughly for about 10 min until transparent and uniform;

[0224] (3) Add phosphonate emulsifier 601P to the solution in (2) above, and stir for 10 min until transparent and uniform;

[0225] (4) Add the remaining water to the solution in (3) above, and stir for 5 min until transparent and uniform, then stand, filter, and obtain.

[0226] The quality technical indicators of the 16% chlorfenapyr·acetamiprid soluble solution prepared in this example are shown in Table 11.

[0227] Table 11 Quality technical indicators of 16% chlorfenapyr·lufenuron soluble solution

[0228]

[0229] After the sample in this example is diluted 20 times with standard hard water, it presents a true solution state, and its appearance is similar to that shown in Fig. 4L, which is more easily wetted, spread and absorbed on the target surface, thereby improving the efficacy. Figure 1

[0230] 3. Biological efficacy comparison

[0231] In order to clarify the difference in control effect of 16% chlorfenapyr·lufenuron soluble solution, 16% chlorfenapyr·lufenuron suspension concentrate and microemulsion on Spodoptera exigua, a field plot efficacy test was conducted.

[0232] The experimental method is as follows:

[0233] This test refers to "GB / T 23392.4-2009 Technical Specifications for Forecasting Diseases and Pests of Cruciferous Vegetables Part 4: Spodoptera exigua", and the test agent, control agent and blank control plot treatment are randomly arranged, with a plot area of 50 m 2 ​, 3WBD-20 type knapsack electric sprayer was used for uniform spraying, and each plot was sprayed with 8 kg of water per 667 m 2 30 kg of water per 667 m

[0234] Investigation and statistical method: 5 larger areas were selected, and 2 plots were investigated in each area at the peak of egg. Before spraying and 1 d, 3 d, and 7 d after spraying, 5-point sampling method was used, 2 plants were fixed at each point, the number of live larvae on the whole plant leaves was observed, and the data were statistically processed and analyzed by using DPS data processing system, and variance analysis was performed by using Duncan new multiple range method. The pest population reduction rate and control effect of cabbage beet armyworm were calculated according to the following formula:

[0235] Pest population reduction rate (%) = {(pre-spraying pest number - post-spraying pest number) / pre-spraying pest number} x 100;

[0236] Control effect (%) = {(pest population reduction rate in pesticide treatment area - pest population reduction rate in blank control area) / (100 - pest population reduction rate in blank control area)} x 100

[0237] Safety investigation and influence on other organisms: the influence of each pesticide treatment on the growth of cabbage and other organisms was observed on the first day after spraying and several days after spraying.

[0238] The preparation method of the used 16% bromofenpyr-ethyl·lufenuron suspension concentrate is as follows:

[0239] 8%, dispersing agent Supragil MNS / 90 (alkyl naphthalene formaldehyde condensate sulfonate, Solvay) 3%, wetting agent Dispersogen LFS (alkyl phenol polyoxyethylene-based phosphate, Solvay) 2%, 1,2-propanediol (antifreeze, Shandong Guohua Chemical Co., Ltd.) 5%, xanthan gum (thickening agent, Hebei Pengyu Biological Technology Co., Ltd.) 0.1%, Kathon (preservative, Beijing Guangyuan Yinan Chemical Co., Ltd.) 0.1%, SAG1522 (organic silicon defoaming agent, Maitu High-tech Materials Group) 0.5%, and deionized water (self-made) to make up 100%. The above raw materials are mixed and sand-milled to a particle size of less than 5 μm, and then filtered to obtain 16% bromofenpyr-ethyl·lufenuron suspension concentrate.

[0240] The preparation method of 16% bromofenpyr-ethyl·lufenuron microemulsion is as follows:

[0241] Bistrifluron 8%, chlorantraniliprole 8%, N-methylpyrrolidone (solvent, new Maychi Materials Co., Ltd.) 25%, cyclohexanone (solvent, Hunan Dongwei New Chemical Material Co., Ltd.) 15%, methanol (solvent, Qilu Petrochemical Company) 5%, 602# (emulsifier, Nanjing Taihua Chemical Co., Ltd.) 15%, deionized water (self-made) to make up 100%. Dissolve bistrifluron and chlorantraniliprole in organic solvents, add emulsifier and stir uniformly, then add water and stir uniformly to obtain 16% bistrifluron·chlorantraniliprole microemulsion.

[0242] Medicine 1: 16% bistrifluron·chlorantraniliprole soluble concentrate diluted 3000 times with water;

[0243] Medicine 2: 16% bistrifluron·chlorantraniliprole soluble concentrate diluted 4500 times with water;

[0244] Medicine 3: 16% bistrifluron·chlorantraniliprole suspension diluted 3000 times with water;

[0245] Medicine 4: 16% bistrifluron·chlorantraniliprole microemulsion diluted 3000 times with water;

[0246] Table 12 bistrifluron·chlorantraniliprole mixture efficacy test data

[0247]

[0248] As can be seen from Table 12, under the same dilution multiple, the control effect of bistrifluron·chlorantraniliprole soluble concentrate on cabbage beet armyworm is obviously higher than that of other formulations with the same content, and it has obvious advantages in reducing amount and increasing efficiency. No phytotoxicity was found during application, and it is safe to cabbage growth.

[0249] Example 7, 5% bistrifluron + 5% tachmanamide soluble concentrate

[0250] 1. The content of each component is as follows:

[0251]

[0252] 2. The preparation process according to the above formula is as follows:

[0253] (1) Prepare various raw materials according to the weight ratio of the formula;

[0254] (2) Add the weighed N,N-dimethyl lactamide, 3-methoxy-3-methyl-1-butanol and N,N-dimethyl octyl decanamide into the kettle, then add bistrifluron and tachmanamide, stir thoroughly and mix for about 10 min until transparent and uniform;

[0255] (3) Add phosphate ester emulsifier OEP-70 into the solution of (2) above, stir for 10 min to be transparent and uniform;

[0256] (4) Add the remaining water into the solution of (3) above, stir for 5 min to be transparent and uniform, stand, filter, and obtain.

[0257] The quality technical index of the 10% chlorantraniliprole·tebufenpyrad soluble solution prepared in this example is shown in Table 13.

[0258] Table 13 Quality technical index of 10% chlorantraniliprole·tebufenpyrad soluble solution

[0259]

[0260] The sample of this example presents a true solution state after 20-fold dilution with standard hard water, and its appearance is similar to that shown in Fig. 4A, which is more easily wetted, spread and absorbed on the target surface, and improves the efficacy. Figure 1

[0261] 3. Biological efficacy comparison

[0262] In order to clarify the difference in the control effect of 10% chlorantraniliprole·tebufenpyrad soluble solution, 10% chlorantraniliprole·tebufenpyrad suspension concentrate and 10% chlorantraniliprole·tebufenpyrad microemulsion on rice leaf roller, a field plot efficacy test was carried out.

[0263] The experimental method is as follows:

[0264] This test refers to GB / T 17980.2-2000 Pesticide Field Efficacy Test Guidelines (I) Insecticide Control of Rice Leaf Roller. The test agent, control agent and blank control plot treatment were randomly arranged, and the plot area was 50 m 2 2. The test agent was sprayed with a 3WBD-20 type backpack electric sprayer, and each plot was sprayed with 30 kg of water per 667 m 2 2. The test agent was sprayed with a 3WBD-20 type backpack electric sprayer, and each plot was sprayed with 30 kg of water per 667 m

[0265] Investigation and statistical method: five samples were taken from each plot, a total of 25 clusters of rice were investigated, the leaf rolling rate was calculated by comparing with the leaf rolling rate of the control area, the insect rate in the rolled leaves was investigated, and the total leaf number before spraying and the number of rolled leaves 1 day, 3 days and 7 days after spraying were investigated. The control effect of rice leaf roller was calculated according to the following formula:

[0266] Leaf rolling rate (%) = (investigated rolled leaf number) / (investigated total leaf number) x 100;

[0267] ​Control effect (%) = {(leaf curl rate of the blank control area after treatment-leaf curl rate of the treatment area after treatment) / leaf curl rate of the blank control area after treatment} x 100

[0268] Safety investigation and effects on other organisms: the effects of each treatment on the growth of rice and other organisms were observed on the first day after each spraying and on several days after spraying.

[0269] The preparation method of the used 10% broflanpyrduam·tolfenpyrad suspension concentrate is as follows:

[0270] Take bromflanpyrduam 5%, tolfenpyrad 5%, dispersant ATLOX 4913 (polyacrylate, CRODA) 3%, wetting agent Dispersogen LFS (alkyl phenol polyoxyethylene phosphate, Solvay) 2%, 1,2-propanediol (antifreeze, Shandong Guohua Chemical Co., Ltd.) 5%, xanthan gum (thickening agent, Hebei Pengyu Biological Technology Co., Ltd.) 0.1%, kathon (preservative, Beijing Guangyunnong Chemical Co., Ltd.) 0.1%, SAG 1522 (organic silicon defoaming agent, Maitu High-tech Materials Group) 0.5%, and deionized water (self-made) to make up 100% by mass percentage. The above raw materials are mixed and sand-milled to a particle size of less than 5 μm, and then filtered to obtain 10% bromflanpyrduam·tolfenpyrad suspension concentrate.

[0271] The preparation method of 10% bromflanpyrduam·tolfenpyrad microemulsion is as follows:

[0272] Take bromflanpyrduam 5%, tolfenpyrad 5%, N,N-dimethylformamide (solvent, Changzhou Poly-feng Chemical Co., Ltd.) 20%, cyclohexanone (solvent, Hunan Dongwei Chemical New Material Co., Ltd.) 15%, methanol (solvent, Qilu Petrochemical Company) 5%, 602# (emulsifier, Nanjing Taihua Chemical Co., Ltd.) 15%, and deionized water (self-made) to make up 100% by mass percentage. Dissolve bromflanpyrduam and tolfenpyrad in organic solvent, add emulsifier and stir uniformly, and finally add water and stir uniformly to obtain 10% bromflanpyrduam·tolfenpyrad microemulsion.

[0273] Pesticide 1: 10% bromflanpyrduam·tolfenpyrad soluble concentrate diluted 1500 times with water;

[0274] Pesticide 2: 10% bromflanpyrduam·tolfenpyrad soluble concentrate diluted 2000 times with water;

[0275] Pesticide 3: 10% bromflanpyrduam·tolfenpyrad suspension concentrate diluted 1500 times with water;

[0276] Pesticide 4: 10% bromflanpyrduam·tolfenpyrad microemulsion diluted 1500 times with water;

[0277] Table 14 Bromothionylphenylhydrazide·azocyclotin mixture phytotoxicity test data

[0278]

[0279] As shown in Table 14, at the same dilution ratio, bromothionylphenylhydrazide·azocyclotin soluble solution has a significantly higher control effect on rice leaf roller than other formulations with the same content, and has a significant advantage in reducing dosage and increasing efficiency. No phytotoxicity was found during application, and it is safe for rice growth.

[0280] Example 8, 10% bromothionylphenylhydrazide + 10% buprofezin soluble solution

[0281] 1. The content of each component is as follows:

[0282]

[0283] 2. The preparation process according to the above formula is as follows:

[0284] (1) Prepare various raw materials according to the weight ratio of the formula;

[0285] (2) Add the measured N,N-dimethylformamide, diacetone alcohol and N,N-dimethyl octylamide into the kettle, then add bromothionylphenylhydrazide and buprofezin, and mix thoroughly for about 10 min until transparent and uniform;

[0286] (3) Add phosphonate emulsifier 601P to the solution in (2) above, and stir for 10 min until transparent and uniform;

[0287] (4) Add the remaining water to the solution in (3) above, and stir for 5 min until transparent and uniform, then stand and filter to obtain the product.

[0288] The quality technical indicators of the 20% bromothionylphenylhydrazide·buprofezin soluble solution prepared in this example are shown in Table 15.

[0289] Table 15 Quality technical indicators of 20% bromothionylphenylhydrazide·buprofezin soluble solution

[0290]

[0291] After the sample in this example is diluted 20 times with standard hard water, it presents a true solution state, and its appearance is similar to that shown in Fig. 4A, which is more easily wetted, spread and absorbed on the target surface, thereby improving the efficacy. Figure 1

[0292] 3. Biological efficacy comparison

[0293] ​In order to clarify the difference of control effect of 20% halofenozide·chlorfenapyr soluble concentrate and 20% halofenozide·chlorfenapyr suspension concentrate and microemulsion on Spodoptera exigua, field plot efficacy test was carried out.

[0294] The experimental method is as follows:

[0295] In this test, the test agent, control agent and blank control plot treatment were arranged randomly according to GB / T 23392.4-2009 Technical Specifications for Forecasting Diseases and Insect Pests of Cruciferous Vegetables Part 4: Spodoptera exigua. The plot area was 50m 2 . 30kg of water was used for each plot, and other agents were not used during the test. Each treatment was repeated 4 times. 2 30kg of water was used for each plot, and other agents were not used during the test. Each treatment was repeated 4 times.

[0296] Investigation and statistical method: 5 larger areas were selected, and 2 plots were investigated in each area at the peak of egg. Before and after spraying, 5-point sampling method was used, 2 plants were selected at each point, the number of live larvae on the whole leaf was observed, and DPS data processing system was used for data statistics and analysis, and Duncan new multiple range method was used for variance analysis. The reduction rate of Spodoptera exigua and the control effect were calculated according to the following formula:

[0297] Reduction rate (%) = {(number of insects before spraying-number of insects after spraying) / number of insects before spraying} x 100;

[0298] Control effect (%) = {(reduction rate of insect population in agent treatment area-reduction rate of insect population in blank control area) / (100-reduction rate of insect population in blank control area)} x 100

[0299] Safety investigation and influence on other organisms: the influence of each agent treatment on the growth of Chinese flowering cabbage and other organisms was observed on the first day after spraying and several days after spraying.

[0300] The preparation method of 20% halofenozide·chlorfenapyr suspension concentrate used is as follows:

[0301] Bistrifluron 10%, chlorfenapyr 10%, dispersing agent ATLOX 4913 (polyacrylate, CRODA) 4%, wetting agent TEGITOL W-600 (isomeric alcohol polyoxyethylene ether, DOW) 3%, 1,2-propanediol (antifreezing agent, Shandong Guohua Chemical Co., Ltd.) 5%, xanthan gum (thickening agent, Hebei Pengyu Biological Technology Co., Ltd.) 0.1%, kathon (preservative, Beijing Guangyuan Yinan Chemical Co., Ltd.) 0.1%, SAG 1522 (silicone antifoaming agent, Momentive Performance Materials) 0.5%, deionized water (self-made) to 100%. The above raw materials were mixed and sand-milled to a particle size of less than 5 μm, and then filtered to obtain 20% bistrifluron·chlorfenapyr SC.

[0302] The preparation method of 20% bistrifluron·chlorfenapyr ME is as follows:

[0303] Bistrifluron 10%, chlorfenapyr 10%, N,N-dimethylformamide (solvent, Changzhou Poly-Feng Chemical Co., Ltd.) 30%, cyclohexanone (solvent, Hunan Dongwei Chemical New Material Co., Ltd.) 10%, methanol (solvent, Qilu Petrochemical Company) 5%, 602# (emulsifier, Nanjing Taihua Chemical Co., Ltd.) 15%, deionized water (self-made) to 100%. Bistrifluron and chlorfenapyr were dissolved in organic solvents, the emulsifier was added and stirred uniformly, and then water was added and stirred uniformly to obtain 20% bistrifluron·chlorfenapyr ME.

[0304] Medicine 1: 20% bistrifluron·chlorfenapyr SL was diluted 3000 times with water;

[0305] Medicine 2: 20% bistrifluron·chlorfenapyr SL was diluted 4500 times with water;

[0306] Medicine 3: 20% bistrifluron·chlorfenapyr SC was diluted 3000 times with water;

[0307] Medicine 4: 20% bistrifluron·chlorfenapyr ME was diluted 3000 times with water;

[0308] Table 16 bistrifluron·chlorfenapyr mixture efficacy test data

[0309]

[0310] As can be seen from Table 16, under the same dilution multiple, the control effect of bistrifluron·chlorfenapyr SL on beet armyworm of Chinese flowering cabbage was obviously higher than that of other formulations with the same content, and it had obvious advantages in reducing amount and increasing efficiency. No phytotoxicity was found during application, and it was safe to Chinese flowering cabbage.

[0311] In summary, the soluble liquid containing bromofenprox provided by the application and the preparation method thereof can achieve the following beneficial effects:

[0312] The application is beneficial to protecting the agricultural ecological environment, the raw materials are safe and environmentally friendly, and the pollution to the environment is reduced.

[0313] The preparation method provided by the application can obtain a preparation product meeting the nanoscale, and can effectively reduce the pesticide usage amount, so that the purpose of reducing the amount and increasing the effect is achieved.

[0314] The raw materials used in the application are convenient and easy to obtain, and have significant market competitiveness for industrialization and popularization and application.

Claims

1. A soluble solvent containing bromfenac, comprising, by weight percentage: 1%~10% bromfenac, 1%~10% active component B, 25%~45% amide solvent, 5%~15% alcohol solvent, 5%~15% phosphate emulsifier, 0%~1% stabilizer, and the balance being water; The active component B is selected from at least one of the following: abamectin, avermectin, lambda-cyhalothrin, thiamethoxam, acetamiprid, lufenuron, chlorfenapyr, and chlorfenapyr. The amide solvent is selected from any one of the following: 1) N,N-diethylformamide and N,N-dimethyloctadecanamide in a mass ratio of 1:0.5~0.8; 2) N,N-dimethyllactic acid and N,N-dimethyldecanoic acid in a mass ratio of 1:0.125~0.25; 3) N,N-dimethyllactic acid and N,N-dimethyloctyldecanoic acid in a mass ratio of 1:0.6~1; The alcohol solvent is selected from at least one of tetrahydrofurfuryl alcohol, diacetone alcohol, 3-methoxy-3-methyl-1-butanol, and isohexanediol; The phosphate emulsifier is selected from at least one of styrene-phenol polyoxyethylene ether phosphate, fatty alcohol polyoxyethylene ether phosphate, polyethylene glycol 400 monooleate phosphate, oleyl alcohol polyoxyethylene ether phosphate, and alkoxylated phosphate.

2. The soluble agent according to claim 1, characterized in that: The stabilizer is selected from at least one of caprylic / capric acid, 2,6-di-tert-butyl-p-methylphenol, and 2-hydroxy-4-n-octyloxybenzophenone.

3. The method for preparing the soluble solvent according to claim 1 or 2, comprising the following steps: (1) Mix the amide solvent, alcohol solvent, bromoxynil diamide, active component B and stabilizer, and stir until transparent and homogeneous; (2) Add the phosphate emulsifier to the solution in (1) and stir until it is transparent and homogeneous; (3) Add water to the solution in (2) and stir until it is transparent and homogeneous.

4. The preparation method according to claim 3, characterized in that: In step (1), the stirring time is 5~15 min; In steps (2) and (3), the stirring time is 5 to 10 minutes.

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