A bisamide compound, a preparation method thereof, an intermediate preparation device and application thereof

Abstract

This invention belongs to the field of insecticide technology, specifically relating to a diamide compound, its preparation method, intermediate preparation equipment, and applications. The preparation method includes: reacting 2-fluoro-3-nitrobenzoic acid with thionyl chloride in the presence of dimethylformamide to generate compound A; condensing compound A with 2-trifluoromethyl-4-heptafluoroisopropyl-6-bromoaniline amide to obtain compound B; reducing compound B to obtain compound C; substituting compound C with formaldehyde to obtain compound D; and condensing compound D with 3,5-dichloro-4-fluorobenzoyl chloride to obtain the diamide compound. The beneficial effects of this invention are: the diamide compound solves the problem of insecticide resistance and possesses high insecticidal activity, exhibiting good insecticidal effect at low doses. Furthermore, the preparation method uses mild reaction conditions, produces few byproducts, and has a high reaction yield, reducing raw material loss and thus lowering production costs.

Description

Technical Field

[0001] This invention belongs to the field of insecticide technology, specifically relating to a diamide compound, its preparation method, intermediate preparation equipment, and applications. Background Technology

[0002] Diamide compounds have become an increasingly popular research focus for pesticide companies due to their unique mechanisms of action, novel targets, and environmental friendliness. While existing diamide compounds bring significant benefits to agricultural production, they also produce certain side effects. In specific pest control processes, long-term use of a single diamide compound can easily lead to varying degrees of resistance in pests. Furthermore, while existing diamide compounds possess insecticidal or acaricidal activity, their insecticidal efficacy is insufficient at low doses. Therefore, this paper proposes a diamide compound with high insecticidal activity that addresses the problem of pest resistance.

[0003] In the preparation of diamide compounds, this invention involves a reduction reaction using hydrogen as a raw material. Due to the rapid movement of hydrogen in the reaction solution and the short contact time between hydrogen and the substrate, the reaction efficiency is reduced. Furthermore, in order to ensure complete reaction of the substrate, an excess of hydrogen needs to be introduced, but a large amount of hydrogen does not participate in the reaction, resulting in low hydrogen utilization, which increases production costs and adds to the risk. Summary of the Invention

[0004] To address the aforementioned problems, this invention provides a diamide compound, its preparation method, intermediate preparation equipment, and applications.

[0005] This invention relates to an apparatus for preparing intermediates of 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 circulation mechanism;

[0006] The hydrogen control mechanism is located above the main body, the hydrogen circulation mechanism is located inside the main body, a stirring mechanism is located below the hydrogen circulation mechanism, the hydrogen inlet mechanism is located below the main body, the hydrogen control mechanism and the hydrogen circulation mechanism are both connected to the main body through the hydrogen inlet mechanism, and the liquid circulation mechanism is located on one side of the main body and is connected to the main body.

[0007] The main body has a material inlet at the top and a material outlet at the bottom. Both the material inlet and the material outlet can be detachably connected with plugs.

[0008] Preferably, the hydrogen control mechanism includes a main hydrogen delivery pipe connected to a hydrogen supply system, a hydrogen flow control component inside the main hydrogen delivery pipe, a hydrogen delivery branch pipe connected to the side of the main hydrogen delivery pipe, a support fixedly connected to the bottom of the main hydrogen delivery pipe, the support fixedly connected to the top of the main body, a transmission rod rotatably connected to one side of the main hydrogen delivery pipe via a bearing, a cylindrical external gear fixedly connected to the end of the transmission rod on the outer side of the main hydrogen delivery pipe, a pneumatic floating component being driven by the cylindrical external gear, and the transmission rod being driven by the hydrogen flow control component.

[0009] Preferably, the hydrogen flow control assembly includes a support rod and a support plate. The edge of the support plate is fixedly connected to the inner wall of the hydrogen delivery main pipe. The bottom of the hydrogen delivery main pipe is sealed. The lower end of the support rod is rotatably connected to the bottom of the hydrogen delivery main pipe via a bearing. The upper end of the support rod is rotatably connected to the support plate via a bearing. A bevel gear one is sleeved below the support rod. The bevel gear one is driven by a bevel gear two. The bevel gear two is fixedly connected to one end of a drive rod. A bevel gear three is sleeved above the support rod. The bevel gear three is driven by four bevel gears four. A rotating crossbar is fixedly connected to the side of each of the four bevel gears away from the bevel gear three. A bevel gear five is fixedly connected to the side of each of the four rotating crossbars away from the bevel gear four. A limiting rod sleeve is rotatably connected to the outer wall of each of the four rotating crossbars. The limiting rod sleeve is fixedly connected to the inner wall of the hydrogen delivery main pipe via an L-shaped bracket. A bevel gear six is ​​driven by each of the four bevel gears five. A rotating vertical rod is fixedly connected above each of the four bevel gears six.

[0010] The support plate has eight fan-shaped holes, with each pair of fan-shaped holes corresponding to each other. A limiting ring plate is fixedly connected to the support plate below each pair of corresponding fan-shaped holes. A rotating groove is provided on the side of each of the four limiting ring plates near the support plate. A double fan-shaped baffle is rotatably connected in each of the four rotating grooves. The bottom center of each of the four double fan-shaped baffles is fixedly connected to the upper end of the four rotating vertical rods.

[0011] Preferably, the pneumatic floating assembly includes a floating plate, which is slidably connected to the upper part of the main body. A sealing ring is provided on the edge of the floating plate. A floating rod is fixedly connected to the upper part of the floating plate. The upper end of the floating rod passes through and is slidably connected to the top of the main body. The floating rod has multiple teeth arranged axially above the main body. The multiple teeth are meshed with a cylindrical external gear.

[0012] Two sliding rods are fixedly connected above the floating plate. 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 to the limiting circular plates. Sealing covers are provided on the outer sides of the two limiting circular plates. The bottoms of the two sealing covers are fixedly connected to the top of the main body. Springs are provided between the top surface inside the two sealing covers and the limiting circular plates.

[0013] Preferably, the hydrogen circulation mechanism includes a hydrogen storage chamber disposed inside the main body below the floating plate. Both sides of the hydrogen storage chamber are connected to suction cylinders. Each suction cylinder contains a piston rod, one end of which passes through the suction cylinder and is fixedly connected to a connecting plate. The other end of the piston rod is fixedly connected to a piston plate. At the bottom of the hydrogen storage chamber, corresponding positions of the two suction cylinders are fixedly connected to linear telescopic devices, and the push rods of both linear telescopic devices are fixedly connected to the connecting plate.

[0014] The hydrogen storage chamber has two hydrogen inlets at its bottom, each detachably connected to an inlet pipe with an inlet check valve. The top of the hydrogen storage chamber has a hydrogen outlet, each detachably connected to a hydrogen circulation main pipe with an outlet check valve. The hydrogen circulation main pipe passes upwards and rotatably connects to a floating plate and the top of the main body. The floating plate slides axially along the hydrogen circulation main pipe. A gear one is fitted onto the outside of the hydrogen circulation main pipe above the main body, meshing with a gear two. A motor is fixedly connected above the gear two, and the motor is fixedly connected to the top of the main body via an L-shaped connecting plate. A rotating joint is connected above the gear one, and a hydrogen circulation branch pipe is connected above the rotating joint.

[0015] Preferably, the hydrogen intake mechanism includes a pressurizing pump, which is fixedly connected to the bottom of the main body. The pressurizing pump has a gas outlet and two gas inlets. The two gas inlets of the pressurizing pump are respectively connected to a hydrogen delivery branch pipe and a hydrogen circulation branch pipe. The gas outlet of the pressurizing pump is connected to a hydrogen intake main pipe, which passes through the bottom of the main body. The outlet end of the hydrogen intake main pipe is connected to an intake pipe assembly, which includes an intake ring pipe I and an intake ring pipe II. The intake ring pipe I, intake ring pipe II, and the hydrogen intake main pipe are interconnected through multiple intake branch pipes. Multiple hydrogen nozzles are provided above the intake ring pipe I, intake ring pipe II, and multiple intake branch pipes.

[0016] Preferably, the stirring mechanism includes a stirring rod disposed between the hydrogen storage chamber and the inlet pipe assembly. The upper end of the stirring rod is fixedly connected to the bottom of the hydrogen storage chamber. Stirring blades are arranged at different heights on the outer wall of the stirring rod. A sieve plate assembly is arranged between adjacent stirring blades. Each of the three sieve plate assemblies includes a sieve plate. Filling layers are fixedly connected to the upper and lower sides of the sieve plate, respectively. The sieve plate and the two filling layers are fixedly connected to the inner wall of the main body. The stirring rod passes through and is rotatably connected to the center position of the sieve plate and the two filling layers.

[0017] The liquid circulation mechanism includes a turbine pump. The inlet of the turbine pump is connected to a liquid circulation pipe one, and two liquid circulation pipes two are connected to the liquid circulation pipe one. The outlet of the turbine pump is connected to a liquid circulation pipe three. On one side of the main body, above three screen plate assemblies, liquid outlets are respectively opened. The three liquid outlets are connected from top to bottom to the side away from the turbine pump of the liquid circulation pipe one and the two liquid circulation pipes two. Below the three liquid outlets, the main body has a liquid inlet. The liquid inlet is located below the third screen plate assembly from top to bottom. The liquid inlet is connected to the side away from the turbine pump of the liquid circulation pipe three.

[0018] This invention also relates to a diamide compound, wherein the intermediate is prepared using the intermediate preparation equipment of the aforementioned diamide compound, and the specific structure is as follows:

[0019] ;

[0020] The chemical name is: N-(2-bromo-4-(perfluoropropane-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-(N-methyl-4-fluoro-3,5-dichlorobenzamide)benzamide.

[0021] This invention also relates to a method for preparing a diamide compound, wherein the preparation method specifically comprises:

[0022] (1) 2-fluoro-3-nitrobenzoic acid, solvent, thionyl chloride and dimethylformamide were added sequentially to the reaction vessel. After stirring evenly, the mixture was heated to react. After the reaction was monitored by TLC, the mixture was distilled under reduced pressure to obtain 2-fluoro-3-nitrobenzoyl chloride, which is compound A. The reaction formula is:

[0023] ;

[0024] (2) Compound A obtained in step (1) and solvent were added to the reaction vessel in sequence. After stirring evenly, sodium bicarbonate and 2-trifluoromethyl-4-heptafluoroisopropyl-6-bromoaniline were added. The mixture was stirred and heated. After the reaction was monitored by TLC, the temperature was lowered first, then water was added for extraction and separation. The organic phase was evaporated to dryness to obtain N-(2-bromo-4-(perfluoroprop-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-nitrobenzamide, which is compound B. The reaction formula is:

[0025] ;

[0026] (3) Add the compound B obtained in step (2), solvent and catalyst to the reaction vessel in sequence, stir evenly, then introduce hydrogen gas, stir and heat the reaction. After the reaction is completed by TLC monitoring, filter, and evaporate the filtrate to dryness to obtain 3-amino-N-(2-bromo-4-(perfluoroprop-2-yl)-6-(trifluoromethyl)phenyl)-2-fluorobenzamide, which is compound C. The reaction formula is:

[0027] ;

[0028] (4) Add compound C obtained in step (3) to the reaction vessel, then add concentrated sulfuric acid, stir until completely dissolved, and slowly add formaldehyde aqueous solution under controlled temperature. After the addition is complete, raise the temperature to react. After the reaction is completed by TLC monitoring, lower the temperature first, then pour the reaction solution into ice water, stir until all the solid precipitates, filter, wash the filter cake with water, and dry the filter cake to obtain N-(2-bromo-4-(perfluoroprop-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-(methylamino)benzamide, which is compound D. The reaction formula is:

[0029] ;

[0030] (5) Add 3,5-dichloro-4-fluorobenzoyl chloride and solvent to the reaction vessel in sequence, stir evenly, add compound D obtained in step (4) in batches, then heat and reflux the reaction. After the reaction is completed by TLC monitoring, cool down and filter. Wash the filter cake with solvent and dry to obtain the final product N-(2-bromo-4-(perfluoropropane-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-(N-methyl-4-fluoro-3,5-dichlorobenzamide)benzamide, which is the diamide compound. The reaction formula is:

[0031] .

[0032] Preferably, in step (1), the molar ratio of 2-fluoro-3-nitrobenzoic acid, thionyl chloride, and dimethylformamide is 1:1 to 1.1:0.01 to 0.1; the solvent is dichloromethane, and the mass ratio of 2-fluoro-3-nitrobenzoic acid to the solvent is 1:1 to 3; the temperature is raised to 60 to 100°C and the reaction is carried out for 4 to 8 hours.

[0033] In step (2), the molar ratio of 2-trifluoromethyl-4-heptafluoroisopropyl-6-bromoaniline, compound A, and sodium bicarbonate is 1:1 to 1.2:1 to 1.2; the solvent is dichloromethane, and the mass ratio of compound A to the solvent is 1:1 to 5; the temperature is raised to 50 to 90°C and reacted for 6 to 10 hours; the temperature is then lowered to 20 to 30°C.

[0034] In step (3), the molar ratio of compound B to catalyst is 1:0.005-0.01, the solvent is anhydrous ethanol, and the mass ratio of solvent to compound B is 1:2-4; the catalyst is 5% palladium on carbon, and the reaction is carried out at 30-35°C for 3-5 hours.

[0035] In step (4), the molar ratio of compound C, formaldehyde, and concentrated sulfuric acid is 1:2 to 6:1 to 1.2; the temperature is controlled at 30 to 35°C when adding the formaldehyde aqueous solution; the temperature is raised to 35 to 45°C and reacted for 10 to 12 hours; the temperature is lowered to 20 to 30°C; the mass ratio of compound C to ice water is 1:2 to 3.

[0036] In step (5), the molar ratio of compound D to 3,5-dichloro-4-fluorobenzoyl chloride is 1:1 to 1.1; the solvent is toluene, and the mass ratio of compound D to solvent is 1:2 to 5; the temperature is raised to 90 to 120°C and refluxed for 6 to 8 hours; the temperature is lowered to 20 to 30°C.

[0037] This invention also relates to the application of a diamide compound, using the diamide compound to prepare a pesticide composition, wherein the diamide compound is the main active ingredient of the pesticide composition, and the pesticide composition further includes a formulation carrier or 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 cotton bollworms or beet armyworms.

[0038] Compared with the prior art, the advantages and positive effects of the present invention are as follows:

[0039] (1) The intermediate preparation equipment for the diamide compound can control the amount of hydrogen added during the reaction through the hydrogen control mechanism, and can circulate the unreacted hydrogen back to the reaction liquid through the hydrogen circulation mechanism to continue to react with the substrate. At the same time, the unreacted hydrogen in the upper reaction liquid is circulated back to the bottom through the turbo pump, and the hydrogen rise rate is effectively reduced through the filling layer of the sieve plate assembly. Thus, the preparation equipment improves the utilization rate of hydrogen, effectively avoids the waste caused by excessive hydrogen, and reduces the production cost.

[0040] (2) The intermediate preparation equipment for the diamide compound increases the pressure of hydrogen entering the reaction liquid by pressurizing pump, which increases the solubility of hydrogen in the reaction liquid. The sieve plate of the sieve plate assembly improves the contact between hydrogen and substrate. At the same time, the reaction liquid in the turbo pump can increase the collision between hydrogen and substrate. The turbo pump solves the problem of uneven reaction liquid caused by the sieve plate assembly, thereby improving the reaction efficiency of the preparation equipment.

[0041] (3) The diamide compound solves the problem of insect resistance and has high insecticidal activity. It has good insecticidal effect at low doses. At the same time, the preparation method of the diamide compound has mild reaction conditions, few by-products, and high reaction yield, which reduces raw material loss and thus reduces production costs. Attached Figure Description

[0042] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the description of the embodiments will be briefly introduced below:

[0043] Figure 1 A schematic diagram of the apparatus for preparing the intermediate of the diamide compound provided in Example 6;

[0044] Figure 2 This is an internal structural diagram of the apparatus for preparing the intermediate of the diamide compound provided in Example 6;

[0045] Figure 3 This is an internal structural diagram of the hydrogen delivery main pipe provided in Example 6;

[0046] Figure 4 The bottom structure diagram of the hydrogen flow control assembly provided in Example 6;

[0047] Figure 5 A schematic diagram of the support plate provided in Example 6;

[0048] Figure 6 This is a schematic diagram of the double-fan-shaped baffle provided in Example 6;

[0049] Figure 7 Internal structure diagram of the sealing cover provided in Example 6;

[0050] Figure 8A schematic diagram of the intake manifold provided in Example 6;

[0051] Figure 9 This is a schematic diagram of the sieve plate assembly provided in Example 6.

[0052] Explanation of reference numerals in the attached figures:

[0053] 1. Main body; 2. Hydrogen delivery main pipe; 3. Hydrogen delivery branch pipe; 4. Support; 5. Transmission rod; 6. Cylindrical external gear; 7. Support rod; 8. Support plate; 9. Bevel gear one; 10. Bevel gear two; 11. Bevel gear three; 12. Bevel gear four; 13. Rotating crossbar; 14. Bevel gear five; 15. Limiting rod sleeve; 16. L-shaped bracket; 17. Bevel gear six; 18. Rotating vertical rod; 19. Sector-shaped hole; 20. Limiting ring plate; 21. Double sector-shaped baffle; 22. Floating plate; 23. Floating rod; 24. Gear; 25. Sliding rod; 26. Limiting circular plate; 27. Sealing cover; 28. Spring; 29. ​​Hydrogen storage chamber; 30. Intake cylinder; 31. Piston. 32. Rod, 33. Connecting plate, 34. Linear telescopic device, 35. Inlet check valve, 36. Outlet check valve, 37. Hydrogen circulation main pipe, 38. Gear 1, 39. Gear 2, 40. Motor, 41. Rotary joint, 42. Hydrogen circulation branch pipe, 43. Pressurizing pump, 44. Hydrogen inlet main pipe, 45. Inlet ring pipe 1, 46. Inlet ring pipe 2, 47. Inlet branch pipe, 48. Hydrogen nozzle, 49. Stirring rod, 50. Stirring blade assembly, 51. Screen plate, 52. Packing layer, 53. Turbine pump, 54. Material circulation pipe 1, 55. Material circulation pipe 2, 56. Material inlet, 57. Material outlet, 58. L-shaped connecting plate. Detailed Implementation

[0054] To better understand the above-mentioned objectives, features and advantages of the present invention, the present invention will be further described below in conjunction with embodiments and accompanying drawings.

[0055] Numerous specific details are set forth in the following description in order to provide a full understanding of the invention. However, the invention may also be practiced in other ways than those described herein, and therefore the invention is not limited to the specific embodiments disclosed in the following specification.

[0056] Example 1

[0057] Preparation of 2-fluoro-3-nitrobenzoyl chloride:

[0058]

[0059] 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 added sequentially to a reaction vessel. After stirring until homogeneous, the mixture was heated to 80 °C and reacted for 6 h. After the reaction was monitored by TLC, the mixture was distilled under reduced pressure until no fraction was obtained, yielding 975 g (4.8 mol) of 2-fluoro-3-nitrobenzoyl chloride (compound A), with a yield of 95.8% and a purity of 98.7%.

[0060] Example 2

[0061] Preparation of N-(2-bromo-4-(perfluoroprop-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-nitrobenzamide:

[0062]

[0063] 814.4 g (4 mol) of compound A prepared in Example 1 and 610 g of dichloromethane were added sequentially to a reaction vessel. After stirring until homogeneous, 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. The mixture was stirred and heated to 70 °C for 8 h. After the reaction was completed by TLC monitoring, the temperature was lowered to 25 °C, and then 1200 g of water was added for extraction and separation. The organic phase was evaporated to dryness to obtain 2275.2 g (3.96 mol) of N-(2-bromo-4-(perfluoropropyl-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 (400MHz, 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).

[0064] Example 3

[0065] Preparation of 3-amino-N-(2-bromo-4-(perfluoroprop-2-yl)-6-(trifluoromethyl)phenyl)-2-fluorobenzamide:

[0066]

[0067] 1725 g (3 mol) of compound B prepared in Example 2, 4500 g of anhydrous ethanol, and 51 g (0.024 mol) of 5% palladium on carbon were added sequentially to a reaction vessel. After stirring until homogeneous, hydrogen gas was introduced, and the mixture was stirred and heated to 35 °C for 4 h. After the reaction was completed by TLC monitoring, the mixture was filtered, and the filtrate was evaporated to dryness to obtain 1619.1 g (2.97 mol) of 3-amino-N-(2-bromo-4-(perfluoroprop-2-yl)-6-(trifluoromethyl)phenyl)-2-fluorobenzamide (compound C), with a yield of 99% and a purity of 98.9%. 1 H NMR (400MHz, DMSO) δ10.50(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).

[0068] Example 4

[0069] Preparation of N-(2-bromo-4-(perfluoroprop-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-(methylamino)benzamide:

[0070]

[0071] 1090.2 g (2 mol) of compound C prepared in Example 3 was added to the reaction vessel, followed by 215.8 g (2.2 mol) of concentrated sulfuric acid. The mixture was stirred until completely dissolved, and 450.4 g (6 mol) of 40% formaldehyde aqueous solution was slowly added dropwise under controlled temperature. After the addition was complete, the temperature was raised to 35 °C and the reaction was carried out for 12 h. After the reaction was completed by TLC monitoring, the temperature was lowered first, and then the reaction solution was poured into 440 g of ice water. The mixture was stirred until all the solid precipitated, filtered, 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 pale yellow solid, which is N-(2-bromo-4-(perfluoroprop-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 (400MHz, DMSO) δ10.53(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).

[0072] Example 5

[0073] Preparation of N-(2-bromo-4-(perfluoropropane-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-(N-methyl-4-fluoro-3-chlorobenzamide)benzamide:

[0074]

[0075] 250 g (1.1 mol) of 3,5-dichloro-4-fluorobenzoyl chloride and 1200 g of toluene were added sequentially to the reaction vessel. After thorough mixing, 560 g (1 mol) of compound D prepared in Example 4 was added in portions. The mixture was then heated to 100 °C and refluxed for 7 h. After the reaction was completed by TLC monitoring, the temperature was lowered to 25 °C, filtered, and the filter cake was washed with solvent and dried to obtain 736.7 g (0.98 mol) of the final product N-(2-bromo-4-(perfluoropropane-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-(N-methyl-4-fluoro-3,5-dichlorobenzamide)benzamide, which is the diamide compound, with a yield of 98.2% and a purity of 98.5%. ¹H NMR (400 MHz, DMSO) was also performed. δ10.67(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).

[0076] Example 6

[0077] like Figures 1-9 The apparatus shown is for preparing an intermediate of a diamide compound, comprising a main body 1, a hydrogen control mechanism, a hydrogen circulation mechanism, a hydrogen inlet mechanism, a stirring mechanism, and a feed liquid circulation mechanism.

[0078] like Figures 1-9 As shown, the hydrogen control mechanism is located above the main body 1, the hydrogen circulation mechanism is located above the main body 1, the stirring mechanism is located below the hydrogen circulation mechanism, the hydrogen inlet mechanism is located below the main body 1, the hydrogen control mechanism and the hydrogen circulation mechanism are both connected to the main body 1 through the hydrogen inlet mechanism, the liquid circulation mechanism is located on one side of the main body 1, and the liquid circulation mechanism is connected to the main body 1.

[0079] like Figures 1-9 As shown, a material inlet 56 is provided at the top of the main body 1, and a material outlet 57 is provided at the bottom of the main body 1. Both the material inlet 56 and the material outlet 57 can be detachably connected with plugs.

[0080] like Figures 1-9 As shown, the hydrogen control mechanism includes a main hydrogen delivery pipe 2, which is externally connected to a hydrogen supply system. A hydrogen flow control component is installed inside the main hydrogen delivery pipe 2. A hydrogen delivery branch pipe 3 is connected to the side of the main hydrogen delivery pipe 2. A support 4 is fixedly connected to the bottom of the main hydrogen delivery pipe 2 and is fixedly connected to the top of the main body 1. A transmission rod 5 is rotatably connected to one side of the main hydrogen delivery pipe 2 via 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 driven by a pneumatic floating component. The transmission rod 5 is driven by the hydrogen flow control component.

[0081] like Figures 1-9 As shown, the hydrogen flow control assembly 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 hydrogen delivery main pipe 2. The bottom of the hydrogen delivery main pipe 2 is sealed. The lower end of the support rod 7 is rotatably connected to the bottom of the hydrogen delivery main pipe 2 via a bearing, and the upper end of the support rod 7 is rotatably connected to the support plate 8 via a bearing. A bevel gear 9 is sleeved below the support rod 7, and a bevel gear 10 is driven by the bevel gear 9. The bevel gear 10 is fixedly connected to one end of the transmission rod 5. A bevel gear 11 is sleeved above the support rod 7. 11. Four bevel gears 12 are connected to the transmission. A rotating crossbar 13 is fixedly connected to the side of each of the four bevel gears 12 away from the side of each of the four bevel gears 12. A bevel gear 14 is fixedly connected to the side of each of the four rotating crossbars 13 away from the side of each of the four bevel gears 12. A limiting sleeve 15 is rotatably connected to the outer wall of each of the four rotating crossbars 13. The limiting sleeves 15 are fixedly connected to the inner wall of the hydrogen transmission main pipe 2 through L-shaped brackets 16. A bevel gear 17 is connected to each of the four bevel gears 14. A rotating vertical rod 18 is fixedly connected above each of the four bevel gears 17.

[0082] like Figures 1-9 As shown, the support plate 8 has eight fan-shaped holes 19, with each pair of fan-shaped holes 19 corresponding to each other. The support plate 8 is fixedly connected to a limiting ring plate 20 below each of the two corresponding fan-shaped holes 19. Each of the four limiting ring plates 20 has a rotating groove on the side near the support plate 8. Each of the four rotating grooves is rotatably connected to a double fan-shaped baffle 21. The bottom center of each of the four double fan-shaped baffles 21 is fixedly connected to the upper end of the four rotating vertical rods 18.

[0083] like Figures 1-9 As shown, the pneumatic floating assembly includes a floating plate 22, which is slidably connected to the upper part of the main body 1. A sealing ring is provided on the edge of the floating plate 22. A floating rod 23 is fixedly connected to the upper part of 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. The floating rod 23 has multiple teeth 24 arranged axially above the main body 1. The multiple teeth 24 mesh with the cylindrical external gear 6.

[0084] like Figures 1-9 As shown, 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. The upper ends of the two sliding rods 25 are fixedly connected to the limiting circular plates 26. Sealing covers 27 are provided on the outside of the two limiting circular plates 26. The bottom of the two sealing covers 27 are fixedly connected to the top of the main body 1. Springs 28 are provided between the top surface of the inside of the two sealing covers 27 and the limiting circular plates 26.

[0085] like Figures 1-9As shown, the hydrogen circulation mechanism includes a hydrogen storage chamber 29, which is located inside the main body 1 below the floating plate 22. Both sides of the hydrogen storage chamber 29 are connected to suction cylinders 30. Each suction cylinder 30 has a piston rod 31 inside. One end of each piston rod 31 passes through the suction cylinder 30 and is fixedly connected to a connecting plate 32. The other end of each piston rod 31 is fixedly connected to a piston plate. At the bottom of the hydrogen storage chamber 29, at the corresponding positions of the two suction cylinders 30, linear telescopic devices 33 are fixedly connected. The push rods of the two linear telescopic devices 33 are fixedly connected to the connecting plate 32.

[0086] like Figures 1-9 As shown, the hydrogen storage chamber 29 has two hydrogen inlets at its bottom. Each hydrogen inlet is detachably connected to an inlet pipe, and an inlet check valve 34 is installed on the inlet pipe. The top of the hydrogen storage chamber 29 has a hydrogen outlet, and a hydrogen circulation main pipe 36 is detachably connected to each hydrogen outlet. An outlet check valve 35 is installed on the hydrogen circulation main pipe 36. The hydrogen circulation main pipe 36 passes upwards and is rotatably connected to the floating plate 22 and the top of the main body 1. The floating plate 22 slides along the axial direction of the hydrogen circulation main pipe 36. A gear 37 is sleeved on the outside of the hydrogen circulation main pipe 36 above the main body 1. Gear 37 meshes with a gear 38. A motor 39 is fixedly connected above gear 38. The motor 39 is fixedly connected to the top of the main body 1 via an L-shaped connecting plate 58. A rotating joint 40 is connected above gear 37 on the hydrogen circulation main pipe 36, and a hydrogen circulation branch pipe 41 is connected above the rotating joint 40.

[0087] like Figures 1-9 As shown, the hydrogen intake mechanism includes a pressurizing pump 42, which is fixedly connected to the bottom of the main body 1. The pressurizing pump 42 is provided with a gas outlet and two gas inlets. The two gas inlets of the pressurizing pump 42 are respectively connected to the hydrogen delivery branch pipe 3 and the hydrogen circulation branch pipe 41. The gas outlet of the pressurizing pump 42 is connected to the hydrogen intake main pipe 43, which passes through the bottom of the main body 1. The outlet end of the hydrogen intake main pipe 43 is connected to the intake pipe group, which includes an intake ring pipe 1 44 and an intake ring pipe 2 45. The intake ring pipe 1 44, the intake ring pipe 2 45 and the hydrogen intake main pipe 43 are interconnected through multiple intake branch pipes 46. Multiple hydrogen nozzles 47 are provided above the intake ring pipe 1 44, the intake ring pipe 2 45 and the multiple intake branch pipes 46.

[0088] like Figures 1-9As shown, the stirring mechanism includes a stirring rod 48, which is disposed between the hydrogen storage chamber 29 and the inlet pipe assembly. The upper end of the stirring rod 48 is fixedly connected to the bottom of the hydrogen storage chamber 29. Stirring blades 49 are provided at different heights on the outer wall of the stirring rod 48. A sieve plate assembly is provided between adjacent stirring blades 49. Each of the three sieve plate assemblies includes a sieve plate 50. Filling layers 51 are fixedly connected to the upper and lower sides of the sieve plate 50, respectively. 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 center position of the sieve plate 50 and the two filling layers 51.

[0089] like Figures 1-9 As shown, the liquid circulation mechanism includes a turbine pump 52, a liquid circulation pipe 53 connected to the inlet of the turbine pump 52, two liquid circulation pipes 54 connected to the liquid circulation pipe 53, and a liquid circulation pipe 55 connected to the outlet of the turbine pump 52. A liquid outlet is provided on one side of the main body 1 above the three screen plate assemblies. The three liquid outlets are connected from top to bottom to the side of the liquid circulation pipe 53 and the two liquid circulation pipes 54 away from the turbine pump 52. A liquid inlet is provided below the three liquid outlets of the main body 1. The liquid inlet is located below the third screen plate assembly from top to bottom. The liquid inlet is connected to the side of the liquid circulation pipe 55 away from the turbine pump 52.

[0090] In this embodiment, the main body 1 is equipped with a temperature control system; the hydrogen supply system is an existing system; and the linear telescopic device 33 is a hydraulic cylinder, a pneumatic cylinder, or an electric telescopic rod.

[0091] Working principle:

[0092] Compound B, anhydrous ethanol, and 5% palladium on carbon are added to the main body 1 through material inlet 56. The motor 39 is turned on, and after stirring evenly, the control valve on the hydrogen storage tank is opened, and hydrogen enters the hydrogen delivery main pipe 2. The hydrogen enters the hydrogen delivery branch pipe 3 through the fan-shaped hole 19 on the support plate 8, and then is pressurized by the pressurizing pump 42. After passing through the hydrogen inlet main pipe 43 and the inlet pipe assembly in sequence, it is finally sprayed out from the hydrogen nozzle 47, comes into contact with the liquid and reacts. The unreacted hydrogen rises above the liquid surface after passing through the sieve plate assembly.

[0093] When the two linear telescopic devices 33 are activated, the push rods of the linear telescopic devices 33 extend, driving the piston rod 31 to extend. The hydrogen above the liquid level enters the hydrogen storage chamber 29 through the inlet check valve 34. When the push rods of the linear telescopic devices 33 retract, the piston rod 31 retracts. The hydrogen in the hydrogen storage chamber 29 enters the hydrogen circulation main pipe 36 through the outlet check valve 35, and further enters the pressurization pump 42, where the hydrogen is circulated again for reaction.

[0094] Turn on the turbine pump 52. The hydrogen and liquid in the upper part of the three sieve plate assemblies enter the turbine pump 52 through the first liquid circulation pipe 53 and the two second liquid circulation pipes 54, respectively, and then circulate to the bottom of the main body 1 through the third liquid circulation pipe 55.

[0095] As the reaction proceeds, the consumption of hydrogen gradually decreases, and the gas pressure inside the main body 1 gradually increases. The gas pressure pushes the floating plate 22 upward, thereby driving the floating rod 23 upward. The cylindrical external gear 6 rotates, which in turn drives the transmission rod 5 to drive the bevel gears 10, 9, 11, 12, 14, and 17 in sequence to rotate. This, in turn, rotates the vertical rod 18, causing the double sector baffle 21 to rotate, reducing the flow rate of hydrogen through the sector orifice 19.

[0096] Example 7

[0097] Field efficacy trials

[0098] G5 is the diamide compound N-(2-bromo-4-(perfluoropropane-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-(N-methyl-4-fluoro-3,5-dichlorobenzamide)benzamide prepared in Example 5.

[0099] 1. Basic Information of the Experiment

[0100] 1.1 Test Name

[0101] Experiment on chemical control of beet armyworm on vegetables.

[0102] 1.2 Experimental Objective

[0103] To clarify the field control efficacy of the tested pesticide against the beet armyworm in corn and to test its safety in corn.

[0104] 3. Test conditions

[0105] 3.1 Experimental Targets and Crops

[0106] Experimental target: beet armyworm;

[0107] Experimental crop: maize.

[0108] 3.2 Environmental Conditions

[0109] Experimental site overview: The site covers an area of ​​approximately 1 acre, with adjacent plots planted with corn. The soil type of the experimental site is sandy loam.

[0110] Test weather: No severe weather conditions that would have affected the test occurred during the test period. Specific weather conditions are shown in Table 1.

[0111] Table 1 Meteorological data during the experiment

[0112]

[0113] 3.3 Agricultural Operations and Evaluation

[0114] The experimental corn planting density was 3000 plants per mu (approximately 0.067 hectares). The plants were in the seedling stage at the time of pesticide application, with a plant height of approximately 40 cm and a plant spacing of 30 cm. The soil around the base of the plants was covered with black mulch. The plants appeared healthy, but their leaves had already been damaged by beet armyworm larvae. Normal water and fertilizer management was maintained throughout the experiment.

[0115] 3.4 Instruments and Materials

[0116] 3.4.1 Application equipment

[0117] The SX-MD16H electric sprayer features a single conical nozzle, a pressure of 2.4 MPa, and a flow rate of 1.2 L / min.

[0118] 3.4.2 Other Instruments and Materials

[0119] 5ml syringes, 20ml syringes, 2000ml and 5000ml plastic graduated cylinders and insert signs, plastic measuring cups, electronic scales, buckets, measuring tapes, markers and other testing equipment.

[0120] 4. Test Methods

[0121] 4.1 Experimental Design

[0122] The experimental design and treatment are shown in Table 2, where EC represents the emulsifiable concentrate formulation.

[0123] Table 2 Experimental Design and Treatment

[0124]

[0125] The experiment consisted of 7 treatments, 3 replicates, and a total of 21 plots; the plot area was 15m². 2 The specific field distribution map for the experiments is shown in Table 3.

[0126] Table 3 Layout of test plots

[0127]

[0128] 4.3 Application Method

[0129] 4.3.1 Preparation of Pharmaceuticals

[0130] Weigh the pesticide according to the dosage shown in Table 2, convert it to the dosage for each plot, dilute it with water to form a spray solution, and use it immediately after preparation for preparing the irrigation medium.

[0131] 4.3.2 Application Method

[0132] For conventional foliar spraying, a water volume test should be conducted before application, with the condition being that water drips from the corn leaves.

[0133] 4.3.4 Usage Capacity

[0134] 60 liters per mu.

[0135] 4.4 Survey Methods

[0136] 4.4.1 Survey Time and Frequency

[0137] The study was conducted twice: 3 days and 7 days after medication.

[0138] 4.4.2 Survey Methodology

[0139] After applying the pesticide, observe the number of live beet armyworm larvae on corn leaves in each treatment, calculate the mortality rate, and calculate the control efficacy.

[0140] 4.4.3 Impact on crops

[0141] No impact.

[0142] 4.4.4 Impact on other organisms

[0143] No impact.

[0144] 4.5 Methods for Calculating and Efficacy

[0145] 4.5.1 Formula for Calculating Drug Efficacy

[0146] The efficacy of the drug is calculated using the following formula:

[0147] .

[0148] 4.5.2 Data Statistics and Analysis

[0149] Input the survey data into Microsoft Excel software to calculate the prevention and control effect; since it involves multiple calculation steps, no rounding is performed in the intermediate calculation process, and the final data is retained to two decimal places.

[0150] The Duncan-style new multiple range method was used to analyze the significance of differences in the control effects using DPS (v9.50) statistical analysis software.

[0151] 5. Experimental Results and Analysis

[0152] Table 4. Raw data from the survey of the beet leaf moth on corn (3 days after pesticide application)

[0153]

[0154] Table 5. Raw data from the survey of the beet leaf moth on corn (7 days after pesticide application)

[0155]

[0156] Table 6. Control efficacy of the tested pesticides against the corn beet armyworm.

[0157]

[0158] Three days after application, almost all beet armyworms in the three treatment plots died from poisoning. G5 showed excellent control efficacy against beet armyworms, with a control efficacy of over 100%. In the two treatment plots, some beet armyworms survived the poisoning, with control efficiencies of 89.58% and 85.42% respectively, indicating only moderate efficacy.

[0159] Seven days after application, no live beet armyworms were found in treatment 3, with a control efficacy of 100%. The corn in the treatment area grew well, and no new symptoms of leaf feeding were observed, indicating excellent results. In treatments 1 and 2, the number of live beet armyworms was relatively high, the corn growth was poor, and many leaves showed symptoms of feeding and fresh excrement. The control efficacy was significantly lower than other treatments, indicating poor results.

[0160] 6. Experimental Conclusions

[0161] None of the tested agents had significant adverse effects on corn and were safe for corn.

[0162] In this experiment, 2% G5 EC showed excellent rapid and sustained efficacy against the beet armyworm, superior to the control agent 2% bromonitrile dimethoate EC. Agents 1 and 2 showed poor rapid efficacy against the beet armyworm and incomplete kill of the insects, resulting in poor overall effectiveness.

[0163] In summary, it is recommended to use 2% G5 EC (300 times dilution) as a routine foliar spray to control the beet armyworm in corn, with a water volume of 60L / mu.

[0164] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any other way. Any person skilled in the art may make changes or modifications to the above-disclosed technical content to create equivalent embodiments that can be applied to other fields. However, any simple modifications or equivalent changes made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the protection scope of the present invention.

Claims

1. An apparatus for preparing an intermediate of a diamide compound, characterized in that, It includes the main body (1), hydrogen control mechanism, hydrogen circulation mechanism, hydrogen inlet mechanism, stirring mechanism and liquid circulation mechanism; The hydrogen control mechanism is located above the main body (1), the hydrogen circulation mechanism is located above the main body (1), a stirring mechanism is located below the hydrogen circulation mechanism, the hydrogen inlet mechanism is located below the main body (1), the hydrogen control mechanism and the hydrogen circulation mechanism are both connected to the main body (1) through the hydrogen inlet mechanism, the liquid circulation mechanism is located on one side of the main body (1), and the liquid circulation mechanism is connected to the main body (1); The main body (1) has a material inlet (56) at the top and a material outlet (57) at the bottom. Both the material inlet (56) and the material outlet (57) can be detachably connected with plugs. The hydrogen control mechanism includes a hydrogen delivery main pipe (2), which is connected to a hydrogen supply system. A hydrogen flow control component is installed inside the hydrogen delivery main pipe (2). A hydrogen delivery branch pipe (3) is connected to the side of the hydrogen delivery main pipe (2). A support (4) is fixedly connected to the bottom of the hydrogen delivery main pipe (2). The support (4) is fixedly connected to the top of the main body (1). A transmission rod (5) is rotatably connected to one side of the hydrogen delivery main pipe (2) through a bearing. A cylindrical external gear (6) is fixedly connected to the end of the transmission rod (5) on the outside side of the hydrogen delivery main pipe (2). A pneumatic floating component is driven by the cylindrical external gear (6). The transmission rod (5) is driven by the hydrogen flow control component. The hydrogen flow control assembly 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 hydrogen delivery main pipe (2). The bottom of the hydrogen delivery main pipe (2) is sealed. The lower end of the support rod (7) is rotatably connected to the bottom of the hydrogen delivery main pipe (2) through a bearing. The upper end of the support rod (7) is rotatably connected to the support plate (8) through a bearing. A bevel gear one (9) is sleeved below the support rod (7). The bevel gear one (9) is driven by a bevel gear two (10). The bevel gear two (10) is fixedly connected to one end of the transmission rod (5). A bevel gear three (11) is sleeved above the support rod (7). Gear 3 (11) is connected to four bevel gears 4 (12). Each of the four bevel gears 4 (12) is fixedly connected to a rotating crossbar (13) on the side away from bevel gear 3 (11). Each of the four rotating crossbars (13) is fixedly connected to a bevel gear 5 (14) on the side away from bevel gear 4 (12). Each of the four rotating crossbars (13) is rotatably connected to a limiting sleeve (15). Each of the limiting sleeves (15) is fixedly connected to the inner wall of the hydrogen conveying main pipe (2) through an L-shaped bracket (16). Each of the four bevel gears 5 (14) is connected to a bevel gear 6 (17). Each of the four bevel gears 6 (17) is fixedly connected to a rotating vertical rod (18) above it. The support plate (8) has eight fan-shaped holes (19), with each pair of fan-shaped holes (19) corresponding to each other. The support plate (8) is fixedly connected to a limiting ring plate (20) below each of the two corresponding fan-shaped holes (19). Each of the four limiting ring plates (20) has a rotating groove on the side near the support plate (8). Each of the four rotating grooves is rotatably connected to a double fan-shaped baffle (21). The bottom center of each of the four double fan-shaped baffles (21) is fixedly connected to the upper end of the four rotating vertical rods (18). The pneumatic floating assembly includes a floating plate (22), which is slidably connected to the upper part of the main body (1). A sealing ring is provided on the edge of the floating plate (22). A floating rod (23) is fixedly connected to the upper part of 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). The floating rod (23) has multiple teeth (24) arranged axially above the main body (1). The multiple teeth (24) mesh 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). The upper ends of the two sliding rods (25) are fixedly connected to the limiting circular plate (26). A sealing cover (27) is provided on the outside of the two limiting circular plates (26). The bottom of the two sealing covers (27) is fixedly connected to the top of the main body (1). A spring (28) is provided between the top surface inside the two sealing covers (27) and the limiting circular plate (26).

2. The apparatus for preparing intermediates of the diamide compound according to claim 1, characterized in that, The hydrogen circulation mechanism includes a hydrogen storage chamber (29), which is located inside the main body (1) below the floating plate (22). Both sides of the hydrogen storage chamber (29) are connected to suction cylinders (30). Both suction cylinders (30) are equipped with piston rods (31). One end of each piston rod (31) passes through the suction cylinder (30) and is fixedly connected to a first connecting plate (32). The other end of each piston rod (31) is fixedly connected to a piston plate. At the bottom of the hydrogen storage chamber (29), linear telescopic devices (33) are fixedly connected at corresponding positions of the two suction cylinders (30). The push rods of the two linear telescopic devices (33) are fixedly connected to the first connecting plate (32). The hydrogen storage chamber (29) has two hydrogen inlets at its bottom. Each hydrogen inlet is detachably connected to an inlet pipe, and an inlet check valve (34) is installed on the inlet pipe. The hydrogen storage chamber (29) has a hydrogen outlet at its top, and a hydrogen circulation main pipe (36) is detachably connected to the hydrogen outlet. An outlet check valve (35) is installed on the hydrogen circulation main pipe (36). The hydrogen circulation main pipe (36) passes upwards and is rotatably connected to the floating plate (22) and the top of the main body (1). Furthermore, the floating plate (22) slides along the axial direction of the hydrogen circulation main pipe (36), and a gear one (37) is sleeved on the outside of the hydrogen circulation main pipe (36) above the main body (1). The gear one (37) is meshed with a gear two (38), and a motor (39) is fixedly connected above the gear two (38). The motor (39) is fixedly connected to the main body (1) through an L-shaped connecting plate (58). A rotating joint (40) is connected above the gear one (37) of the hydrogen circulation main pipe (36), and a hydrogen circulation branch pipe (41) is connected above the rotating joint (40).

3. The apparatus for preparing intermediates of the diamide compound according to claim 1, characterized in that, The hydrogen intake mechanism includes a pressurizing pump (42), which is fixedly connected to the bottom of the main body (1). The pressurizing pump (42) is provided with a gas outlet and two gas inlets. The two gas inlets of the pressurizing pump (42) are respectively connected to the hydrogen delivery branch pipe (3) and the hydrogen circulation branch pipe (41). The gas outlet of the pressurizing pump (42) is connected to the hydrogen intake main pipe (43), which passes through the main body (1). At the bottom, the outlet end of the hydrogen inlet main pipe (43) is connected to an inlet pipe group, which includes an inlet ring pipe one (44) and an inlet ring pipe two (45). The inlet ring pipe one (44), the inlet ring pipe two (45) and the hydrogen inlet main pipe (43) are interconnected through multiple inlet branch pipes (46). Multiple hydrogen nozzles (47) are provided above the inlet ring pipe one (44), the inlet ring pipe two (45) and the multiple inlet branch pipes (46).

4. The apparatus for preparing intermediates of diamide compounds according to claim 2, characterized in that, The stirring mechanism includes a stirring rod (48), which is disposed between the hydrogen storage chamber (29) and the inlet pipe assembly. The upper end of the stirring rod (48) is fixedly connected to the bottom of the hydrogen storage chamber (29). The outer wall of the stirring rod (48) is provided with stirring blade groups (49) at different heights. A sieve plate assembly is provided between adjacent stirring blade groups (49). Each of the three sieve plate assemblies includes a sieve plate (50). A filling layer (51) is 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 center position of the sieve plate (50) and the two filling layers (51). The liquid circulation mechanism includes a turbine pump (52), a liquid circulation pipe 1 (53) connected to the inlet of the turbine pump (52), two liquid circulation pipes 2 (54) connected to the liquid circulation pipe 1 (53), and a liquid circulation pipe 3 (55) connected to the outlet of the turbine pump (52). The main body (1) has a liquid outlet on one side above the three sieve plate assemblies. The three liquid outlets are connected from top to bottom to the side of the liquid circulation pipe 1 (53) and the two liquid circulation pipes 2 (54) away from the turbine pump (52). The main body (1) has a liquid inlet below the three liquid outlets. The liquid inlet is located below the third sieve plate assembly from top to bottom. The liquid inlet is connected to the side of the liquid circulation pipe 3 (55) away from the turbine pump (52).

5. A method for preparing a diamide compound, characterized in that, The diamide compound is prepared using the intermediate preparation apparatus for the diamide compound according to any one of claims 1-4, wherein the preparation method specifically comprises: (1) 2-fluoro-3-nitrobenzoic acid, solvent, thionyl chloride and dimethylformamide were added sequentially to the reaction vessel. After stirring evenly, the mixture was heated to react. After the reaction was monitored by TLC, the mixture was distilled under reduced pressure to obtain 2-fluoro-3-nitrobenzoyl chloride, which is compound A. The reaction formula is: ； (2) Compound A obtained in step (1) and solvent were added to the reaction vessel in sequence. After stirring evenly, sodium bicarbonate and 2-trifluoromethyl-4-heptafluoroisopropyl-6-bromoaniline were added. The mixture was stirred and heated. After the reaction was monitored by TLC, the temperature was lowered first, then water was added for extraction and separation. The organic phase was evaporated to dryness to obtain N-(2-bromo-4-(perfluoroprop-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-nitrobenzamide, which is compound B. The reaction formula is: ； (3) Add the compound B obtained in step (2), solvent and catalyst to the reaction vessel in sequence, stir evenly, then introduce hydrogen gas, stir and heat the reaction. After the reaction is completed by TLC monitoring, filter, and evaporate the filtrate to dryness to obtain 3-amino-N-(2-bromo-4-(perfluoroprop-2-yl)-6-(trifluoromethyl)phenyl)-2-fluorobenzamide, which is compound C. The reaction formula is: ； (4) Add compound C obtained in step (3) to the reaction vessel, then add concentrated sulfuric acid, stir until completely dissolved, and slowly add formaldehyde aqueous solution under controlled temperature. After the addition is complete, raise the temperature to react. After the reaction is completed by TLC monitoring, lower the temperature first, then pour the reaction solution into ice water, stir until all the solid precipitates, filter, wash the filter cake with water, and dry the filter cake to obtain N-(2-bromo-4-(perfluoroprop-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 solvent to the reaction vessel in sequence, stir evenly, add compound D obtained in step (4) in batches, then heat and reflux the reaction. After the reaction is completed by TLC monitoring, cool down and filter. Wash the filter cake with solvent and dry to obtain the final product N-(2-bromo-4-(perfluoropropane-2-yl)-6-(trifluoromethyl)phenyl)-2-fluoro-3-(N-methyl-4-fluoro-3,5-dichlorobenzamide)benzamide, which is the diamide compound. The reaction formula is: 。

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