Bisamide compound as well as preparation method, intermediate preparation equipment and application thereof

Abstract

The invention belongs to the technical field of insecticides, and particularly relates to a bisamide compound and a preparation method, intermediate preparation equipment and application thereof. The preparation method comprises the steps that 2-fluoro-3-nitrobenzoic acid and thionyl chloride generate a compound A under the action of dimethylformamide; the compound A and 2-trifluoromethyl-4-heptafluoroisopropyl-6-bromaniline amide are subjected to a condensation reaction, and a compound B is obtained; performing reduction reaction on the compound B to obtain a compound C; carrying out substitution reaction on the compound C and formaldehyde to obtain a compound D; the compound D and 3, 5-dichloro-4-fluorobenzoyl chloride are subjected to an amide condensation reaction, and the bisamide compound is obtained. The bisamide compound has the beneficial effects that the problem of drug resistance of pests is solved, the bisamide compound has high insecticidal activity and a good insecticidal effect under a low dosage, and meanwhile, the preparation method of the bisamide compound is mild in reaction condition, few in by-products and high in reaction yield, and reduces the raw material loss, so that the production cost is reduced.

Description

Technical Field

[0001] The present invention belongs to the technical field of insecticides, and particularly relates to a diamide compound, a preparation method thereof, an intermediate preparation device and an application thereof. Background Art

[0002] Due to their unique action mechanisms, novel action targets and environmental friendliness, diamide compounds have increasingly become a research hotspot for pesticide companies. Existing diamide compounds have brought great benefits to agricultural production, but they also have certain side effects. In the specific control process, due to the long-term single use of a certain diamide compound, pests are likely to develop varying degrees of drug resistance. In addition, existing diamide compounds have insecticidal or acaricidal activity, but their insecticidal effects are not ideal at low doses. Therefore, a diamide compound is provided, which has high insecticidal activity and can solve the problem of pest drug resistance.

[0003] When the present invention prepares the diamide compound, it involves a reduction reaction with hydrogen as the raw material. Since the moving speed of hydrogen in the reaction solution is fast and the contact time between hydrogen and the substrate is short, the reaction efficiency is reduced. And in order to make the substrate react completely, an excessive amount of hydrogen needs to be introduced. However, a large amount of hydrogen does not participate in the reaction, resulting in low hydrogen utilization rate, thereby increasing the production cost and increasing the danger. Summary of the Invention

[0004] The present invention addresses the above problems and provides a diamide compound, a preparation method thereof, an intermediate preparation device and an application thereof.

[0005] The present invention relates to an intermediate preparation device for a diamide compound, comprising a main body, a hydrogen control mechanism, a hydrogen circulation mechanism, a hydrogen inlet mechanism, a stirring mechanism and a liquid material circulation mechanism; The hydrogen control mechanism is arranged above the main body, the hydrogen circulation mechanism is arranged above the inside of the main body, a stirring mechanism is arranged below the hydrogen circulation mechanism, the hydrogen inlet mechanism is arranged below the main body, both the hydrogen control mechanism and the hydrogen circulation mechanism are communicated with the main body through the hydrogen inlet mechanism, the liquid material circulation mechanism is arranged on one side of the main body, and the liquid material circulation mechanism is communicated with the main body; A material inlet is provided above the main body, a material outlet is provided at the bottom of the main body, and plugs are detachably connected inside the material inlet and the material outlet.

[0006] Preferably, the hydrogen control mechanism includes a main hydrogen delivery pipe, which is externally connected to a hydrogen supply system. A hydrogen flow control component is arranged inside the main hydrogen delivery pipe. A hydrogen delivery branch pipe is connected to the side of the main hydrogen delivery pipe. A support is fixedly connected to the bottom of the main hydrogen delivery pipe, and the support is fixedly connected to the top of the main body. One side of the main hydrogen delivery pipe is rotatably connected to a transmission rod through a bearing. The end of the transmission rod on the outside of the main hydrogen delivery pipe is fixedly connected with an external cylindrical gear. The external cylindrical gear is connected to a pneumatic floating component in a transmission manner, and the transmission rod is connected to the hydrogen flow control component in a transmission manner.

[0007] Preferably, the hydrogen flow control component includes a support rod and a support plate. The edge of the support plate is fixedly connected to the inner wall of the main hydrogen delivery pipe. The bottom of the main hydrogen delivery pipe is sealed. The lower end of the support rod is rotatably connected to the bottom inside the main hydrogen delivery pipe through a bearing, and the upper end of the support rod is rotatably connected to the support plate through a bearing. A first bevel gear is sleeved below the support rod. The first bevel gear is connected to a second bevel gear in a transmission manner, and the second bevel gear is fixedly connected to one end of the transmission rod. A third bevel gear is sleeved above the support rod. The third bevel gear is connected to four fourth bevel gears in a transmission manner. One side of each of the four fourth bevel gears away from the third bevel gear is fixedly connected with a rotating cross bar. One side of each of the four rotating cross bars away from the fourth bevel gear is fixedly connected with a fifth bevel gear. The outer walls of the four rotating cross bars are all rotatably connected with limiting rod sleeves. The limiting rod sleeves are all fixedly connected to the inner wall of the main hydrogen delivery pipe through L-shaped brackets. Each of the four fifth bevel gears is connected to a sixth bevel gear in a transmission manner. A rotating vertical rod is fixedly connected above each of the four sixth bevel gears. Eight fan-shaped holes are formed in the support plate. Every two of the fan-shaped holes correspond to each other. A limiting ring plate is fixedly connected below each of the two corresponding fan-shaped holes on the support plate. A rotating groove is formed on one side of each of the four limiting ring plates close to the support plate. A double-sector baffle is rotatably connected in each of the four rotating grooves. The centers of the bottoms of the four double-sector baffles are respectively fixedly connected to the upper ends of the four rotating vertical rods.

[0008] Preferably, the pneumatic floating component includes a floating plate, which is slidably connected above the inside of the main body. A sealing ring is arranged on the edge of the floating plate. A floating rod is fixedly connected above the floating plate. The upper end of the floating rod passes through and is slidably connected to the top of the main body. A plurality of teeth are axially arranged on the floating rod above the main body. The plurality of teeth are meshed with the external cylindrical gear. Above the floating plate, two sliding rods are fixedly connected. The upper ends of the two sliding rods pass through and are slidably connected to the top of the main body. The upper ends of the two sliding rods are fixedly connected with limit circular plates. A sealing cover is arranged outside the two limit circular plates. The bottoms of the two sealing covers are fixedly connected to the top of the main body. Springs are arranged between the top surfaces inside the two sealing covers and the limit circular plates.

[0009] Preferably, the hydrogen circulation mechanism includes a hydrogen storage cavity, which is arranged below the floating plate inside the main body. Both sides of the hydrogen storage cavity are communicated with suction cylinders. Inside both suction cylinders, piston rods are arranged. One end of each of the two piston rods passes through the suction cylinder and is fixedly connected with a connecting plate, and the other end of each of the two piston rods is fixedly connected with a piston plate. At the corresponding positions of the two suction cylinders at the bottom of the hydrogen storage cavity, linear telescopic devices are fixedly connected. The push rods of the two linear telescopic devices are fixedly connected to the connecting plate. Two hydrogen inlets are opened at the bottom of the hydrogen storage cavity. At the two hydrogen inlets, the hydrogen storage cavity is detachably connected with inlet pipes, and inlet one-way valves are installed on the inlet pipes. A hydrogen outlet is opened at the top of the hydrogen storage cavity. At the hydrogen outlet, the hydrogen storage cavity is detachably connected with a main hydrogen circulation pipe, and an outlet one-way valve is installed on the main hydrogen circulation pipe. The main hydrogen circulation pipe passes through and is rotatably connected to the floating plate and the top of the main body in sequence upwards, and the floating plate slides along the axial direction of the main hydrogen circulation pipe. A gear one is sleeved outside the main hydrogen circulation pipe above the main body. The gear one is meshed with a gear two. Above the gear two, a motor is fixedly connected. The motor is fixedly connected to the top of the main body through an L-shaped connecting plate. The main hydrogen circulation pipe is connected with a rotary joint above the gear one, and a hydrogen circulation branch pipe is connected above the rotary joint.

[0010] Preferably, the hydrogen intake mechanism includes a pressure pump, which is fixedly connected to the bottom of the main body. The pressure pump is provided with a gas outlet and two gas inlets. The two gas inlets of the pressure pump are respectively connected with a hydrogen delivery branch pipe and a hydrogen circulation branch pipe. The gas outlet of the pressure pump is communicated with a main hydrogen intake pipe. The main hydrogen intake pipe passes through the bottom of the main body. The outlet end of the main hydrogen intake pipe is communicated with an intake pipe group. The intake pipe group includes an intake ring pipe one and an intake ring pipe two. The intake ring pipe one, the intake ring pipe two and the main hydrogen intake pipe are interconnected through a plurality of intake branch pipes. Above the intake ring pipe one, the intake ring pipe two and the plurality of intake branch pipes, a plurality of hydrogen spray nozzles are arranged.

[0011] Preferably, the stirring mechanism includes a stirring rod disposed between the hydrogen storage cavity and the intake pipe group. The upper end of the stirring rod is fixedly connected to the bottom of the hydrogen storage cavity. Stirring blade groups are provided on the outer wall of the stirring rod at different heights, and sieve plate assemblies are provided between adjacent stirring blade groups. Each of the three sieve plate assemblies includes a sieve plate, with filling layers fixedly connected to the upper and lower sides of the sieve plate respectively. The sieve plate and the two filling layers are all fixedly connected to the inner wall of the main body. The stirring rod passes through and is rotatably connected to the central positions of the sieve plate and the two filling layers; The liquid material circulation mechanism includes a turbine pump. A first liquid material circulation pipe is connected to the inlet of the turbine pump. Two second liquid material circulation pipes are connected to the first liquid material circulation pipe. A third liquid material circulation pipe is connected to the outlet of the turbine pump. On one side of the main body, liquid material outlets are respectively provided above the three sieve plate assemblies. The three liquid material outlets are sequentially connected to the side of the first liquid material circulation pipe and the two second liquid material circulation pipes away from the turbine pump from top to bottom. A liquid material inlet is provided below the main body at the positions of the three liquid material outlets. The liquid material inlet is disposed below the third sieve plate assembly from top to bottom, and the liquid material inlet is connected to the side of the third liquid material circulation pipe away from the turbine pump.

[0012] The present invention also relates to a bisamide compound, and an intermediate thereof is prepared using the preparation equipment for the intermediate of the bisamide compound, and the specific structure is as follows: ; The chemical name is: N-(2-bromo-4-(perfluoropropan-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-(N-methyl-4-fluoro-3,5-dichlorobenzamide)benzamide.

[0013] The present invention also relates to a preparation method of a bisamide compound. The bisamide compound is prepared, and the specific preparation method is as follows: (1) 2-Fluoro-3-nitrobenzoic acid, a solvent, thionyl chloride and dimethylformamide are sequentially added to a reaction vessel. After stirring evenly, the temperature is raised for reaction. After the reaction is monitored by TLC and ended, distillation under reduced pressure is carried out to obtain 2-fluoro-3-nitrobenzoyl chloride, which is compound A. The reaction formula is: ; (2) Compound A prepared in step (1) and a solvent are sequentially added to a reaction vessel. After stirring evenly, sodium bicarbonate and 2-trifluoromethyl-4-heptafluoroisopropyl-6-bromoaniline are added. Stirring and temperature raising reactions are carried out. After the reaction is monitored by TLC and ended, the temperature is first lowered, and then water extraction and liquid separation are carried out. The organic phase is evaporated to dryness to obtain N-(2-bromo-4-(perfluoropropan-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-nitrobenzamide, which is compound B. The reaction formula is: ; (3) Add the compound B prepared in step (2), a solvent, and a catalyst into the reaction vessel in sequence. After stirring evenly, introduce hydrogen gas, stir and heat up for reaction. After monitoring the reaction by TLC until it ends, filter, and evaporate the filtrate to dryness to obtain 3-amino-N-(2-bromo-4-(perfluoropropan-2-yl)-6-(trifluoromethyl)phenyl)-2-fluorobenzamide, which is compound C. The reaction formula is as follows: ; (4) Add the compound C prepared in step (3) into the reaction vessel, then add concentrated sulfuric acid, stir until completely dissolved, and slowly dropwise add an aqueous formaldehyde solution under temperature control conditions. After the addition is complete, heat up for reaction. After monitoring the reaction by TLC until it ends, first cool down, then pour the reaction solution into ice water, stir until all solids precipitate, filter, wash the filter cake with water, and dry the filter cake to obtain N-(2-bromo-4-(perfluoropropan-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-(methylamino)benzamide, which is compound D. The reaction formula is as follows: ; (5) Add 3,5-dichloro-4-fluorobenzoyl chloride and a solvent into the reaction vessel in sequence. After stirring evenly, add the compound D prepared in step (4) in batches, then heat up and carry out a reflux reaction. After monitoring the reaction by TLC until it ends, cool down and filter. Wash the filter cake with the solvent and dry it to obtain the final product N-(2-bromo-4-(perfluoropropan-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-(N-methyl-4-fluoro-3,5-dichlorobenzamide)benzamide, which is the said diamide compound. The reaction formula is as follows: .

[0014] Preferably, in the said step (1), the molar ratio of 2-fluoro-3-nitrobenzoic acid, thionyl chloride, and dimethylformamide is 1:1 - 1.1:0.01 - 0.1; the solvent is dichloromethane, and the mass ratio of 2-fluoro-3-nitrobenzoic acid to the solvent is 1:1 - 3; heat up to 60 - 100 °C and react for 4 - 8 h; In the said step (2), the molar ratio of 2-trifluoromethyl-4-heptafluoroisopropyl-6-bromoaniline, compound A, and sodium bicarbonate is 1:1 - 1.2:1 - 1.2; the solvent is dichloromethane, and the mass ratio of compound A to the solvent is 1:1 - 5; heat up to 50 - 90 °C and react for 6 - 10 h; cool down to 20 - 30 °C; In the said step (3), the molar ratio of compound B and the catalyst is 1:0.005 - 0.01, the solvent is absolute ethanol, and the mass ratio of the solvent to compound B is 1:2 - 4; the catalyst is 5% palladium-carbon, heat up to 30 - 35 °C and react for 3 - 5 h; In step (4), the molar ratio of compound C, formaldehyde and concentrated sulfuric acid is 1:2-6:1-1.2; when dropping the aqueous formaldehyde solution, the temperature is controlled at 30-35°C; the temperature is raised to 35-45°C and reacted for 10-12 h; the temperature is lowered to 20-30°C; the mass ratio of compound C to ice water is 1:2-3; In step (5), the molar ratio of compound D and 3,5-dichloro-4-fluorobenzoyl chloride is 1:1-1.1; the solvent is toluene, and the mass ratio of compound D to the solvent is 1:2-5; the temperature is raised to 90-120°C and refluxed for 6-8 h; the temperature is lowered to 20-30°C.

[0015] The present invention also relates to the application of a diamide compound. The diamide compound is used to prepare a pesticide composition. The diamide compound is used as the main active ingredient of the pesticide composition, and the pesticide composition further includes a formulation carrier or a formulation adjuvant; the pesticide composition is used as an insecticide to control crop pests or mites; the pesticide composition is used as a repellent to repel crop pests; the crop pests are Helicoverpa armigera or Spodoptera exigua.

[0016] Compared with the prior art, the advantages and positive effects of the present invention are as follows: (1) For the intermediate preparation equipment of the diamide compound, the hydrogen addition amount during the reaction can be controlled by the hydrogen control mechanism, and the unreacted hydrogen can be recycled back to the reaction solution through the hydrogen circulation mechanism and continue to react with the substrate. At the same time, the unreacted hydrogen in the upper reaction solution is recycled back to the bottom by the turbine pump, and the filling layer of the sieve plate assembly effectively reduces the rising rate of hydrogen. Therefore, the preparation equipment improves the utilization rate of hydrogen, effectively avoids the waste caused by excessive hydrogen, and reduces the production cost; (2) For the intermediate preparation equipment of the diamide compound, the pressure of hydrogen entering the reaction solution is increased by the pressure pump, the solubility of hydrogen in the reaction solution is increased, and the sieve plate of the sieve plate assembly improves the contact between hydrogen and the substrate. At the same time, the reaction solution can increase the collision between hydrogen and the substrate in the turbine pump, and the turbine pump solves the unevenness of the reaction solution caused by the sieve plate assembly. Therefore, the preparation equipment improves the reaction efficiency; (3) The diamide compound solves the problem of pest resistance, has high insecticidal activity, has good insecticidal effect at low doses, and the preparation method of the diamide compound has mild reaction conditions, few by-products, and high reaction yield, reducing raw material loss and thus reducing the production cost. Description of the Drawings

[0017] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly introduced below: Figure 1Schematic diagram of the intermediate preparation equipment for the diamide compound provided in Example 6; Figure 2 Internal structure diagram of the intermediate preparation equipment for the diamide compound provided in Example 6; Figure 3 Internal structure diagram of the main hydrogen delivery pipe provided in Example 6; Figure 4 Bottom structure diagram of the hydrogen flow control component provided in Example 6; Figure 5 Schematic diagram of the support plate provided in Example 6; Figure 6 Schematic diagram of the double-sector baffle provided in Example 6; Figure 7 Internal structure diagram of the sealing cover provided in Example 6; Figure 8 Schematic diagram of the intake pipe group provided in Example 6; Figure 9 Schematic diagram of the sieve plate assembly provided in Example 6.

[0018] Explanation of reference numerals: 1, main body; 2, main hydrogen delivery pipe; 3, hydrogen delivery branch pipe; 4, support; 5, transmission rod; 6, external cylindrical gear; 7, support rod; 8, support plate; 9, first bevel gear; 10, second bevel gear; 11, third bevel gear; 12, fourth bevel gear; 13, rotating cross bar; 14, fifth bevel gear; 15, limit rod sleeve; 16, L-shaped bracket; 17, sixth bevel gear; 18, rotating vertical rod; 19, fan-shaped hole; 20, limit ring plate; 21, double-sector baffle; 22, floating plate; 23, floating rod; 24, tooth; 25, sliding rod; 26, limit circular plate; 27, sealing cover; 28, spring; 29, hydrogen storage cavity; 30, suction cylinder; 31, piston rod; 32, connecting plate; 33, linear expansion device; 34, intake one-way valve; 35, outlet one-way valve; 36, main hydrogen circulation pipe; 37, first gear; 38, second gear; 39, motor; 40, rotating joint; 41, hydrogen circulation branch pipe; 42, pressure pump; 43, main hydrogen intake pipe; 44, first intake ring pipe; 45, second intake ring pipe; 46, intake branch pipe; 47, hydrogen spray head; 48, stirring rod; 49, stirring blade group; 50, sieve plate; 51, filling layer; 52, turbine pump; 53, first liquid circulation pipe; 54, second liquid circulation pipe; 55, third liquid circulation pipe; 56, material inlet; 57, material outlet; 58, L-shaped connecting plate. Detailed implementation manners

[0019] In order to more clearly understand the above-mentioned objects, features and advantages of the present invention, the present invention will be further described below in conjunction with the embodiments and the drawings.

[0020] In the following description, many specific details are set forth to facilitate a full understanding of the present invention. However, the present invention may also be implemented in other ways different from those described herein. Therefore, the present invention is not limited by the specific embodiments disclosed in the following specification.

[0021] Example 1 Preparation of 2-fluoro-3-nitrobenzoyl chloride: 925 g (5 mol) of 2-fluoro-3-nitrobenzoic acid, 2775 g of dichloromethane, 625 g (5.25 mol) of thionyl chloride and 18.25 g (0.25 mol) of dimethylformamide were successively added to a reaction vessel. After stirring evenly, the temperature was raised to 80 °C and the reaction was carried out for 6 h. After monitoring the reaction by TLC and the reaction was completed, the mixture was distilled under reduced pressure until no distillate was obtained, and 975 g (4.8 mol) of 2-fluoro-3-nitrobenzoyl chloride (Compound A) was obtained, with a yield of 95.8% and a purity of 98.7%.

[0022] Example 2 Preparation of N-(2-bromo-4-(perfluoropropan-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-nitrobenzamide: 814.4 g (4 mol) of Compound A prepared in Example 1 and 610 g of dichloromethane were successively added to a reaction vessel. After stirring evenly, 369.6 g (4.4 mol) of sodium bicarbonate and 1795.2 g (4.4 mol) of 2-trifluoromethyl-4-heptafluoroisopropyl-6-bromoaniline were added. Stirring was started and the temperature was raised to 70 °C for 8 h. After monitoring the reaction by TLC and the reaction was completed, the temperature was first lowered to 25 °C, and then 1200 g of water was added for extraction and liquid separation. The organic phase was evaporated to dryness to obtain 2275.2 g (3.96 mol) of N-(2-bromo-4-(perfluoropropan-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-nitrobenzamide (Compound B), with a yield of 98.9% and a purity of 99.1%. 1 H NMR (400 MHz, DMSO) δ 11.10 (s, 1H), 8.46 (d, 1H), 8.38 (ddd, 1H), 8.04 (ddd, 1H), 7.99 (d, 1H), 7.64 (t, 1H).

[0023] Example 3 Preparation of 3-amino-N-(2-bromo-4-(perfluoropropan-2-yl)-6-(trifluoromethyl)phenyl)-2-fluorobenzamide: To the reaction vessel, 1725 g (3 mol) of compound B prepared in Example 2, 4500 g of absolute ethanol, and 51 g (0.024 mol) of 5% palladium on carbon were added in sequence. After stirring evenly, hydrogen was introduced, and the mixture was stirred and heated to 35 °C for reaction for 4 h. After monitoring the end of the reaction by TLC, filtration was carried out, and the filtrate was evaporated to dryness to obtain 1619.1 g (2.97 mol) of 3-amino-N-(2-bromo-4-(perfluoropropan-2-yl)-6-(trifluoromethyl)phenyl)-2-fluorobenzamide (compound C), with a yield of 99% and a purity of 98.9%. 1 1H NMR (400 MHz, DMSO) δ 10.50 (d, 1H), 8.41 (d, 1H), 7.96 (d, 1H), 7.01 (t, 1H), 6.94 (td, 1H), 6.81 (ddd, 1H), 5.43 (s, 2H).

[0024] Example 4 Preparation of N-(2-bromo-4-(perfluoropropan-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-(methylamino)benzamide: To the reaction vessel, 1090.2 g (2 mol) of compound C prepared in Example 3 was added, and then 215.8 g (2.2 mol) of concentrated sulfuric acid was added. After stirring until completely dissolved, 450.4 g (6 mol) of 40% aqueous formaldehyde solution was slowly added dropwise under temperature control. After the addition was completed, the temperature was raised to 35 °C for reaction for 12 h. After monitoring the end of the reaction by TLC, the temperature was first lowered, and then the reaction solution was poured into 440 g of ice water. After stirring until all the solids precipitated, filtration was carried out, and the filter cake was washed with 200 ml of water. The filter cake was dried to obtain 1065.8 g (1.9 mol) of a pale yellow solid, which was N-(2-bromo-4-(perfluoropropan-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-(methylamino)benzamide (compound D), with a yield of 95.3% and a purity of 98.7%. 1H NMR (400 MHz, DMSO) δ 10.53 (m, 1H), 8.42 (d, 1H), 7.96 (d, 1H), 7.13 (t, 1H), 6.83 (t, 2H), 5.87 (s, 1H), 2.76 (s, 3H).

[0025] Example 5 Preparation of N-(2-bromo-4-(perfluoropropan-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-(N-methyl-4-fluorobenzamide)benzamide: 250 g (1.1 mol) of 3,5-dichloro-4-fluorobenzoyl chloride and 1200 g of toluene were successively added to a reaction vessel. After stirring evenly, 560 g (1 mol) of compound D prepared in Example 4 was added in batches. Then the temperature was raised to 100 °C and reflux reaction was carried out for 7 h. After monitoring the reaction by TLC and the reaction was completed, the temperature was lowered to 25 °C, then filtered. The filter cake was washed with a solvent and dried to obtain 736.7 g (0.98 mol) of the final product N-(2-bromo-4-(2,2,2-trifluoropropan-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-(N-methyl-4-fluoro-3,5-dichlorobenzamide)benzamide, which is the bisamide compound. The yield was 98.2% and the purity was 98.5%. 1H NMR (400 MHz, DMSO) δ 10.67 (s, 1H), 8.40 (s, 1H), 7.94 (s, 1H), 7.79 (t, 1H), 7.64 (t, 1H), 7.44 (m, 3H), 3.37 (s, 3H).

[0026] Example 6 As Figures 1-9 shown, a preparation device for an intermediate of a bisamide compound includes a main body 1, a hydrogen control mechanism, a hydrogen circulation mechanism, a hydrogen inlet mechanism, a stirring mechanism and a liquid material circulation mechanism.

[0027] As Figures 1-9 shown, the hydrogen control mechanism is arranged above the main body 1, the hydrogen circulation mechanism is arranged above the main body 1, a stirring mechanism is arranged below the hydrogen circulation mechanism, the hydrogen inlet mechanism is arranged below the main body 1, both the hydrogen control mechanism and the hydrogen circulation mechanism are communicated with the main body 1 through the hydrogen inlet mechanism, the liquid material circulation mechanism is arranged on one side of the main body 1, and the liquid material circulation mechanism is communicated with the main body 1.

[0028] As Figures 1-9 shown, a material inlet 56 is opened above the main body 1, a material outlet 57 is opened at the bottom of the main body 1, and plugs are detachably connected in both the material inlet 56 and the material outlet 57.

[0029] As Figures 1-9 shown, the hydrogen control mechanism includes a hydrogen delivery main pipe 2. The hydrogen delivery main pipe 2 is externally connected to a hydrogen supply system. A hydrogen flow control component is arranged inside the hydrogen delivery main pipe 2. A hydrogen delivery branch pipe 3 is communicated with the side surface of the hydrogen delivery main pipe 2. A support 4 is fixedly connected to the bottom of the hydrogen delivery main pipe 2, and the support 4 is fixedly connected to the top of the main body 1. One side of the hydrogen delivery main pipe 2 is rotationally connected with a transmission rod 5 through a bearing. An end of the transmission rod 5 on the outer side of the hydrogen delivery main pipe 2 is fixedly connected with a cylindrical external gear 6. The cylindrical external gear 6 is in transmission connection with a pneumatic floating component, and the transmission rod 5 is in transmission connection with the hydrogen flow control component.

[0030] As Figures 1-9As shown in the figure, the hydrogen flow control component includes a support rod 7 and a support plate 8. The edge of the support plate 8 is fixedly connected to the inner wall of the main hydrogen delivery pipe 2. The bottom of the main hydrogen delivery pipe 2 is sealed. The lower end of the support rod 7 is rotatably connected to the bottom inside the main hydrogen delivery pipe 2 through a bearing, and the upper end of the support rod 7 is rotatably connected to the support plate 8 through a bearing. A first bevel gear 9 is sleeved below the support rod 7. The first bevel gear 9 is drivingly connected to a second bevel gear 10. The second bevel gear 10 is fixedly connected to one end of a transmission rod 5. A third bevel gear 11 is sleeved above the support rod 7. The third bevel gear 11 is drivingly connected to four fourth bevel gears 12. One side of each of the four fourth bevel gears 12 away from the third bevel gear 11 is fixedly connected to a rotating cross bar 13. One side of each of the four rotating cross bars 13 away from the fourth bevel gear 12 is fixedly connected to a fifth bevel gear 14. A limiting rod sleeve 15 is rotatably connected to the outer wall of each of the four rotating cross bars 13. The limiting rod sleeves 15 are fixedly connected to the inner wall of the main hydrogen delivery pipe 2 through L-shaped brackets 16. Each of the four fifth bevel gears 14 is drivingly connected to a sixth bevel gear 17. A rotating vertical rod 18 is fixedly connected above each of the four sixth bevel gears 17.

[0031] As Figures 1-9 shown in the figure, eight sector holes 19 are formed in the support plate 8. Every two sector holes 19 correspond to each other. A limiting ring plate 20 is fixedly connected below each pair of corresponding sector holes 19 on the support plate 8. A rotating groove is formed on one side of each of the four limiting ring plates 20 close to the support plate 8. A double-sector baffle 21 is rotatably connected in each of the four rotating grooves. The centers of the bottoms of the four double-sector baffles 21 are fixedly connected to the upper ends of the four rotating vertical rods 18 respectively.

[0032] As Figures 1-9 shown in the figure, the air pressure floating component includes a floating plate 22. The floating plate 22 is slidably connected above the inside of the main body 1. A sealing ring is arranged at the edge of the floating plate 22. A floating rod 23 is fixedly connected above the floating plate 22. The upper end of the floating rod 23 passes through and is slidably connected to the top of the main body 1. A plurality of teeth 24 are arranged axially above the main body 1 on the floating rod 23. The plurality of teeth 24 are meshed and connected with an external cylindrical gear 6.

[0033] As Figures 1-9 shown in the figure, two sliding rods 25 are fixedly connected above the floating plate 22. The upper ends of the two sliding rods 25 pass through and are slidably connected to the top of the main body 1. Limiting circular plates 26 are fixedly connected to the upper ends of the two sliding rods 25. A sealing cover 27 is arranged outside the two limiting circular plates 26. The bottoms of the two sealing covers 27 are fixedly connected to the top of the main body 1. Springs 28 are arranged between the top surfaces inside the two sealing covers 27 and the limiting circular plates 26.

[0034] As Figures 1-9As shown, the hydrogen circulation mechanism includes a hydrogen storage cavity 29. The hydrogen storage cavity 29 is arranged inside the main body 1 below the floating plate 22. Both sides of the hydrogen storage cavity 29 are communicated with an air suction cylinder body 30. A piston rod 31 is arranged inside each of the two air suction cylinder bodies 30. One end of each of the two piston rods 31 passes through the air suction cylinder body 30 and is fixedly connected to a connecting plate 32. The other ends of the two piston rods 31 are fixedly connected to a piston plate. At the corresponding positions of the two air suction cylinder bodies 30, a linear expansion device 33 is fixedly connected to the bottom of the hydrogen storage cavity 29. The push rods of the two linear expansion devices 33 are fixedly connected to the connecting plate 32.

[0035] As Figures 1-9 As shown, two hydrogen inlets are opened at the bottom of the hydrogen storage cavity 29. An intake pipe is detachably connected to the hydrogen storage cavity 29 at the two hydrogen inlets. An intake check valve 34 is installed on the intake pipe. A hydrogen outlet is opened at the top of the hydrogen storage cavity 29. A hydrogen circulation main pipe 36 is detachably connected to the hydrogen storage cavity 29 at the hydrogen outlet. An outlet check valve 35 is installed on the hydrogen circulation main pipe 36. The hydrogen circulation main pipe 36 passes through and is rotatably connected to the floating plate 22 and the top of the main body 1 upwards in sequence. And the floating plate 22 slides along the axial direction of the hydrogen circulation main pipe 36. A gear one 37 is sleeved outside the hydrogen circulation main pipe 36 above the main body 1. The gear one 37 is meshed with a gear two 38. Above the gear two 38, a motor 39 is fixedly connected. The motor 39 is fixedly connected to the top of the main body 1 through an L-shaped connecting plate 58. The hydrogen circulation main pipe 36 is connected with a rotary joint 40 above the gear one 37. Above the rotary joint 40, a hydrogen circulation branch pipe 41 is connected.

[0036] As Figures 1-9 As shown, the hydrogen intake mechanism includes a pressure pump 42. The pressure pump 42 is fixedly connected to the bottom of the main body 1. The pressure pump 42 is provided with a gas outlet and two gas inlets. The two gas inlets of the pressure pump 42 are respectively connected to the hydrogen delivery branch pipe 3 and the hydrogen circulation branch pipe 41. The gas outlet of the pressure pump 42 is communicated with a hydrogen intake main pipe 43. The hydrogen intake main pipe 43 passes through the bottom of the main body 1. The outlet end of the hydrogen intake main pipe 43 is communicated with an intake pipe group. The intake pipe group includes an intake ring pipe one 44 and an intake ring pipe two 45. The intake ring pipe one 44, the intake ring pipe two 45 and the hydrogen intake main pipe 43 are communicated with each other through a plurality of intake branch pipes 46. Above the intake ring pipe one 44, the intake ring pipe two 45 and the plurality of intake branch pipes 46, a plurality of hydrogen spray heads 47 are arranged.

[0037] As Figures 1-9As shown in the figure, the stirring mechanism includes a stirring rod 48. The stirring rod 48 is arranged between the hydrogen storage cavity 29 and the intake pipe group. The upper end of the stirring rod 48 is fixedly connected to the bottom of the hydrogen storage cavity 29. Stirring blade groups 49 are arranged on the outer wall of the stirring rod 48 at different heights. Sieve plate assemblies are arranged between adjacent stirring blade groups 49. Each of the three sieve plate assemblies includes a sieve plate 50. Filling layers 51 are respectively fixedly connected to the upper and lower sides of the sieve plate 50. The sieve plate 50 and the two filling layers 51 are all fixedly connected to the inner wall of the main body 1. The stirring rod 48 passes through and is rotatably connected to the central positions of the sieve plate 50 and the two filling layers 51. As Figures 1-9 shown in the figure, the liquid material circulation mechanism includes a turbine pump 52. A liquid material circulation pipe 1 53 is connected to the inlet of the turbine pump 52. Two liquid material circulation pipes 2 54 are connected to the liquid material circulation pipe 1 53. A liquid material circulation pipe 3 55 is connected to the outlet of the turbine pump 52. Liquid material outlets are respectively opened on one side of the main body 1 above the three sieve plate assemblies. The three liquid material outlets are sequentially connected to the side of the liquid material circulation pipe 1 53 and the two liquid material circulation pipes 2 54 away from the turbine pump 52 from top to bottom. A liquid material inlet is opened below the three liquid material outlets of the main body 1. The liquid material inlet is arranged below the third sieve plate assembly from top to bottom. The liquid material inlet is connected to the side of the liquid material circulation pipe 3 55 away from the turbine pump 52.

[0038] In this embodiment, a temperature control system is arranged inside the main body 1; the hydrogen supply system is an existing system; the linear telescopic device 33 is a hydraulic cylinder, a pneumatic cylinder or an electric telescopic rod.

[0039] Working principle: Compound B, absolute ethanol and 5% palladium-carbon are added into the main body 1 from the material inlet 56. The motor 39 is started. After stirring evenly, the control valve on the hydrogen storage tank is opened. Hydrogen enters the hydrogen delivery main pipe 2. The hydrogen passes through the fan-shaped holes 19 on the support plate 8 and enters the hydrogen delivery branch pipe 3. Then, after being pressurized by the pressure pump 42, it passes through the hydrogen intake main pipe 43 and the intake pipe group in sequence, and finally sprays out from the hydrogen nozzle 47, contacts and reacts with the liquid material. The unreacted hydrogen rises above the liquid level after passing through the sieve plate assembly.

[0040] The two linear telescopic devices 33 are started. The push rods of the linear telescopic devices 33 are pushed out, driving the piston rod 31 to be pushed out. The hydrogen above the liquid level enters the hydrogen storage cavity 29 through the intake one-way valve 34. The push rods of the linear telescopic devices 33 are retracted, driving the piston rod 31 to be retracted. The hydrogen in the hydrogen storage cavity 29 enters the hydrogen circulation main pipe 36 through the outlet one-way valve 35, and further enters the pressure pump 42. The hydrogen is recycled for reaction again.

[0041] Start the turbo pump 52. The hydrogen and the liquid material above the three sieve plate assemblies respectively enter the turbo pump 52 through the first liquid material circulation pipe 53 and the two second liquid material circulation pipes 54, and then circulate to the bottommost part of the main body 1 through the third liquid material circulation pipe 55.

[0042] As the reaction proceeds, the consumption of hydrogen gradually decreases, and the air pressure inside the main body 1 gradually increases. The air pressure pushes the floating plate 22 to move upward, thereby driving the floating rod 23 to move upward, and the cylindrical external gear 6 rotates. By driving the transmission rod 5, the second bevel gear 10, the first bevel gear 9, the third bevel gear 11, the four fourth bevel gears 12, the four fifth bevel gears 14 and the four sixth bevel gears 17 rotate in sequence, thereby rotating the vertical rod 18 to drive the double-sector baffle 21 to rotate, reducing the hydrogen flow rate through the sector hole 19.

[0043] Example 7 Field efficacy test G5 is the diamide compound N-(2-bromo-4-(2-perfluoropropyl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-(N-methyl-4-fluoro-3,5-dichlorobenzamide) benzamide prepared in Example 5.

[0044] 1 Test basic information 1.1 Test name Test on the control of Spodoptera exigua in vegetables with pesticides.

[0045] 1.2 Test purpose To clarify the field control effect of the tested pesticides on Spodoptera exigua in corn and the safety test on corn.

[0046] 3 Test conditions 3.1 Test target and crop Test target: Spodoptera exigua; Test crop: Corn.

[0047] 3.2 Environmental conditions General situation of the test plot: The area is about 1 mu, and the adjacent plots around are planted with corn. The soil type of the test plot is sandy loam.

[0048] Test weather: During the test, there was no severe weather condition that affected the test. The specific weather conditions are shown in Table 1.

[0049] Table 1 Meteorological data table during the test 3.3 Agricultural operations and evaluation The planting amount per mu of corn in the test plot is 3000 plants / mu. At the time of pesticide application, it is in the seedling stage, the plant height is about 40 cm, the plant spacing is 30 cm, the soil at the base of the plant is covered with black plastic film, and the growth is complete but the leaves have been damaged by the larvae of Spodoptera exigua. During the test, normal water and fertilizer management was carried out.

[0050] 3.4 Instruments and Materials 3.4.1 Pesticide Application Equipment SX-MD16H electric sprayer, with a conical single nozzle, pressure of 2.4 Mpa, and flow rate of 1.2 L / Min.

[0051] 3.4.2 Other Instruments and Materials Test instruments such as 5 ml syringes, 20 ml syringes, 2000 ml and 5000 ml plastic measuring cylinders, ground stakes, plastic measuring cups, electronic scales, water buckets, tape measures, and marker pens.

[0052] 4 Test Methods 4.1 Test Design The test design and treatments are shown in Table 2, where EC represents the emulsifiable concentrate formulation.

[0053] Table 2 Test Design and Treatments The test has 7 treatments, with 3 replicates, for a total of 21 plots; the plot area is 15 m 2 ; the specific test field distribution map is shown in Table 3.

[0054] Table 3 Arrangement of Test Plots 4.3 Pesticide Application Method 4.3.1 Preparation of Pesticide Weigh the pesticides according to the dosages shown in Table 2 for each plot, dilute with water to form a liquid for spraying. Prepare and use immediately, and the preparation medium is irrigation water.

[0055] 4.3.2 Application Method Conventional foliar spraying. Conduct a water volume test before pesticide application, and it is qualified when water drips from the corn leaves.

[0056] 4.3.4 Application Rate 60 liters per mu.

[0057] 4.4 Investigation Method 4.4.1 Investigation Time and Frequency A total of 2 investigations are conducted: 3 days after pesticide application and 7 days after pesticide application.

[0058] 4.4.2 Investigation Method Observe the number of live larvae of Spodoptera exigua on the corn leaves of each treatment after pesticide application, calculate the mortality rate, and calculate the control efficacy.

[0059] 4.4.3 Impact on Crops No impact.

[0060] 4.4.4 Effects on Other Organisms No effect

[0061] 4.5 Pharmacodynamic Calculation and Evaluation Methods 4.5.1 Pharmacodynamic Calculation Formula The pharmacodynamic effect is calculated according to the following formula: .

[0062] 4.5.2 Data Statistics and Analysis Input the survey data into Microsoft Excel software for the calculation of the control effect; for multi-step calculations, no rounding is performed during the intermediate calculation process, and the final data is retained to two decimal places after the decimal point.

[0063] Use DPS (v9.50) statistical analysis software to conduct a significance analysis of the difference in the control effect by Duncan's new multiple range method.

[0064] 5 Test Results and Analysis Table 4 Original Data Sheet for the Investigation of Spodoptera exigua on Maize (3 days after treatment) Table 5 Original Data Sheet for the Investigation of Spodoptera exigua on Maize (7 days after treatment) Table 6 Control Effect Results of Tested Pesticides against Spodoptera exigua on Maize Three days after treatment, almost all Spodoptera exigua in Plot 3 were poisoned to death, and the control effects of G5 against Spodoptera exigua were all over 100%, with excellent effects; there were still some Spodoptera exigua that were not killed after being poisoned in Plots 1 and 2, and the control effects were 89.58% and 85.42% respectively, with average effects.

[0065] Seven days after treatment, no live Spodoptera exigua were found in Plot 3, and its control effect was up to 100%. The maize in the plot grew well, and no new symptoms of being eaten were found on the leaves, with excellent effects; there were more live Spodoptera exigua in Plots 1 and 2, the maize grew poorly, and many leaves had symptoms of being eaten and fresh feces, and the control effect was significantly lower than that of other treatments, with poor effects.

[0066] 6 Test Conclusions All the tested pesticides had no obvious adverse effects on maize and were safe for maize.

[0067] In this test, the quick-acting property and long-lasting period of 2% G5 EC against Spodoptera exigua on maize were both very excellent, and it was better than the control pesticide 2% broflanilide EC. The quick-acting property of Pesticides 1 and 2 against Spodoptera exigua on maize was poor and the dead insects were not complete, with poor effects.

[0068] In summary, it is recommended to use the medicament 2% G5 EC (the application dosage is 300 times dilution) for conventional foliar spraying to control Spodoptera exigua in corn, with a water consumption of 60 L per mu.

[0069] The above are only the preferred embodiments of the present invention, and are not limitations on the present invention in other forms. Any person skilled in the art may use the disclosed technical content to make changes or modifications into equivalent embodiments with equivalent changes and apply them to other fields. However, as long as it does not depart from the technical solution content of the present invention, any simple modification or equivalent change made to the above embodiments based on the technical essence of the present invention still falls within the protection scope of the technical solution of the present invention.

Claims

1. An intermediate preparation device for a diamide compound, characterized in that, It includes a main body (1), a hydrogen control mechanism, a hydrogen circulation mechanism, a hydrogen intake mechanism, a stirring mechanism, and a liquid material circulation mechanism; The hydrogen control mechanism is arranged above the main body (1), the hydrogen circulation mechanism is arranged above the interior of the main body (1), a stirring mechanism is arranged below the hydrogen circulation mechanism, the hydrogen intake mechanism is arranged below the main body (1), both the hydrogen control mechanism and the hydrogen circulation mechanism are communicated with the main body (1) through the hydrogen intake mechanism, the liquid material circulation mechanism is arranged on one side of the main body (1), and the liquid material circulation mechanism is communicated with the main body (1); A material inlet (56) is opened above the main body (1), a material outlet (57) is opened at the bottom of the main body (1), and plugs are detachably connected in both the material inlet (56) and the material outlet (57).

2. The intermediate preparation device of the diamide compound according to claim 1, characterized in that, The hydrogen control mechanism includes a main hydrogen delivery pipe (2), the main hydrogen delivery pipe (2) is externally connected to a hydrogen supply system, a hydrogen flow control component is arranged inside the main hydrogen delivery pipe (2), a hydrogen delivery branch pipe (3) is communicated with the side surface of the main hydrogen delivery pipe (2), a support (4) is fixedly connected to the bottom of the main hydrogen delivery pipe (2), the support (4) is fixedly connected to the top of the main body (1), one side of the main hydrogen delivery pipe (2) is rotationally connected with a transmission rod (5) through a bearing, a cylindrical external gear (6) is fixedly connected to the end of the transmission rod (5) on the outer side of the main hydrogen delivery pipe (2), the cylindrical external gear (6) is in transmission connection with a pneumatic floating component, and the transmission rod (5) is in transmission connection with the hydrogen flow control component.

3. The intermediate preparation device of the diamide compound according to claim 2, characterized in that, The hydrogen flow control component includes a support rod (7) and a support plate (8), the edge of the support plate (8) is fixedly connected to the inner wall of the main hydrogen delivery pipe (2), the bottom of the main hydrogen delivery pipe (2) is sealed, the lower end of the support rod (7) is rotationally connected to the bottom inside the main hydrogen delivery pipe (2) through a bearing, and the upper end of the support rod (7) is rotationally connected to the support plate (8) through a bearing; a first bevel gear (9) is sleeved below the support rod (7), the first bevel gear (9) is in transmission connection with a second bevel gear (10), the second bevel gear (10) is fixedly connected to one end of the transmission rod (5), a third bevel gear (11) is sleeved above the support rod (7), the third bevel gear (11) is in transmission connection with four fourth bevel gears (12), a rotating cross bar (13) is fixedly connected to the side of each of the four fourth bevel gears (12) away from the third bevel gear (11), a fifth bevel gear (14) is fixedly connected to the side of each of the four rotating cross bars (13) away from the fourth bevel gear (12), a limiting rod sleeve (15) is rotationally connected to the outer wall of each of the four rotating cross bars (13), the limiting rod sleeves (15) are fixedly connected to the inner wall of the main hydrogen delivery pipe (2) through an L-shaped bracket (16), each of the four fifth bevel gears (14) is in transmission connection with a sixth bevel gear (17), and a rotating vertical rod (18) is fixedly connected above each of the four sixth bevel gears (17); Eight sector holes (19) are formed in the support plate (8), and every two of the sector holes (19) correspond to each other. A limiting ring plate (20) is fixedly connected below each of the two corresponding sector holes (19) on the support plate (8). A rotating groove is formed on one side of each of the four limiting ring plates (20) close to the support plate (8). A double-sector baffle (21) is rotatably connected in each of the four rotating grooves. The central positions of the bottoms of the four double-sector baffles (21) are fixedly connected to the upper ends of four rotating vertical rods (18) respectively.

4. The intermediate preparation equipment of the diamide compound according to claim 2, characterized in that, The air pressure floating assembly includes a floating plate (22). The floating plate (22) is slidably connected above the interior of the main body (1). A sealing ring is arranged at the edge of the floating plate (22). A floating rod (23) is fixedly connected above the floating plate (22). The upper end of the floating rod (23) passes through and is slidably connected to the top of the main body (1). A plurality of teeth (24) are axially arranged above the main body (1) on the floating rod (23). The plurality of teeth (24) are meshed and connected with the cylindrical external gear (6); Two sliding rods (25) are fixedly connected above the floating plate (22). The upper ends of the two sliding rods (25) pass through and are slidably connected to the top of the main body (1). Limiting circular plates (26) are fixedly connected to the upper ends of the two sliding rods (25). A sealing cover (27) is arranged outside the two limiting circular plates (26). The bottoms of the two sealing covers (27) are fixedly connected to the top of the main body (1). Springs (28) are arranged between the top surfaces inside the two sealing covers (27) and the limiting circular plates (26).

5. The intermediate preparation device of the diamide compound according to claim 4, characterized in that, The hydrogen circulation mechanism includes a hydrogen storage cavity (29). The hydrogen storage cavity (29) is arranged below the floating plate (22) inside the main body (1). An air suction cylinder body (30) is communicated on each side of the hydrogen storage cavity (29). A piston rod (31) is arranged inside each of the two air suction cylinder bodies (30). One end of each of the two piston rods (31) passes through the air suction cylinder body (30) and is fixedly connected to a connecting plate (32). The other end of each of the two piston rods (31) is fixedly connected to a piston plate. Linear telescopic devices (33) are fixedly connected to the corresponding positions of the two air suction cylinder bodies (30) at the bottom of the hydrogen storage cavity (29). The push rods of the two linear telescopic devices (33) are fixedly connected to the connecting plate (32); The bottom of the hydrogen storage cavity (29) is provided with two hydrogen inlets. At each of the two hydrogen inlets of the hydrogen storage cavity (29), an intake pipe is detachably connected. An intake one-way valve (34) is installed on the intake pipe. The top of the hydrogen storage cavity (29) is provided with a hydrogen outlet. At the hydrogen outlet of the hydrogen storage cavity (29), a hydrogen circulation main pipe (36) is detachably connected. An outlet one-way valve (35) is installed on the hydrogen circulation main pipe (36). The hydrogen circulation main pipe (36) sequentially passes through and is rotatably connected to the floating plate (22) and the top of the main body (1) upward, and the floating plate (22) slides axially along the hydrogen circulation main pipe (36). A first gear (37) is sleeved outside the hydrogen circulation main pipe (36) above the main body (1). The first gear (37) is meshed with a second gear (38). Above the second gear (38), a motor (39) is fixedly connected. The motor (39) is fixedly connected to the top of the main body (1) through an L-shaped connecting plate (58). The hydrogen circulation main pipe (36) is connected with a rotary joint (40) above the first gear (37). Above the rotary joint (40), a hydrogen circulation branch pipe (41) is connected.

6. The intermediate preparation device of the diamide compound according to claim 2, characterized in that, The hydrogen intake mechanism includes a pressure pump (42). The pressure pump (42) is fixedly connected to the bottom of the main body (1). The pressure pump (42) is provided with a gas outlet and two gas inlets. The two gas inlets of the pressure pump (42) are respectively connected to the hydrogen delivery branch pipe (3) and the hydrogen circulation branch pipe (41). The gas outlet of the pressure pump (42) is communicated with a hydrogen intake main pipe (43). The hydrogen intake main pipe (43) passes through the bottom of the main body (1). The outlet end of the hydrogen intake main pipe (43) is communicated with an intake pipe group. The intake pipe group includes a first intake ring pipe (44) and a second intake ring pipe (45). The first intake ring pipe (44), the second intake ring pipe (45) and the hydrogen intake main pipe (43) are interconnected through a plurality of intake branch pipes (46). Above the first intake ring pipe (44), the second intake ring pipe (45) and the plurality of intake branch pipes (46), a plurality of hydrogen spray nozzles (47) are provided.

7. The intermediate preparation device of the diamide compound according to claim 5, characterized in that, The stirring mechanism includes a stirring rod (48). The stirring rod (48) is arranged between the hydrogen storage cavity (29) and the intake pipe group. The upper end of the stirring rod (48) is fixedly connected to the bottom of the hydrogen storage cavity (29). Stirring blade groups (49) are arranged on the outer wall of the stirring rod (48) at different heights. Sieve plate assemblies are arranged between adjacent stirring blade groups (49). Each of the three sieve plate assemblies includes a sieve plate (50). Filling layers (51) are respectively fixedly connected to the upper and lower sides of the sieve plate (50). The sieve plate (50) and the two filling layers (51) are fixedly connected to the inner wall of the main body (1). The stirring rod (48) passes through and is rotatably connected to the central positions of the sieve plate (50) and the two filling layers (51); The liquid material circulation mechanism includes a turbine pump (52). A first liquid material circulation pipe (53) is connected to the inlet of the turbine pump (52). Two second liquid material circulation pipes (54) are connected to the first liquid material circulation pipe (53). A third liquid material circulation pipe (55) is connected to the outlet of the turbine pump (52). On one side of the main body (1), liquid material outlets are respectively arranged above the three sieve plate assemblies. The three liquid material outlets are sequentially connected to the side of the first liquid material circulation pipe (53) and the two second liquid material circulation pipes (54) away from the turbine pump (52) from top to bottom. A liquid material inlet is arranged below the three liquid material outlets on the main body (1). The liquid material inlet is arranged below the third sieve plate assembly from top to bottom. The liquid material inlet is connected to the side of the third liquid material circulation pipe (55) away from the turbine pump (52).

8. A bisamide compound, characterized in that, The intermediate is prepared by using the preparation equipment for the intermediate of the bisamide compound described in Claims 1-7, and the specific structure is as follows: ； The chemical name is: N-(2-bromo-4-(perfluoropropan-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-(N-methyl-4-fluoro-3,5-dichlorobenzamide)benzamide.

9. A method for preparing a bisamide compound, characterized in that, To prepare the bisamide compound described in Claim 8, the specific preparation method is as follows: (1) 2-Fluoro-3-nitrobenzoic acid, a solvent, thionyl chloride and dimethylformamide are sequentially added into a reaction vessel. After stirring evenly, the temperature is raised for reaction. After the reaction is monitored by TLC and ends, vacuum distillation is carried out to obtain 2-fluoro-3-nitrobenzoyl chloride, which is Compound A. The reaction formula is: ； (2) The Compound A prepared in step (1) and a solvent are sequentially added into a reaction vessel. After stirring evenly, sodium bicarbonate and 2-trifluoromethyl-4-heptafluoroisopropyl-6-bromoaniline are added. Stir and raise the temperature for reaction. After the reaction is monitored by TLC and ends, first cool down, then add water for extraction and separation. The organic phase is evaporated to dryness to obtain N-(2-bromo-4-(perfluoropropan-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-nitrobenzamide, which is Compound B. The reaction formula is: ； (3) The Compound B prepared in step (2), a solvent and a catalyst are sequentially added into a reaction vessel. After stirring evenly, hydrogen gas is introduced. Stir and raise the temperature for reaction. After the reaction is monitored by TLC and ends, filter. The filtrate is evaporated to dryness to obtain 3-amino-N-(2-bromo-4-(perfluoropropan-2-yl)-6-(trifluoromethyl)phenyl)-2-fluorobenzamide, which is Compound C. The reaction formula is: ； (4) The Compound C prepared in step (3) is added into a reaction vessel, and then concentrated sulfuric acid is added. Stir until completely dissolved. An aqueous formaldehyde solution is slowly added dropwise under temperature control conditions. After the addition is completed, raise the temperature for reaction. After the reaction is monitored by TLC and ends, first cool down, then pour the reaction solution into ice water. Stir until all solids precipitate. Filter, wash the filter cake with water, and dry the filter cake to obtain N-(2-bromo-4-(perfluoropropan-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-(methylamino)benzamide, which is Compound D. The reaction formula is: ； (5) Add 3,5-dichloro-4-fluorobenzoyl chloride and a solvent into a reaction vessel in sequence. After stirring evenly, add the compound D prepared in step (4) in batches, then raise the temperature and carry out a reflux reaction. After monitoring the end of the reaction by TLC, cool down and filter. Wash the filter cake with a solvent and dry it to obtain the final product N-(2-bromo-4-(2,2,2-trifluoropropan-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-(N-methyl-4-fluoro-3,5-dichlorobenzamide)benzamide, which is the said diamide compound. The reaction formula is as follows: 。 10. Application of a diamide compound, characterized in that, Use the diamide compound described in claim 8 to prepare a pesticide composition. The said diamide compound is used as the main active ingredient of the pesticide composition, and the pesticide composition further comprises a formulation carrier or a formulation adjuvant; the pesticide composition is used as an insecticide to control crop pests or pest mites; the pesticide composition is used as a repellent to repel crop pests; the crop pests are Helicoverpa armigera or Spodoptera exigua.

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