High-safety pyrazoline oxidation reaction device

Abstract

The invention discloses a high-safety pyrazoline oxidation reaction device, and relates to the technical field of oxidation reaction devices, the high-safety pyrazoline oxidation reaction device comprises a shell and a heat conduction oil circulation temperature control assembly, and the side surface of the outer wall of the shell is connected with the heat conduction oil circulation temperature control assembly; the heat conduction oil circulation temperature control assembly comprises an oil outlet upper connector, an oil outlet lower connector, an oil outlet pipe, a circulation temperature control pump, an oil inlet pipe and an oil inlet connector. According to the present invention, by installing the heat conduction oil circulation temperature control assembly, the accurate control of the reaction temperature is achieved, the heat conduction oil temperature is adjusted in real time, the reaction temperature is stably controlled in the target interval, the abnormal reaction caused by the temperature fluctuation is avoided, and the temperature stability and the safety of the reaction system are maintained.

Description

Technical Field

[0001] The present invention relates to the technical field of oxidation reaction devices, and specifically to a pyrazoline oxidation reaction device with high safety. Background Art

[0002] In the industrial synthesis of the pesticide active ingredient chlorantraniliprole, 3-bromo-1-(3-chloro-2-pyridyl)-1H-pyrazole-5-carboxylic acid is a key intermediate, and the core step of its preparation process is the oxidation reaction of the pyrazoline intermediate. The traditional oxidation reaction process generally uses organic solvents such as acetonitrile as the reaction medium. Acetonitrile is a flammable and explosive solvent, and it is easy to volatilize to form an explosive mixture gas during the oxidation reaction at high temperatures. At the same time, the traditional reaction tank lacks real-time monitoring and emergency treatment mechanisms, further exacerbating the risks of explosion and fire.

[0003] Patent CN114787141B discloses a method for preparing ethyl 3-bromo-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carboxylate. The above patent has solved the problems of improving the total yield, reducing the cost, and reducing the process hazards.

[0004] The above patent has achieved an increase in the total yield and a reduction in cost, but there is still room for optimization in accurately controlling the reaction temperature during the oxidation reaction.

[0005] Therefore, the present application proposes a pyrazoline oxidation reaction device with high safety that can accurately control the temperature. Summary of the Invention

[0006] The purpose of the present invention is to provide a pyrazoline oxidation reaction device with high safety to solve the technical problems of the solvent being easily volatilized to form an explosive mixture gas during the high-temperature oxidation reaction, exacerbating the risks of fire and explosion as mentioned in the above background art.

[0007] To achieve the above purpose, the present invention provides the following technical solution: A pyrazoline oxidation reaction device with high safety, including a housing and a heat transfer oil circulation temperature control component, wherein the outer wall side of the housing is connected with the heat transfer oil circulation temperature control component; The heat transfer oil circulation temperature control component includes: an upper oil outlet interface, a lower oil outlet interface, an oil outlet pipe, a circulating temperature control pump, an oil inlet pipe, and an oil inlet interface; The housing is provided with an upper oil outlet interface and an oil inlet interface on the side. The upper oil outlet interface and the oil inlet interface are interconnected with the jacket inside the housing. The upper oil outlet interface is engaged with the lower oil outlet interface through internal threads. Bolts pass through the four screw holes of the upper and lower interfaces to fix the two interfaces. The lower oil outlet interface is arranged at one end of the oil outlet pipe, and the other end of the oil outlet pipe is connected to the outer wall side of the circulating temperature control pump. The other side of the outer wall of the circulating temperature control pump is connected with an oil inlet pipe, and the oil inlet pipe and the oil inlet interface are interconnected.

[0008] Preferably, a sealing layer is installed at the top end of the outer wall of the outer shell. At the top of the outer wall of the sealing layer, there is a connecting layer. At the top of the outer wall of the connecting layer, a lower connecting port is installed. At the bottom of the outer wall of the sealing cover, there is an upper connecting port. The upper connecting port is engaged with the lower connecting port through internal threads. Bolts pass through the four screw holes of the upper and lower interfaces to fix the two interfaces.

[0009] Preferably, a water inlet pipe is provided at the top end of the outer wall of the circulating temperature control pump, and a water outlet pipe is provided at the bottom end of the outer wall of the circulating temperature control pump. The circulating temperature control pump includes a circulating pump, a heater, and a cooler; The circulating pump is installed in the heat transfer oil circulation pipeline. The pump body is made of stainless steel material, and the inner wall is polished by mirror to reduce the flow resistance of the heat transfer oil and push the heat transfer oil to continuously flow in the jacket and the entire circulation pipeline; The heater includes a heating element, and the heating element is a nickel-chromium alloy resistance wire. The nickel-chromium alloy resistance wire is evenly wound around the ceramic insulating column in a spiral shape and immersed in the heat transfer oil circulation pipeline; The cooler is internally provided with a heat exchange box. The top end of the outer wall of the heat exchange box is connected to the water inlet pipe, and the bottom end of the outer wall of the heat exchange box is connected to the water outlet pipe. The heat exchange box wraps the heat transfer oil circulation pipe. The heat transfer oil circulation pipe enters from one end of the side of the outer wall of the heat exchange box and is led out from the other side of the outer wall of the heat exchange box.

[0010] Preferably, a stirring assembly is installed at the top end of the outer wall of the sealing cover; The stirring assembly includes: a coupling, a lower motor interface, an upper motor interface, a bearing, a motor, a stirring shaft, and a paddle; A cover hole is provided at the top end of the outer wall of the sealing cover. The coupling is embedded in the cover hole. At the top end of the outer wall of the coupling, there is a lower motor interface. The lower motor interface is engaged with the upper motor interface through internal threads. After engagement, bolts pass through the four screw holes of the upper and lower interfaces to fix the two interfaces. The upper motor interface is provided at the bottom end of the outer wall of the motor. The bearing is connected to the motor. The bottom of the outer wall of the coupling is connected to a stirring shaft, and nine spiral paddles are provided on the side of the outer wall of the stirring shaft.

[0011] Preferably, a monitoring and warning assembly is provided on the sealing cover; The monitoring and warning assembly includes: a control screen, a connecting rod, a pressure sensor, a pressure data line, a temperature sensor, and a temperature data line; A connecting rod is installed at the top end of the outer wall of the sealing cover. At the end of the outer wall of the connecting rod, there is a control screen. At the bottom end of the outer wall of the connecting rod, a pressure data line and a temperature data line are connected. The pressure data line and the temperature data line pass through the sealing cover and are embedded in the inner wall of the reaction tank. The pressure data line is connected to the pressure sensor, and the temperature data line is connected to the temperature sensor. The pressure sensor is provided on the side of the inner wall of the reaction tank, and the temperature sensor is provided at the bottom of the inner wall of the reaction tank.

[0012] Preferably, an oxidant tank lower interface is installed at the top end of the outer wall of the sealing cover. The oxidant tank lower interface is engaged with the oxidant tank upper interface through internal threads. The oxidant tank upper interface is connected to the second delivery pipe, and the second delivery pipe is connected to the bottom of the outer wall of the oxidant tank. A novel oxidant is added to the oxidant tank; The novel oxidant includes: potassium persulfate, tetrabutylammonium bromide, and deionized water; The potassium persulfate accounts for 20% of the mass of the pyrazoline intermediate and can efficiently oxidize the pyrazoline intermediate; The tetrabutylammonium bromide is a phase transfer catalyst for the reaction, accounting for 4% of the mass of the pyrazoline intermediate, and can promote the reaction; The deionized water has stable chemical properties, is non-flammable and non-explosive, can dissolve potassium persulfate and tetrabutylammonium bromide, and provides a safe reaction medium for the oxidation reaction.

[0013] Preferably, an oxidant tank lower interface is provided at the top end of the outer wall of the sealing cover. The oxidant tank lower interface is engaged with the oxidant tank upper interface through internal threads. Bolts pass through the four screw holes of the upper and lower interfaces to fix the two interfaces. The oxidant tank upper interface is provided at one end of the second delivery pipe, and the other end of the second delivery pipe is connected to the bottom of the outer wall of the oxidant tank. A second valve is provided on the side of the outer wall of the second delivery pipe.

[0014] Preferably, a jacket is provided inside the outer shell, and heat-conducting oil is filled inside the jacket. The heat-conducting oil covers the outer wall of the reaction tank. A feed pipe is provided inside the reaction tank. One end of the feed pipe is connected to the raw material tank lower interface, and the other end is placed at the bottom end inside the reaction tank. A stirring shaft and blades are placed in the middle inside the reaction tank. A pressure sensor is provided on the side of the inner wall of the reaction tank, a temperature sensor is provided at the bottom of the inner wall of the reaction tank, pressure data lines and temperature data lines are embedded in the inner wall of the reaction tank, and a discharge valve port is provided at the bottom of the inner wall of the reaction tank.

[0015] Preferably, a discharge valve port is provided at the bottom of the inner wall of the reaction tank. The discharge valve port is connected to the discharge upper interface. The discharge upper interface is engaged with the discharge lower interface through internal threads. The discharge lower interface is provided at one end of the discharge pipe, and the other end of the discharge pipe is connected to the collection tank interface. The collection tank interface is provided at the top end of the outer wall of the collection tank. A third valve is provided on the side of the outer wall of the discharge pipe.

[0016] Preferably, a raw material tank lower interface is provided at the top end of the outer wall of the sealing cover. The raw material tank lower interface is engaged with the raw material tank upper interface through internal threads. Bolts pass through the four screw holes of the upper and lower interfaces to fix the two interfaces. The raw material tank upper interface is provided at one end of the first delivery pipe, and the other end of the first delivery pipe is connected to the bottom of the outer wall of the raw material tank. A first valve is provided on the side of the outer wall of the first delivery pipe.

[0017] Compared with the prior art, the beneficial effects of the present invention are: 1. The present invention realizes the precise control of the reaction temperature by installing a heat transfer oil circulation temperature control component, adjusts the temperature of the heat transfer oil in real time, stably controls the reaction temperature within the target range, avoids reaction abnormalities caused by temperature fluctuations, and maintains the temperature stability and safety of the reaction system; 2. The present invention realizes the uniform dispersion of the multiphase system and the acceleration of the reaction by installing a stirring component. The spiral high-efficiency stirring promotes the uniform distribution of the phase transfer catalyst, accelerates the dissolution of the oxidant and the heat transfer of the reaction heat, shortens the reaction time, makes the reaction process more balanced, reduces the phenomena of local overheating or insufficient reaction, and improves the overall reaction efficiency; 3. The present invention designs a new oxidant system, realizes a safe oxidation reaction and an improvement in oxidation efficiency, completely abandons flammable and explosive organic solvents, uses a non-flammable aqueous medium as the reaction carrier, significantly reduces the fire and explosion risk of the reaction system, creates a safe and stable reaction environment, and completely eliminates safety accidents caused by solvent volatilization and violent reactions from the source; 4. The present invention realizes a rapid emergency response by installing a monitoring and early warning component. High-precision pressure sensors and temperature sensors capture the pressure and temperature changes in the reaction tank in real time, and combine with the control panel to achieve early warning of abnormal states, providing sufficient emergency handling time for operators, minimizing the probability of safety accidents, ensuring the safety of personnel and the integrity of equipment, and improving the reliability of the entire production system. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 is a three-dimensional structural schematic diagram of the present invention; Figure 2 is a front structural schematic diagram of the present invention; Figure 3 is a structural schematic diagram of the sealing cover of the present invention; Figure 4 is a schematic diagram of the overall internal structure of the present invention; Figure 5 is a schematic diagram of the internal structure of the reaction tank of the present invention; Figure 6 is a schematic diagram of the cross-sectional structure of the jacket of the present invention; Figure 7 is a schematic diagram of the structure of the stirring component of the present invention; Figure 8 is a schematic diagram of the structure of the temperature sensor of the present invention.

[0019] In the figure: 1. Outer shell; 2. Sealing layer; 3. Connecting layer; 4. Lower connection port; 5. Upper connection port; 6. Bolt; 7. Sealing cover; 8. Connecting rod; 9. Control panel; 10. Coupling; 11. Cover hole; 12. Lower interface of raw material tank; 13. Lower interface of oxidant tank; 14. Screw hole; 15. Upper interface of raw material tank; 16. First conveying pipe; 17. Raw material tank; 18. Upper interface of oxidant tank; 19. Second conveying pipe; 20. Oxidant tank; 21. Upper oil outlet interface; 22. Lower oil outlet interface; 23. Oil outlet pipe; 24. Circulating temperature control pump; 25. Inlet pipe; 26. Inlet oil interface; 27. Upper discharge interface; 28. Lower discharge interface; 29. Discharge pipe; 30. Collection tank interface; 31. Collection tank; 32. Jacket; 33. Reaction tank; 34. Feed pipe; 35. Lower interface of motor; 36. Upper interface of motor; 37. Bearing; 38. Motor; 39. Stirring shaft; 40. Paddle; 41. Pressure sensor; 42. Pressure data line; 43. Temperature sensor; 44. Temperature data line; 45. First valve; 46. Second valve; 47. Third valve; 48. Water inlet pipe; 49. Water outlet pipe. Detailed implementation mode

[0020] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0021] In the description of the present invention, it should be noted that the orientation or positional relationship indicated by the terms "upper", "lower", "inner", "outer", "front end", "rear end", "both ends", "one end", "the other end", etc. is based on the orientation or positional relationship shown in the accompanying drawings. It is only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of the present invention. In addition, the terms "first" and "second" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance.

[0022] In the description of the present invention, it should be noted that unless otherwise clearly specified and limited, the terms "installation", "provided with", "connection", etc. should be understood in a broad sense. For example, "connection" can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium, and it can be the communication inside two elements. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0023] Please refer to Figure 1 , Figure 3 , Figure 4 and Figure 5 , an embodiment provided by the present invention: a pyrazoline oxidation reaction device with high safety. An oxidant tank lower interface 13 is installed at the top end of the outer wall of the sealing cover 7. The oxidant tank lower interface 13 is engaged with the oxidant tank upper interface 18 through internal threads. The oxidant tank upper interface 18 is connected to the second delivery pipe 19. The second delivery pipe 19 is connected to the bottom of the outer wall of the oxidant tank 20. A novel oxidant is added to the oxidant tank 20; The novel oxidant includes: potassium persulfate, tetrabutylammonium bromide, and deionized water. The potassium persulfate accounts for 20% of the mass of the pyrazoline intermediate and can efficiently oxidize the pyrazoline intermediate; The tetrabutylammonium bromide is a phase transfer catalyst for the reaction and accounts for 4% of the mass of the pyrazoline intermediate, which can promote the reaction; A raw material tank lower interface 12 is provided at the top end of the outer wall of the sealing cover 7. The raw material tank lower interface 12 is engaged with the raw material tank upper interface 15 through internal threads. The bolt 6 passes through the four screw holes 14 of the upper and lower interfaces to fix the two interfaces. The raw material tank upper interface 15 is provided at one end of the first delivery pipe 16. The other end of the first delivery pipe 16 is connected to the bottom of the outer wall of the raw material tank 17. A first valve 45 is provided on the side of the outer wall of the first delivery pipe 16; The deionized water has stable chemical properties, is non-flammable and non-explosive, can dissolve potassium persulfate and tetrabutylammonium bromide, and provides a safe reaction medium for the oxidation reaction; An oxidant tank lower interface 13 is provided at the top end of the outer wall of the sealing cover 7. The oxidant tank lower interface 13 is engaged with the oxidant tank upper interface 18 through internal threads. The bolt 6 passes through the four screw holes 14 of the upper and lower interfaces to fix the two interfaces. The oxidant tank upper interface 18 is provided at one end of the second delivery pipe 19. The other end of the second delivery pipe 19 is connected to the bottom of the outer wall of the oxidant tank 20. A second valve 46 is provided on the side of the outer wall of the second delivery pipe 19; Further, open the lid of the raw material tank 17, add 500 g of pyrazoline intermediate, then open the lid of the oxidant tank 20, add the novel oxidant, and sequentially add 100 g of potassium persulfate, 20 g of tetrabutylammonium bromide and 800 mL of deionized water, and then close the lid; the top end of the outer wall of the sealing cover 7 provides an installation position for the lower interface 13 of the oxidant tank, the upper interface 18 of the oxidant tank is arranged at one end of the second delivery pipe 19, the lower interface 13 of the oxidant tank and the upper interface 18 of the oxidant tank are engaged by internal threads, after engagement, place the bolt 6 in the four screw holes 14 of the upper and lower interfaces to fix the interfaces, tightly connect the second delivery pipe 19 and the lower interface 13 of the oxidant tank, the lower interface 13 of the oxidant tank leads into the reaction tank 33 below the sealing cover 7, and then issue an instruction to open the second valve 46 through the control panel 9, the control panel 9 is connected to the second valve 46 through the data line embedded in the second delivery pipe 19, after the second valve 46 is opened, the novel oxidant flows from the oxidant tank 20 into the second delivery pipe 19, and the second delivery pipe 19 transports the novel oxidant to the reaction tank 33; The top end of the outer wall of the sealing cover 7 provides an installation position for the lower interface 12 of the raw material tank, the upper interface 15 of the raw material tank is arranged at one end of the first delivery pipe 16, the lower interface 12 of the raw material tank and the upper interface 15 of the raw material tank are engaged by internal threads, after engagement, place the bolt 6 in the four screw holes 14 of the upper and lower interfaces to fix the interfaces, tightly connect the first delivery pipe 16 and the lower interface 12 of the raw material tank, the lower interface 12 of the raw material tank is connected to the feed pipe 34, and then issue an instruction to open the first valve 45 through the control panel 9, the control panel 9 is connected to the first valve 45 through the data line embedded in the first delivery pipe 16, after the first valve 45 is opened, the pyrazoline intermediate flows from the raw material tank 17 into the first delivery pipe 16, the first delivery pipe 16 transports the pyrazoline intermediate to the feed pipe 34, and the feed pipe 34 transports the pyrazoline intermediate to the bottom end inside the reaction tank 33; In the reaction tank 33, the pyrazoline intermediate undergoes an oxidation reaction. During the oxidation reaction, potassium persulfate first decomposes in the aqueous solution to generate sulfate radicals SO4 - ; Decomposition reaction formula: K2S2O8 → 2K + + 2SO4 - ; Sulfate radicals have extremely strong oxidizing properties and can undergo an oxidation reaction with the pyrazoline intermediate to oxidize it into the target product. However, the pyrazoline intermediate has certain hydrophobicity and poor solubility in the aqueous phase, which limits the progress of the reaction. At this time, the phase transfer catalyst tetrabutylammonium bromide plays an important role. The cationic part of tetrabutylammonium bromide, tetrabutylammonium ion, can combine with the pyrazoline intermediate to form an ion pair, enabling it to transfer from the organic phase to the aqueous phase. In the aqueous phase, the pyrazoline intermediate comes into full contact with sulfate radicals and undergoes a full oxidation reaction, improving the reaction efficiency and product yield; the deionized water as the aqueous medium in the reaction tank 33 provides a stable environment for the decomposition of potassium persulfate and the action of the phase transfer catalyst tetrabutylammonium bromide, reducing the risks of explosion and combustion. At the same time, by dissolving potassium persulfate and the phase transfer catalyst, they are evenly dispersed in the reaction system to ensure that the reaction can proceed under uniform conditions.

[0024] Please refer to Figure 1 、 Figure 2 、 Figure 4 and Figure 6 ,An embodiment provided by the present invention: A pyrazoline oxidation reaction device with high safety, wherein the outer wall side of the outer shell 1 is connected with a heat transfer oil circulation temperature control component; the heat transfer oil circulation temperature control component includes: an oil outlet upper interface 21, an oil outlet lower interface 22, an oil outlet pipe 23, a circulation temperature control pump 24, an oil inlet pipe 25, and an oil inlet interface 26; The outer shell 1 is provided with an oil outlet upper interface 21 and an oil inlet interface 26 on the side. The oil outlet upper interface 21 and the oil inlet interface 26 are in mutual communication with the jacket 32 inside the outer shell 1. The oil outlet upper interface 21 is meshed with the oil outlet lower interface 22 through internal threads. The bolt 6 passes through the four screw holes 14 of the upper and lower interfaces to fix the two interfaces. The oil outlet lower interface 22 is arranged at one end of the oil outlet pipe 23. The other end of the oil outlet pipe 23 is connected to the outer wall side of the circulation temperature control pump 24. The other side of the outer wall of the circulation temperature control pump 24 is connected with an oil inlet pipe 25, and the oil inlet pipe 25 and the oil inlet interface 26 are mutually connected; The outer wall top of the circulation temperature control pump 24 is provided with a water inlet pipe 48, and the outer wall bottom of the circulation temperature control pump 24 is provided with a water outlet pipe 49. The circulation temperature control pump 24 includes a circulation pump, a heater, and a cooler; The circulation pump is installed in the heat transfer oil circulation pipeline. The pump body is made of stainless steel material, and the inner wall is mirror-polished to reduce the flow resistance of the heat transfer oil and promote the continuous flow of the heat transfer oil in the jacket 32 and the entire circulation pipeline; The heater includes a heating element, and the heating element is a nickel-chromium alloy resistance wire. The nickel-chromium alloy resistance wire is evenly wound around the ceramic insulating column in a spiral shape and immersed in the heat transfer oil circulation pipeline; Inside the cooler, there is a heat exchange box. The top end of the outer wall of the heat exchange box is connected to the water inlet pipe 48, and the bottom end of the outer wall of the heat exchange box is connected to the water outlet pipe 49. The heat exchange box wraps the heat-conducting oil circulation pipe. The heat-conducting oil circulation pipe enters from one end of the side of the outer wall of the heat exchange box and exits from the other side of the outer wall of the heat exchange box. Further, the side of the outer shell 1 provides an installation position for the oil outlet upper interface 21 and the oil inlet interface 26. Inside the outer shell 1, there is a reaction tank 33. The space gap between the outer shell 1 and the reaction tank 33 is a jacket 32. The oil outlet lower interface 22 is arranged at one end of the oil outlet pipe 23. One end of the oil outlet upper interface 21 communicates with the jacket 32, and the other end is engaged with the oil outlet lower interface 22 through internal threads. The bolt 6 passes through the four screw holes 14 of the upper and lower interfaces to fix the two interfaces, tightly connecting the oil outlet upper interface 21 and the oil outlet pipe 23. The other end of the oil outlet pipe 23 is connected to the interface on the side wall of the outer wall of the circulating temperature control pump 24, communicating with one end of the side wall of the heat exchange box inside the circulating temperature control pump 24. The heat exchange box is placed inside the circulating temperature control pump 24. The oil outlet pipe 23 exits from the other side of the heat exchange box and is connected to the heater. The heater is placed inside the circulating temperature control pump 24 and is connected to the heat exchange box through the oil outlet pipe 23 on the side. The other side of the heater is connected to the oil inlet pipe 25. The oil inlet pipe 25 is connected to the interface on the side wall of the circulating temperature control pump 24, and the other side of the oil inlet pipe 25 is connected to the oil inlet interface 26. The oil inlet interface 26 is arranged on the side wall of the outer shell 1. Before putting in the raw materials and the new oxidant, preheat the reaction tank 33 to a temperature between 50 - 80 °C to reach the optimal temperature for the oxidant reaction. First, start the circulation pump, pump the heat-conducting oil in the oil inlet pipe 25 into the jacket 32 through the oil inlet interface 26. At the same time, start the heater, and the resistance wire heats up to make the temperature of the heat-conducting oil higher. The heat-conducting oil transfers heat to the reaction tank 33 in the jacket 32, causing the temperature inside the reaction tank 33 to rise. The temperature sensor 43 on the side wall of the inner wall of the reaction tank 33 monitors the temperature in real time. When it reaches 65 °C, stop heating. After the heat-conducting oil in the jacket 32 transfers the heat, it transports the heat-conducting oil to the oil outlet pipe 23 through the upper and lower oil outlet interfaces. The oil outlet pipe 23 transports the heat-conducting oil to the circulating temperature control pump 24. At this time, the cooler is closed, and the heat-conducting oil passes through the cooler and then enters the heater again for heating. When the temperature sensor 43 monitors that the temperature reaches 65 °C, stop heating, and then open the first valve 45 and the second valve 46 to inject the pyrazoline intermediate and the oxidant into the reaction tank 33.

[0025] Please refer to Figure 2 、 Figure 4 、 Figure 6 and Figure 7 As shown in, an embodiment provided by the present invention: A pyrazoline oxidation reaction device with high safety. A stirring assembly is installed at the top end of the outer wall of the sealing cover 7. The stirring assembly includes: a coupling 10, a motor lower interface 35, a motor upper interface 36, a bearing 37, a motor 38, a stirring shaft 39, and a paddle 40. The top end of the outer wall of the sealing cover 7 is provided with a cover hole 11. The coupling 10 is embedded in the cover hole 11. The top end of the outer wall of the coupling 10 is provided with a lower motor interface 35. The lower motor interface 35 is meshed with the upper motor interface 36 through internal threads. After meshing, the bolt 6 passes through the four screw holes 14 of the upper and lower interfaces to fix the two interfaces. The upper motor interface 36 is arranged at the bottom end of the outer wall of the motor 38. The bearing 37 is connected to the motor 38. The bottom of the outer wall of the coupling 10 is connected with a stirring shaft 39. Nine spiral blades 40 are arranged on the side of the outer wall of the stirring shaft 39; A jacket 32 is arranged inside the outer shell 1. Heat-conducting oil is filled inside the jacket 32. The heat-conducting oil covers the outer wall of the reaction tank 33. A feed pipe 34 is arranged inside the reaction tank 33. One end of the feed pipe 34 is connected to the lower interface 12 of the raw material tank, and the other end is placed at the bottom end inside the reaction tank 33. A stirring shaft 39 and blades 40 are placed in the middle inside the reaction tank 33. A pressure sensor 41 is arranged on the side of the inner wall of the reaction tank 33. A temperature sensor 43 is arranged at the bottom of the inner wall of the reaction tank 33. Pressure data lines 42 and temperature data lines 44 are embedded in the inner wall of the reaction tank 33. A discharge valve port is arranged at the bottom of the inner wall of the reaction tank 33; Furthermore, the sealing cover 7 provides an installation position for the cover hole 11. The coupling 10 is embedded in the cover hole 11. The top end of the outer wall of the coupling 10 is provided with a lower motor interface 35. The upper motor interface 36 is arranged at the bottom end of the outer wall of the motor 38. The lower motor interface 35 is connected to the upper motor interface 36 to tightly fix the coupling 10 and the motor 38. The coupling 10 is connected to the drive shaft of the motor 38 through the bearing 37. The bottom end of the outer wall of the coupling 10 is connected to the stirring shaft 39. The stirring shaft 39 is driven by the motor 38 to rotate. Nine spiral blades 40 are arranged on the side of the outer wall of the stirring shaft 39. The spirally dispersed blades 40 break up larger material particles, promote the uniform dispersion of the phase transfer catalyst in the aqueous medium, accelerate the reaction rate, and improve the efficiency and uniformity of the oxidation reaction; After adding the pyrazoline intermediate and the oxidant, start the stirring assembly. The motor 38 is started. The drive shaft in the motor 38 rotates. Through the action of the coupling 10, the torque of the motor 38 is transmitted from the drive shaft to the stirring shaft 39. The stirring shaft 39 starts to rotate, driving the nine spiral blades 40 on the side of the stirring shaft 39. The blades 40 rotate in the reaction tank 33 to uniformly stir the mixture of the pyrazoline intermediate and the oxidant and fully react.

[0026] Please refer to Figure 2 、 Figure 5 and Figure 6, An embodiment provided by the present invention: A pyrazoline oxidation reaction device with high safety. A sealing layer 2 is installed at the top end of the outer wall of the outer shell 1. A connection layer 3 is provided at the top of the outer wall of the sealing layer 2. A lower connection port 4 is installed at the top of the outer wall of the connection layer 3. An upper connection port 5 is provided at the bottom of the outer wall of the sealing cover 7. The upper connection port 5 is engaged with the lower connection port 4 through internal threads. The bolt 6 passes through the four screw holes 14 of the upper and lower interfaces to fix the two interfaces. A discharge valve port is provided at the bottom of the inner wall of the reaction tank 33. The discharge valve port is connected to the upper discharge interface 27. The upper discharge interface 27 is engaged with the lower discharge interface 28 through internal threads. The lower discharge interface 28 is provided at one end of the discharge pipe 29. The other end of the discharge pipe 29 is connected to the collection tank interface 30. The collection tank interface 30 is provided at the top end of the outer wall of the collection tank 31. A third valve 47 is provided on the side of the outer wall of the discharge pipe 29. Furthermore, the bottom of the outer wall of the sealing cover 7 provides an installation position for the upper connection port 5. The lower connection port 4 is provided at the top end of the outer wall of the connection layer 3. The upper connection port 5 is engaged with the lower connection port 4 through internal threads. After engagement, the bolt 6 passes through the four screw holes 14 of the upper and lower interfaces to fix the two interfaces, tightly connecting the connection layer 3 and the sealing cover 7. The bottom of the outer wall of the connection layer 3 is connected to the sealing layer 2. The sealing layer 2 keeps the tank body in a sealed state. The bottom end of the outer wall of the sealing layer 2 is connected to the outer shell 1. The bottom of the inner wall of the reaction tank 33 provides an installation position for the discharge valve port. When the oxidation reaction is carried out, the discharge valve port is closed to block the reaction solution above the reaction tank 33. When the reaction is completed, the discharge valve port is opened, and the reaction product pyrazole acid flows towards the upper discharge interface 27. The lower discharge interface 28 is provided at one end of the discharge pipe 29. The upper discharge interface 27 is engaged with the lower discharge interface 28 through internal threads. After engagement, the bolt 6 passes through the four screw holes 14 of the upper and lower interfaces to fix the two interfaces, tightly connecting the upper discharge interface 27 and the discharge pipe 29. At this time, the reaction product pyrazole acid flows from the upper discharge interface 27 to the discharge pipe 29. The side of the outer wall of the discharge pipe 29 provides an installation position for the third valve 47. At the same time, the third valve 47 is opened. The other end of the discharge pipe 29 is connected to the collection tank interface 30. The collection tank interface 30 is provided at the top end of the outer wall of the collection tank 31. The reaction product pyrazole acid flows from the discharge pipe 29 to the collection tank 31 when the third valve 47 is opened.

[0027] Please refer to Figure 3 , Figure 4 , Figure 5 and Figure 8 , An embodiment provided by the present invention: A pyrazoline oxidation reaction device with high safety. A monitoring and warning component is provided on the sealing cover 7. The monitoring and warning component includes: a control screen 9, a connecting rod 8, a pressure sensor 41, a pressure data line 42, a temperature sensor 43, and a temperature data line 44. At the top end of the outer wall of the sealing cover 7, a connecting rod 8 is installed. At the end of the outer wall of the connecting rod 8, a control screen 9 is provided. At the bottom end of the outer wall of the connecting rod 8, a pressure data line 42 and a temperature data line 44 are connected. The pressure data line 42 and the temperature data line 44 pass through the sealing cover 7 and are embedded in the inner wall of the reaction tank 33. The pressure data line 42 is connected to the pressure sensor 41, and the temperature data line 44 is connected to the temperature sensor 43. The pressure sensor 41 is arranged on the side surface of the inner wall of the reaction tank 33, and the temperature sensor 43 is arranged at the bottom of the inner wall of the reaction tank 33; At the top end of the outer wall of the circulating temperature control pump 24, a water inlet pipe 48 is provided. At the bottom end of the outer wall of the circulating temperature control pump 24, a water outlet pipe 49 is provided. The circulating temperature control pump 24 includes a circulating pump, a heater, and a cooler; the circulating pump is installed in the heat-conducting oil circulation pipeline. The pump body is made of stainless steel material, and the inner wall is polished by mirror surface to reduce the flow resistance of the heat-conducting oil and promote the continuous flow of the heat-conducting oil in the jacket 32 and the entire circulation pipeline; The heater includes a heating element, and the heating element is a nickel-chromium alloy resistance wire. The nickel-chromium alloy resistance wire is evenly wound around the ceramic insulating column in a spiral shape and immersed in the heat-conducting oil circulation pipeline; Inside the cooler, a heat exchange box is provided. At the top end of the outer wall of the heat exchange box, the water inlet pipe 48 is connected. At the bottom end of the outer wall of the heat exchange box, the water outlet pipe 49 is connected. The heat exchange box wraps the heat-conducting oil circulation pipe. The heat-conducting oil circulation pipe enters from one end of the side surface of the outer wall of the heat exchange box and exits from the other side of the outer wall of the heat exchange box; Furthermore, a monitoring and warning component is installed on the sealing cover 7. The top end of the outer wall of the sealing cover 7 provides an installation position for the connecting rod 8. At the top end of the outer wall of the connecting rod 8, a control screen 9 is installed. The control screen 9 is connected to the first valve 45 and the second valve 46 through a data line. The control screen 9 is also connected to a pressure data line 42 and a temperature data line 44. The two data lines are embedded in the connecting rod 8 and connected to the pressure sensor 41 and the temperature sensor 43 in the reaction tank 33; When the heat-conducting oil circulation temperature control component is started, the temperature sensor 43 in the reaction tank 33 monitors the temperature in the reaction tank 33 in real time and transmits the monitored data to the control screen 9 through the temperature data line 44. After the processor in the control screen 9 receives the temperature data, it detects whether it reaches 65 °C. When it reaches 65 °C, the control screen 9 controls the circulating temperature control pump 24 to stop heating the heater. The control screen 9 is connected to the circulating temperature control pump 24 through a data line embedded in the pipe wall; When it is monitored that the temperature in the reaction tank 33 rises above the threshold value of 80°C, the control panel 9 controls the circulating temperature control pump 24 to stop the heater from heating, and at the same time opens the cooler. Cooling water enters from the water inlet pipe 48 and flows into the heat exchange box. The cooling water covers the outer wall of the oil outlet pipe 23, absorbs the heat of the heat-conducting oil, reduces the temperature of the heat-conducting oil, and then pumps the low-temperature heat-conducting oil from the water inlet pipe 25 into the jacket 32 through the circulating pump to absorb the heat of the reaction tank 33 and reduce the temperature of the reaction tank 33. The heat-conducting oil that has absorbed the heat enters the cooler again from the oil outlet pipe 23 for cooling, and so on. When the temperature sensor 43 monitors that the temperature drops to 65°C, the control panel 9 controls the cooler in the circulating temperature control pump 24 to stop running; The pressure sensor 41 monitors the pressure inside the reaction tank 33 in real time and transmits the data back to the control panel 9. When the processor in the control panel 9 detects that the pressure exceeds the threshold value of 0.5 MPa, the control panel 9 issues a red light alarm to remind the staff to stay away. At the same time, the control panel 9 closes the first valve 45, the second valve 46 and the motor 38 through the data line to prevent feeding and stirring and slow down the reaction rate until the pressure sensor 41 monitors that the data returns to normal.

[0028] Working principle: First, start the heat-conducting oil circulation temperature control component, raise the temperature in the reaction tank 33 to a suitable reaction temperature through the heat-conducting oil, and then inject the pyrazoline intermediate and the novel oxidant into the reaction tank 33; Then start the stirring component, accelerate the reaction rate through the rotational movement of the spiral blade 40. At the same time, the monitoring and warning component monitors the temperature and pressure in the reaction tank 33 in real time through the temperature sensor 43 and the pressure sensor 41. When the data exceeds the threshold value, the control panel 9 takes safety measures to ensure the safe progress of the reaction and reminds the staff to stay away; Finally, when the oxidation reaction is over, open the discharge valve opening, and collect the reaction product pyrazole acid into the collection tank 31 through the discharge pipe 29.

[0029] For those skilled in the art, it is obvious that the present invention is not limited to the details of the above exemplary embodiments, and the present invention can be implemented in other specific forms without departing from the spirit or basic characteristics of the present invention. Therefore, from any point of view, the embodiments should be regarded as exemplary and non-limiting. The scope of the present invention is defined by the appended claims rather than the above description. Therefore, all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be included in the present invention. Any reference signs in the claims should not be regarded as limiting the claims involved.

Claims

1. A pyrazoline oxidation reaction device with high safety, comprising a housing (1) and a heat transfer oil circulation temperature control component, characterized in that: A heat-conducting oil circulation temperature control component is connected to the side of the outer wall of the outer shell (1). The heat-conducting oil circulation temperature control component includes: an upper oil outlet interface (21), a lower oil outlet interface (22), an oil outlet pipe (23), a circulating temperature control pump (24), an oil inlet pipe (25), and an oil inlet interface (26). An upper oil outlet interface (21) and an oil inlet interface (26) are arranged on the side of the outer shell (1). The upper oil outlet interface (21) and the oil inlet interface (26) are communicated with the jacket (32) inside the outer shell (1). The upper oil outlet interface (21) is meshed with the lower oil outlet interface (22) through internal threads. Bolts (6) pass through the four screw holes (14) of the upper and lower interfaces to fix the two interfaces. The lower oil outlet interface (22) is arranged at one end of the oil outlet pipe (23). The other end of the oil outlet pipe (23) is connected to the side of the outer wall of the circulating temperature control pump (24). The other side of the outer wall of the circulating temperature control pump (24) is connected with an oil inlet pipe (25), and the oil inlet pipe (25) and the oil inlet interface (26) are connected to each other.

2. The pyrazoline oxidation reaction device with high security according to claim 1, wherein: A sealing layer (2) is installed at the top of the outer wall of the outer shell (1). A connecting layer (3) is arranged at the top of the outer wall of the sealing layer (2). A lower connecting port (4) is installed at the top of the outer wall of the connecting layer (3). An upper connecting port (5) is arranged at the bottom of the outer wall of the sealing cover (7). The upper connecting port (5) is meshed with the lower connecting port (4) through internal threads. Bolts (6) pass through the four screw holes (14) of the upper and lower interfaces to fix the two interfaces.

3. A highly secure pyrazoline oxidation reaction device according to claim 1, characterized in that: A water inlet pipe (48) is arranged at the top of the outer wall of the circulating temperature control pump (24), and a water outlet pipe (49) is arranged at the bottom of the outer wall of the circulating temperature control pump (24). The circulating temperature control pump (24) includes a circulating pump, a heater, and a cooler. The circulating pump is installed in the heat-conducting oil circulation pipeline. The pump body is made of stainless steel material, and the inner wall is polished by mirror surface, reducing the flow resistance of the heat-conducting oil and pushing the heat-conducting oil to continuously flow in the jacket (32) and the whole circulation pipeline. The heater includes a heating element, and the heating element is a nickel-chromium alloy resistance wire. The nickel-chromium alloy resistance wire is evenly wound around the ceramic insulating column in a spiral shape and immersed in the heat-conducting oil circulation pipeline. A heat exchange box is arranged inside the cooler. The top of the outer wall of the heat exchange box is connected with a water inlet pipe (48), and the bottom of the outer wall of the heat exchange box is connected with a water outlet pipe (49). The heat exchange box wraps the heat-conducting oil circulation pipe. The heat-conducting oil circulation pipe enters from one end of the side of the outer wall of the heat exchange box and exits from the other side of the outer wall of the heat exchange box.

4. A high-safety pyrazoline oxidation reaction device according to claim 2, characterized in that: A stirring component is installed at the top of the outer wall of the sealing cover (7). The stirring component includes: a coupling (10), a lower motor interface (35), an upper motor interface (36), a bearing (37), a motor (38), a stirring shaft (39), and a paddle (40). The top end of the outer wall of the sealing cover (7) is provided with a cover hole (11), the coupling (10) is embedded in the cover hole (11), the top end of the outer wall of the coupling (10) is provided with a lower motor interface (35), the lower motor interface (35) is meshed with the upper motor interface (36) through internal threads, and after meshing, the bolt (6) passes through the four screw holes (14) of the upper and lower interfaces to fix the two interfaces. The upper motor interface (36) is arranged at the bottom end of the outer wall of the motor (38), the bearing (37) is connected to the motor (38), the bottom of the outer wall of the coupling (10) is connected with a stirring shaft (39), and nine spiral blades (40) are arranged on the side surface of the outer wall of the stirring shaft (39).

5. A high-security pyrazoline oxidation reaction device according to claim 2, characterized in that: A monitoring and warning component is arranged on the sealing cover (7); The monitoring and warning component includes: a control screen (9), a connecting rod (8), a pressure sensor (41), a pressure data line (42), a temperature sensor (43) and a temperature data line (44); The top end of the outer wall of the sealing cover (7) is installed with a connecting rod (8), the end of the outer wall of the connecting rod (8) is provided with a control screen (9), the bottom end of the outer wall of the connecting rod (8) is connected with a pressure data line (42) and a temperature data line (44), the pressure data line (42) and the temperature data line (44) pass through the sealing cover (7) and are embedded in the inner wall of the reaction tank (33). The pressure data line (42) is connected with the pressure sensor (41), the temperature data line (44) is connected with the temperature sensor (43), the pressure sensor (41) is arranged on the side surface of the inner wall of the reaction tank (33), and the temperature sensor (43) is arranged at the bottom of the inner wall of the reaction tank (33).

6. The pyrazoline oxidation reaction device with high safety according to claim 2, characterized in that: The top end of the outer wall of the sealing cover (7) is installed with a lower oxidant tank interface (13), the lower oxidant tank interface (13) is meshed with the upper oxidant tank interface (18) through internal threads, the upper oxidant tank interface (18) is connected with a second delivery pipe (19), the second delivery pipe (19) is connected to the bottom of the outer wall of the oxidant tank (20), and a new oxidant is added to the oxidant tank (20); The new oxidant includes: potassium persulfate, tetrabutylammonium bromide and deionized water; The potassium persulfate accounts for 20% of the mass of the pyrazoline intermediate and can efficiently oxidize the pyrazoline intermediate; The tetrabutylammonium bromide is a phase transfer catalyst for the reaction, accounting for 4% of the mass of the pyrazoline intermediate and can promote the reaction; The deionized water has stable chemical properties, is non-flammable and non-explosive, can dissolve potassium persulfate and tetrabutylammonium bromide, and provides a safe reaction medium for the oxidation reaction.

7. A high-safety pyrazoline oxidation reaction device according to claim 2, characterized in that: The top end of the outer wall of the sealing cover (7) is provided with a lower oxidant tank interface (13), the lower oxidant tank interface (13) is meshed with the upper oxidant tank interface (18) through internal threads, the bolt (6) passes through the four screw holes (14) of the upper and lower interfaces to fix the two interfaces. The upper oxidant tank interface (18) is arranged at one end of the second delivery pipe (19), the other end of the second delivery pipe (19) is connected to the bottom of the outer wall of the oxidant tank (20), and a second valve (46) is arranged on the side surface of the outer wall of the second delivery pipe (19).

8. A high-security pyrazoline oxidation reaction device according to claim 1, characterized in that: Inside the said housing (1), there is a jacket (32) provided. Inside the jacket (32), there is heat-conducting oil filled, and the heat-conducting oil covers the outer wall of the reaction tank (33). Inside the reaction tank (33), there is a feed pipe (34) provided. One end of the feed pipe (34) is connected to the lower interface (12) of the raw material tank, and the other end is placed at the bottom end inside the reaction tank (33). Inside the reaction tank (33), a stirring shaft (39) and paddle blades (40) are placed in the middle. On the side of the inner wall of the reaction tank (33), there is a pressure sensor (41) provided. At the bottom of the inner wall of the reaction tank (33), there is a temperature sensor (43) provided. The pressure data line (42) and temperature data line (44) are embedded in the inner wall of the reaction tank (33). At the bottom of the inner wall of the reaction tank (33), there is a discharge valve port.

9. A high-security pyrazoline oxidation reaction device according to claim 8, characterized in that: At the bottom of the inner wall of the said reaction tank (33), there is a discharge valve port, and the discharge valve port is connected to the upper discharge interface (27). The upper discharge interface (27) is meshed with the lower discharge interface (28) through internal threads. The lower discharge interface (28) is provided at one end of the discharge pipe (29). The other end of the discharge pipe (29) is connected to the collection tank interface (30). The collection tank interface (30) is provided at the top of the outer wall of the collection tank (31). On the side of the outer wall of the discharge pipe (29), there is a third valve (47) provided.

10. A highly secure pyrazoline oxidation reaction device according to claim 2, characterized in that: At the top of the outer wall of the said sealing cover (7), there is a lower interface (12) of the raw material tank. The lower interface (12) of the raw material tank is meshed with the upper interface (15) of the raw material tank through internal threads. Bolts (6) pass through the four screw holes (14) of the upper and lower interfaces to fix the two interfaces. The upper interface (15) of the raw material tank is provided at one end of the first delivery pipe (16). The other end of the first delivery pipe (16) is connected to the bottom of the outer wall of the raw material tank (17). On the side of the outer wall of the first delivery pipe (16), there is a first valve (45) provided.

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