Continuous oxidation equipment for heliotropin

Abstract

The heliotropin continuous oxidation equipment comprises a feeding device, a main body reaction device, a gas inlet device and a material storage device, all the device parts are communicated through corresponding pipelines, the feeding device is communicated with the main body reaction device through a feeding pipeline and conveys reaction raw materials for the main body reaction device, the gas inlet device is communicated with the main body reaction device through a gas inlet pipeline, and the material storage device is communicated with the main body reaction device through a gas outlet pipeline. The main body reaction device is used for conveying reaction gas, the main body reaction device is communicated with the storage device through a discharge pipeline, a finished product material after reaction is conveyed to the corresponding storage device for storage through the discharge pipeline, and the devices and the pipelines are provided with a plurality of corresponding monitoring devices and control valve bodies. The device is higher in efficiency, more stable, simple in structure, safer and more environment-friendly.

Description

Technical Field

[0001] The utility model belongs to the field of chemical equipment, and in particular relates to continuous oxidation equipment for preparing piperonal by utilizing nano bubbles. Background Art

[0002] In the prior art, when synthesizing piperonal with catechol methylene ether as raw material, piperonyl glycolic acid is first obtained, and then piperonal is obtained by oxidation and decarboxylation. The traditional oxidation method is to use air oxidation. In the traditional air oxidation, ordinary foam will quickly merge, rise and break due to the large bubble effect, the diffusivity in water is poor, the air and raw materials are unevenly mixed, and the reaction efficiency is low. Patent No.: CN 01804348.8 uses nitric acid as an oxidant, and the product has nitration byproducts that are difficult to separate, which affects the product quality and causes troublesome environmental pollution. Patent No.: CN 103923056 B uses hydrogen peroxide as an oxidant, but hydrogen peroxide has safety hazards during industrial use. Due to the unstable reaction, explosion accidents occur from time to time. In addition, in the existing piperonal oxidation equipment, due to the high cost of continuous preparation equipment, intermittent preparation equipment is often used in production, because it needs to be stopped and restarted intermittently, which makes the production efficiency low. Utility Model Content

[0003] The utility model aims to provide a safe, environmentally friendly, highly stable continuous oxidation device for preparing piperonal by using nanobubbles, so as to solve the technical problems of low production efficiency, low product quality, high safety hazards and easy environmental pollution caused by existing piperonal oxidation equipment.

[0004] In order to achieve the above purpose, the specific technical solution of the utility model is as follows:

[0005] A piperonal continuous oxidation device comprises a feeding device, a main reaction device, an air intake device and a storage device, wherein the components of each device are connected via corresponding pipelines, wherein the feeding device is connected to the main reaction device via a feeding pipeline to convey reaction raw materials thereto, the air intake device is connected to the main reaction device via an air intake pipeline to convey reaction gas thereto, the main reaction device is connected to the storage device via a discharge pipeline, and finished products after the reaction are completed are conveyed to the corresponding storage device for storage via the discharge pipeline, and a plurality of corresponding monitoring devices and control valve bodies are arranged on the above devices and pipelines.

[0006] Further, the main reaction device includes a main reaction box, in which a nanobubble disperser and a microchannel reactor are arranged in the inner cavity of the main reaction box, wherein the nanobubble disperser is arranged at the lower part of the inner cavity of the main reaction box, and the microchannel reactor is arranged above the nanobubble disperser. An air inlet corresponding to the nanobubble disperser is arranged at the bottom of the main reaction box, and the main reaction device is connected with the air inlet device through the air inlet. A feed pipe connected with the inner cavity of the main reaction box is arranged on the side wall of the main reaction box between the nanobubble disperser and the microchannel reactor, and the main reaction device is connected with the feed device through the feed pipe. A corresponding sight glass and a pressure sensor are arranged on the side wall of the main reaction box between the microchannel reactor and the feed pipe. A gas-liquid separator connected with its inner cavity is arranged above the main reaction box, and the gas-liquid separator is connected with the storage device through a discharge pipeline. A corresponding first pressure-temperature sensor is arranged at the bottom end of the side wall of the main reaction box, and a corresponding second pressure-temperature sensor is arranged on the gas-liquid separator.

[0007] Further, the nanobubble disperser is provided with a corresponding dispersion membrane, and a plurality of nanochannels are provided on the dispersion membrane. The microchannel reactor comprises a plurality of microchannels that are not interconnected, and the plurality of microchannels are evenly distributed in an array in the inner cavity of the shell of the microchannel reactor. An interlayer is provided between the microchannel and the shell, and an interlayer inlet connected to the interlayer is provided at the upper part of one side wall of the shell, and an interlayer outlet connected to the interlayer is provided at the lower part of the side wall opposite thereto. The microchannel reactor is externally connected to a corresponding heat exchange device through the interlayer inlet and the interlayer outlet, and the microchannel comprises a reaction chamber, and the plurality of reaction chambers are connected in series to form a microchannels, corresponding reaction channels are arranged at the upper and lower ends of each reaction chamber, and the two upper and lower adjacent reaction chambers are interconnected through the corresponding reaction channels, and a pair of channel baffles are arranged above the reaction channel at the lower end of each reaction chamber, a gap channel corresponding to the reaction channel below is arranged between the two channel baffles, and a corresponding arc baffle is arranged above the gap channel, and side gaps are arranged between the two sides of the arc baffle and the corresponding channel baffle, the lower reaction channel of the bottom reaction chamber is the microchannel inlet, and the upper reaction channel of the top reaction chamber is the microchannel outlet.

[0008] Further, the feeding device includes a raw material kettle, which is connected to the main reaction device through a feeding pipeline, the inlet of the feeding pipeline is connected to the discharge port of the raw material kettle, the outlet of the feeding pipeline is connected to the feeding pipe of the main reaction device, a corresponding raw material kettle valve is provided at the discharge port of the raw material kettle, and a corresponding feed pump, feed heat exchanger and feed flow meter are provided on the feeding pipeline between the raw material kettle and the feed pipe, wherein the feed pump is arranged at one end close to the raw material kettle, the feed flowmeter is arranged at one end close to the feed pipe, a feed heat exchanger is provided between the feed pump and the feed flowmeter, and a feed check valve and a feed valve are provided between the feed flowmeter and the feed pipe in sequence.

[0009] Furthermore, the air intake device includes an air supply machine, which is connected to the main reaction box through an air intake pipeline, the inlet of the air intake pipeline is connected to the air outlet of the air supply machine, and the outlet of the air intake pipeline is connected to the air inlet of the main reaction box. An air intake valve, a supply pressure gauge, an air supply check valve and an air outlet valve are sequentially provided on the air intake pipeline between the air supply machine and the main reaction box, wherein the air intake valve and the air outlet valve are respectively arranged at the inlet and outlet of the air intake pipeline, the supply pressure gauge is arranged on the side of the air intake pipeline close to the air intake valve, and the air supply check valve is arranged between the supply pressure gauge and the air outlet valve.

[0010] Furthermore, the storage device includes a receiving kettle, which is connected to the gas-liquid separator through a discharge pipeline. The inlet end of the discharge pipeline is connected to the liquid outlet of the gas-liquid separator. A corresponding discharge valve is provided at the inlet end of the discharge pipeline, and a discharge flowmeter and a discharge heat exchanger are provided between the discharge valve and the receiving kettle.

[0011] Furthermore, the gas-liquid separator is connected to a buffer tank via a buffer pipeline, the inlet end of the buffer pipeline is connected to the gas outlet of the gas-liquid separator, and a pressure reducing valve and a buffer heat exchanger are provided on the buffer pipeline between the gas-liquid separator and the buffer tank, wherein the pressure reducing valve is arranged at one end of the buffer pipeline close to the gas-liquid separator, and the buffer heat exchanger is arranged between the pressure reducing valve and the buffer tank.

[0012] Furthermore, a reflux pipeline is provided between the gas-liquid separator and the main reaction device, the inlet end of the reflux pipeline is connected to the gas-liquid separator, a corresponding reflux port is added to the feed pipe of the main reaction device, the outlet end of the reflux pipeline is connected to the feed pipe of the main reaction device through the reflux port, and a corresponding reflux device is provided on the reflux pipeline, including a reflux pump, a reflux valve, a reflux check valve, a reboiler and a reflux flowmeter. The above components are arranged in sequence from the inlet end to the outlet end of the reflux pipeline and are connected in series on the reflux pipeline.

[0013] The utility model piperonal continuous oxidation equipment utilizes nanobubble technology. Compared with traditional air oxidation, the nanobubble oxidation has a larger bubble surface area, a longer existence time, a greater solubility, a high mass transfer efficiency, and can produce highly oxidizing free radicals, thereby making the oxidation reaction more efficient. The utility model piperonal continuous oxidation equipment has a more stable reaction, higher production efficiency, and more stable equipment. At the same time, its structure is simpler, the cost is lower, and the economic benefits are higher. No other by-products are produced in the reaction, and it is safer and more environmentally friendly. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 It is a schematic diagram of the structure of the utility model;

[0015] Figure 2 For this utility model Figure 1 A schematic structural diagram of a nano bubble disperser 7;

[0016] Figure 3 For this utility model Figure 1 A schematic structural diagram of a microchannel reactor 8;

[0017] Explanation of the markings in the figure: 1. Raw material kettle; 11. Kettle valve; 12. Feed pump; 13. Feed heat exchanger; 14. Feed flow meter; 15. Feed check valve; 16. Feed valve; 2. Gas supply machine; 21. Inlet valve; 22. Supply pressure gauge; 23. Supply check valve; 24. Outlet valve; 25. Gas supply machine pressure gauge; 3. Receiving kettle; 31. Discharge heat exchanger; 32. Discharge flow meter; 33. Discharge valve; 34. Pressure reducing valve; 35. Buffer heat exchanger; 36. Buffer tank; 4. Reflux pump; 41. Reflux valve; 42. Reflux check valve; 43. Reboiler; 44. Reflux flow meter; 5. Main Reaction box; 51. air inlet; 52. pressure sensor; 53. first pressure-temperature sensor; 54. sight glass; 55. feed pipe; 56. reflux port; 6. feed pipeline; 61. air inlet pipeline; 62. discharge pipeline 62; 63. buffer pipeline; 64. reflux pipeline; 7. nano bubble disperser; 71. dispersion membrane; 72. nano channel; 8. micro channel reactor; 81. reaction chamber; 82. reaction channel; 83. interlayer; 84. channel baffle; 85. arc baffle; 86. interlayer inlet; 87. interlayer outlet; 88. shell; 9. gas-liquid separator; 91. second pressure-temperature sensor. DETAILED DESCRIPTION

[0018] In order to better understand the purpose, structure and function of the utility model, the following is a further detailed description of a piperonal continuous oxidation device of the utility model in conjunction with the accompanying drawings.

[0019] like Figure 1-3 As shown, the piperonal continuous oxidation device of the utility model includes a feeding device, a main reaction device, an air intake device and a storage device, and the components of each device are connected through corresponding pipelines, wherein the feeding device is arranged at the front end of the main reaction device, and the two are connected through a feeding pipeline 6, the feeding device conveys reaction raw materials to the main reaction device through the feeding pipeline 6, the main reaction device is connected to the air intake device through the air intake pipeline 61, and the air intake device conveys the required reaction gas to the main reaction device through the air intake pipeline 61, and the main reaction device is connected to the storage device through the discharge pipeline 62, and the finished product prepared after the reaction of the main reaction device is completed is transported to the corresponding storage device through the discharge pipeline 62, and then stored for subsequent transportation and use. The above devices and pipelines are provided with a plurality of corresponding monitoring devices and control valve bodies, and the monitoring device monitors the reaction operation of the equipment in real time, which is convenient for the staff to control the equipment and the reaction situation, and is also more conducive to the investigation of safety hazards and the reduction of dangerous accidents. The control valve body is more convenient for the staff to control the equipment and its operation.

[0020] The main reaction device comprises a main reaction box 5, in which a nanobubble disperser 7 and a microchannel reactor 8 are arranged in the inner cavity of the main reaction box 5, wherein the nanobubble disperser 7 is arranged at the lower part of the main reaction box 5, and the microchannel reactor 8 is arranged at the upper part of the main reaction box 5 above the nanobubble disperser 7. A corresponding air inlet 51 is arranged at the bottom of the main reaction box 5 below the nanobubble reactor. The main reaction device is connected with the air inlet device through the air inlet 51, and the air inlet device provides the nanobubble reactor with reaction gas through the air inlet 51, so that the nanobubble reactor regenerates a large number of nanobubbles wrapped with reaction gas. A corresponding feed pipe 55 is arranged on the side wall of the main reaction box 5 between the nanobubble disperser 7 and the microchannel reactor 8. The feed pipe 55 is provided on the side wall of the main reaction box 5 between the nanobubble disperser 7 and the microchannel reactor 8. 5 is connected to the inner cavity of the main reaction box 5, the main reaction device is connected to the feeding device through the feeding pipe 55, the feeding device provides the main reaction device with reaction raw materials through the feeding pipe 55, the reaction raw materials and the nanobubbles generated in the nanobubble reactor meet and mix, and then react with the reaction gas in the nanobubbles, so as to obtain the finished product to be prepared, the microchannel reactor 8 is arranged above the nanobubble reactor, the reaction raw materials and the nanobubbles transported by the feeding pipe 55 are mixed and then enter the microchannel reactor 8, the two can be more fully and effectively mixed and oxidized in the microchannel reactor 8, and the reaction process in the microchannel reactor 8 becomes a continuous flow, so that the production efficiency of the product is higher, and a corresponding gas is arranged above the main reaction box 5. Liquid separator 9, gas-liquid separator 9 is connected with the inner cavity of main reaction box 5, the reaction liquid after reaction in microchannel reactor 8 is separated into gas and liquid under the action of gas-liquid separator 9, gas-liquid separator 9 separates unreacted waste gas from reaction liquid, the reaction liquid remaining after waste gas separation is finished material, gas-liquid separator 9 is connected with storage device through discharge pipeline 62, the finished material after gas-liquid separation is transported to corresponding storage device through discharge pipeline 62, a corresponding sight glass 54 is provided on the side wall of main reaction box below microchannel reactor 8, sight glass 54 is provided between nano bubble disperser 7 and microchannel reactor 8, it is convenient to observe the material state in main reaction box, between nano bubble disperser 7 and microchannel reactor 8 A corresponding pressure sensor 52 is provided on the side wall of the main reaction box between the two, and the pressure sensor 52 can be used to detect the gas pressure between the two in real time. The sight glass 54 and the pressure sensor 52 are both arranged above the feed pipe 55, and a corresponding first pressure-temperature sensor 53 is provided at the bottom end of the side wall of the main reaction box, and the first pressure-temperature sensor 53 can be used to detect the temperature and pressure in the main reaction box in real time. A corresponding second pressure-temperature sensor 91 is provided on the gas-liquid separator 9, and the second pressure-temperature sensor 91 can be used to detect the temperature and pressure in the gas-liquid separator 9 in real time. Through the synergistic effect of the above monitoring devices, it is convenient for the staff to better monitor and control the main reaction box and avoid the occurrence of dangerous conditions during the reaction process.

[0021] The nanobubble disperser 7 is provided with a corresponding dispersion membrane 71, and a plurality of nano-passages are provided on the dispersion membrane 71. The reaction gas provided by the air intake device is converted into a large number of nano-bubbles under the action of the dispersion membrane 71. The reaction gas is wrapped in the nano-bubbles. The nano-bubbles leave the nano-bubble disperser 7 along the nano-passages and then enter the main reaction box 5.

[0022] The microchannel reactor 8 includes a plurality of microchannels, and the plurality of microchannels that are not interconnected are evenly distributed in an array in the inner cavity of a shell 88 of the microchannel reactor 8. An interlayer 83 is provided between the microchannel and the shell 88. An interlayer inlet 86 connected to the interlayer 83 is provided at the upper portion of one side wall of the shell 88, and an interlayer outlet 87 connected to the interlayer 83 is provided at the lower portion of the other side wall corresponding thereto. The microchannel reactor 8 is externally connected to a corresponding heat exchange device through the interlayer inlet 86 and the interlayer outlet 87. The heat exchange medium of the heat exchange device enters the interlayer 83 of the microchannel reactor 8 through the interlayer inlet 86 to exchange heat with the microchannel. The heat exchange medium after heat exchange leaves the interlayer 83 of the microchannel reactor 8 through the interlayer outlet 87 and returns to the heat exchange device. Such a reciprocating cycle keeps the microchannel reactor 8 at an appropriate temperature, and the reaction in the microchannel can be more stable. The microchannel includes a reaction chamber 81. A plurality of reaction chambers 81 are connected in series to form a microchannel. In this embodiment, five rhombus reaction chambers 81 are vertically connected in series to form a vertical microchannel. Each reaction chamber 81 is provided with corresponding reaction channels 82 at both ends. The two upper and lower adjacent reaction chambers 81 are interconnected through the corresponding reaction channels 82. In each reaction chamber 81, a pair of channel baffles 84 are provided above the reaction channel 82 at the lower end. The two ends of the two channel baffles 84 are respectively connected to the walls of the corresponding reaction chambers 81 on both sides, and a certain gap channel is left between the two channel baffles 84. The slit channel corresponds to the reaction channel 82 below, and a corresponding arc baffle 85 is provided above the slit channel. The arc baffle 85 has a certain curvature bending in the direction of the slit channel, and there is a certain side gap between the two sides of the arc baffle 85 and the corresponding channel baffle 84. The reaction channel 82 at the lower end of the reaction chamber 81 is the entrance of the reaction chamber 81. The reaction liquid enters the reaction chamber 81 from the entrance of the reaction chamber 81, and then rushes to the arc baffle 85 through the slit channel under the action of the two channel baffles 84. It is broken up under the obstruction of the arc baffle 85 and flows to the side gaps on both sides of the arc baffle 85, and flows to the top of the arc baffle 85 in the reaction chamber 81. The disturbance coefficient of the reaction liquid is The process is amplified, the oxidation rate of the reaction liquid is increased, and the oxidation is more complete. The reaction channel 82 at the upper end of the reaction chamber 81 is the outlet of the reaction chamber 81. The reaction liquid above the arc baffle 85 leaves the corresponding reaction chamber 81 through the outlet of the reaction chamber 81. The lower end reaction channel 82 of the bottommost reaction chamber 81 is the microchannel inlet. The reaction liquid in the main reaction box 5 below the microchannel reactor 8 enters the microchannel through this inlet. The reaction liquid passes through the five reaction chambers 81 connected in series from bottom to top in the microchannel. The upper end reaction channel 82 of the topmost reaction chamber 81 is the microchannel outlet. The reaction liquid finally leaves the microchannel reactor 8 through the microchannel outlet. In this process, the reaction raw materials in the reaction liquid are fully oxidized.

[0023] The feeding device includes a raw material kettle 1. In this embodiment, a raw material kettle 1 with a stirring function is used, which can make the reaction raw materials dispersed more finely, thereby increasing their contact area and being more conducive to their oxidation reaction. The raw material kettle 1 is connected to the feed pipe 55 of the main reaction device through a feed pipeline 6, and the inlet of the feed pipeline 6 is connected to the discharge port of the raw material kettle 1, and the outlet of the feed pipeline 6 is connected to the feed pipe 55. The reaction raw materials in the raw material kettle 1 are transported to the feed pipe 55 through the feed pipeline 6, and then are input into the main reaction device. A corresponding material kettle valve 11 is provided at the discharge port of the raw material kettle 1 to control its discharge. A corresponding feed pump 12, a feed heat exchanger 13 and a feed flow meter 14 are provided on the feed pipeline 6 between the raw material kettle 1 and the feed pipe 55, wherein the feed pump 12 is arranged at one end of the feed pipeline 6 close to the raw material kettle 1 to provide a heat exchanger 13 and a feed flow meter 14 for the reaction raw materials in the feed pipeline 6. Power is used to transport the reaction raw materials to the main device. The feed flow meter 14 is arranged at one end of the feed pipeline 6 close to the feed pipe 55. It monitors the flow rate of the reaction raw materials in the feed pipeline 6 in real time, so that the staff can better control the feed rate of the main device. A feed heat exchanger 13 is provided between the feed pump 12 and the feed flow meter 14. The feed heat exchanger 13 is used to exchange heat for the reaction raw materials in the feed pipeline 6, which makes it more convenient for the staff to control the feed temperature of the reaction raw materials. A feed check valve 15 and a feed valve 16 are provided in sequence on the feed pipeline 6 between the feed flow meter 14 and the feed pipe 55. The feed check valve 15 can prevent the raw materials in the feed pipeline 6 from flowing back toward its feed port, thereby preventing the reaction raw materials of the main device from flowing back toward the raw material kettle 1. The feed valve 16 can better control the feeding speed of the main device.

[0024] The air intake device includes an air supply machine 2, which is connected to the main reaction box 5 through an air intake pipeline 61. The inlet of the air intake pipeline 61 is connected to the air outlet of the air supply machine 2, and the outlet of the air intake pipeline 61 is connected to the air inlet 51 of the main reaction box 5. An air intake valve 21, a pressure gauge 22, a gas supply check valve 23 and an air outlet valve 24 are sequentially arranged on the air intake pipeline 61 between the air supply machine 2 and the main reaction box 5, wherein the air intake valve 21 and the air outlet valve 24 are respectively arranged at the inlet and outlet of the air intake pipeline 61. The output of the gas in the air supply machine 2 can be controlled by the air intake valve 21, and the flow of the gas into the main reaction box 5 can be controlled by the air outlet valve 24. The pressure gauge 22 is arranged on the side of the air intake pipeline 61 close to the air intake valve 21, and it controls the air supply pressure in the air intake pipeline 61. Real-time monitoring is carried out to ensure the gas supply of the entire equipment while also supervising the gas supply safety of the gas supply equipment in real time. The gas supply one-way valve 23 is arranged between the supply pressure gauge 22 and the outlet valve 24 to prevent the material in the main reaction device from flowing back into the gas intake device through the gas intake pipeline 61, thereby protecting the various components of the gas intake device. The gas intake device introduces oxygen or air with a high oxygen content into the main reaction device through the gas supply machine 2. In the piperonal oxidation process, there are many types of gas supply machines 2 that can be used, such as oxygen generators, pressure tanks, etc. In this embodiment, an oxygen generator is used as the gas supply machine 2, and a corresponding gas supply machine pressure gauge 25 is arranged on the gas supply machine 2. The gas supply machine pressure gauge 25 can be used to monitor the pressure of the gas supply machine 2 in real time, so that the staff can better control the gas intake device.

[0025] The storage device includes a receiving kettle 3, which is connected to the gas-liquid separator 9 through a discharge pipeline 62. The inlet end of the discharge pipeline 62 is connected to the liquid outlet of the gas-liquid separator 9, and the outlet end is connected to the receiving kettle 3. The finished material separated by the gas-liquid separator 9 is transported to the receiving kettle through the discharge pipeline 62, and is stored for subsequent transportation and use. A corresponding discharge valve 33 is provided at the inlet end of the discharge pipeline 62. The discharge valve 33 can effectively control the output flow rate of the finished material reaction liquid in the gas-liquid separator 9. A discharge flowmeter 32 and a discharge heat exchanger 31 are provided in sequence on the discharge pipeline 62 between the discharge valve 33 and the receiving kettle 3. The discharge flowmeter 32 monitors the discharge rate of the finished material reaction liquid in the discharge pipeline 62 in real time, and the discharge heat exchanger 31 cools the finished material reaction liquid in the discharge pipeline 62 for subsequent centralized storage and transportation of the receiving kettle 3.

[0026] The gas-liquid separator 9 is connected to the buffer tank 36 through a buffer pipeline 63, and the inlet end of the buffer pipeline 63 is connected to the gas outlet of the gas-liquid separator 9. The waste gas and excess gas in the gas-liquid separator 9 are discharged into the buffer tank 36 through the buffer pipeline 63. A pressure reducing valve 34 and a buffer heat exchanger 35 are also provided on the buffer pipeline 63 between the gas-liquid separator 9 and the buffer tank 36. The pressure reducing valve 34 is arranged at one end of the buffer pipeline 63 close to the gas-liquid separator 9, which can effectively control the discharge of the gas in the gas-liquid separator 9. The buffer heat exchanger 35 is arranged between the pressure reducing valve 34 and the buffer tank 36 to cool the gas discharged from the gas-liquid separator 9. The cooled gas is transported to the buffer tank 36 for buffering through the buffer pipeline 63. In this way, the liquid brought out of the gas can be recovered and the excess gas in the gas-liquid separator 9 can be discharged, thereby ensuring the gas-liquid balance in the gas-liquid separator 9, thereby making the reaction of the overall equipment more stable and safer, and reducing the probability of accidents.

[0027] A reflux pipeline 64 is provided between the gas-liquid separator 9 and the main reaction device. The inlet end of the reflux pipeline 64 is connected to the gas-liquid separator 9, and the outlet end thereof is connected to the feed pipe 55 of the main reaction device. The feed pipe 55 is provided with a corresponding reflux port 56. The feed pipe 55 is connected to the reflux pipeline 64 through the reflux port 56. The reflux pipeline 64 is provided with a corresponding reflux device, including a reflux pump 4, a reflux valve 41, a reflux check valve 42, a reboiler 43 and a reflux flowmeter 44. The above components are connected in series on the reflux pipeline 64, and are arranged in sequence from the inlet end to the outlet end of the reflux pipeline 64. The reflux pump 4 is a power device for the reaction liquid in the reflux pipeline 64. The reaction liquid in the gas-liquid separator 9 flows to the feed pipe 55 of the main reaction device through the reflux pipeline 64 under the action of the reflux pump 4. The flow rate of the reaction liquid in the reflux pipeline 64 can be effectively controlled by the reflux valve 41 at the rear end of the reflux pump 4. The rear end of the reflux valve 41 is a reflux check valve 42. The reflux check valve 42 is a check valve 42. The check valve 42 can effectively prevent the reaction liquid in the reflux line 64 from flowing toward the gas-liquid separator 9 at its inlet end, so that it can only flow toward the outlet end of the reflux line 64, and prevent the unreacted reaction raw materials in the feed pipe 55 from flowing into the gas-liquid separator 9 through the reflux line 64, thereby affecting the reaction quality of the overall equipment. The rear end of the reflux check valve 42 is a reboiler 43, and the reboiler 43 can reheat the reaction liquid in the reflux line 64. The temperature of the reaction liquid in the reflux line 64 can be better controlled by the reboiler 43 to prevent the quality of the secondary reaction from being affected by its temperature inappropriateness. The rear end of the reboiler 43 is a reflux flowmeter 44, and the reflux flowmeter 44 monitors the flow rate of the reaction liquid in the reflux line 64 in real time, which is convenient for the staff to control the reaction liquid delivery flow rate of the reflux line 64 in real time, so that the reaction can be carried out better. The setting of the reflux line 64 increases the circulation amount of the reaction liquid, and the reaction liquid can return to the main reaction device for multiple times, and its oxidation can be more sufficient.

[0028] When in use, firstly, the reaction raw materials are added into the raw material kettle 1. In this embodiment, a mixed solution of piperonyl alcohol and water is used as the reaction raw material. The reaction raw materials in the raw material kettle 1 are transported to the main reaction box 5 through the feed pipe 6 and the feed pipe 55. At the same time, the gas supply machine 2 passes a large amount of high oxygen content gas into the main reaction box 5 through the air inlet 51 through the air inlet pipe 61 as the reaction gas. The reaction gas forms a large amount of nano bubbles under the action of the nano bubble disperser 7. The reaction gas is wrapped by the nano bubbles and passed into the reaction raw materials of the main reaction box 5. The nano bubbles and the reaction raw materials are fully mixed to form a reaction solution. The oxygen in the bubbles undergoes an oxidation reaction with the piperonyl alcohol in the reaction raw materials to form piperonal. The reaction liquid enters the microchannel reactor 8 to undergo a more sufficient oxidation reaction, so that more piperonal is produced in the reaction liquid. The reaction liquid enters the gas-liquid separator 9, and the gas-liquid separation technology is used to separate the unreacted excess waste gas from the reaction liquid. The remaining piperonal finished material after the excess waste gas in the reaction liquid is separated. The reaction liquid enters the gas-liquid separator 9 above the main reaction box 5 upward, and the gas-liquid separation technology is used to separate the unreacted excess waste gas from the reaction liquid. The remaining after the waste gas is separated is the piperonal finished product. The waste gas and the finished product are cooled respectively. The cooled waste gas is transported to the buffer tank 36 through the buffer pipeline 63. The liquid in the waste gas is recovered separately for subsequent reuse. The cooled finished product is transported to the receiving kettle 3 through the discharge pipeline 62. The finished product is more convenient for storage after cooling. After the finished product is concentrated in the receiving kettle 3, it will be transported and used later. In this process, the reaction liquid after the excess waste gas is separated by the gas-liquid separator 9 is transported again through the reflux pipeline 64 and the feed pipe 55 under the action of the reflux pump 4. The piperonyl alcohol in the reaction solution is passed into the main reaction box 5, and nanobubbles are introduced into the main reaction box again through the nanobubble disperser 7, so that the unreacted piperonyl alcohol remaining in the main reaction box 5 is subjected to oxidation reaction again, and gas-liquid separation is performed on the piperonyl alcohol after it is fully oxidized again in the microchannel reactor 8. This cycle is repeated for multiple times, so that the oxidation of piperonyl alcohol in the reaction solution is more thorough, and the piperonyl alcohol residue is less, so that more piperonal can be generated, and the oxidation ratio of piperonal is improved. During the operation of the overall equipment, each pressure and temperature monitoring device monitors the pressure and temperature of each pipeline and corresponding device in real time to prevent the reaction efficiency from being affected by too low pressure, or the danger from being caused by too high pressure.

[0029] The piperonal continuous oxidation device of the utility model uses the nano bubble disperser 7 and the microchannel reactor 8 to allow the reaction raw materials and the reaction gas to be more fully and effectively mixed and oxidized, so that the oxidation reaction becomes sustainable. The piperonal continuous oxidation device of the utility model has a simple structure, low cost, and higher production efficiency, so that it has higher economic benefits. It does not produce other by-products, the reaction is more stable, and it is safer and more environmentally friendly.

[0030] It is understood that the present invention is described by some embodiments, and those skilled in the art are aware that various changes or equivalent substitutions may be made to these features and embodiments without departing from the spirit and scope of the present invention. In addition, under the teachings of the present invention, these features and embodiments may be modified to adapt to specific circumstances and materials without departing from the spirit and scope of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed herein, and all embodiments falling within the scope of the claims of this application are within the scope of protection of the present invention.

Claims

1. A piperonal continuous oxidation device, characterized in that, The invention comprises a feeding device, a main reaction device, an air intake device and a storage device, and the components of each device are connected through corresponding pipelines. The feeding device is connected to the main reaction device through a feeding pipeline (6) to transport reaction raw materials to it, the air intake device is connected to the main reaction device through an air intake pipeline (61) to transport reaction gas to it, and the main reaction device is connected to the storage device through a discharge pipeline (62). The finished product after the reaction is completed is transported to the corresponding storage device for storage through the discharge pipeline (62). The above devices and pipelines are provided with a plurality of corresponding monitoring devices and control valve bodies.

2. The piperonal continuous oxidation device according to claim 1, characterized in that: The main reaction device comprises a main reaction box (5), wherein a nanobubble disperser (7) and a microchannel reactor (8) are arranged in the inner cavity of the main reaction box (5), wherein the nanobubble disperser (7) is arranged at the lower part of the inner cavity of the main reaction box (5), and the microchannel reactor (8) is arranged above the nanobubble disperser (7); an air inlet (51) corresponding to the nanobubble disperser (7) is arranged at the bottom of the main reaction box (5); the main reaction device is connected to the air inlet (51); and a gas inlet (51) corresponding to the main reaction device is arranged on the side wall of the main reaction box (5) between the nanobubble disperser (7) and the microchannel reactor (8). A feed pipe (55) is connected to the inner cavity of the reaction box (5); the main reaction device is connected to the feed device through the feed pipe (55); a corresponding sight glass (54) and a pressure sensor (52) are provided on the side wall of the main reaction box between the microchannel reactor (8) and the feed pipe (55); a gas-liquid separator (9) connected to the inner cavity of the main reaction box (5) is provided above the main reaction box (5); the gas-liquid separator (9) is connected to the storage device through a discharge pipeline (62); a corresponding first pressure-temperature sensor (53) is provided at the bottom end of the side wall of the main reaction box; and a corresponding second pressure-temperature sensor (91) is provided on the gas-liquid separator (9).

3. The piperonal continuous oxidation device according to claim 2, characterized in that: The feeding device comprises a raw material kettle (1), the raw material kettle (1) is connected to the main reaction device through a feeding pipeline (6), the inlet of the feeding pipeline (6) is connected to the discharge port of the raw material kettle (1), the outlet of the feeding pipeline (6) is connected to the feeding pipe (55) of the main reaction device, a corresponding kettle valve (11) is arranged at the discharge port of the raw material kettle (1), and a corresponding feed pipe (55) is arranged on the feeding pipeline (6) between the raw material kettle (1) and the feeding pipe (55). A feed pump (12), a feed heat exchanger (13) and a feed flow meter (14), wherein the feed pump (12) is arranged at one end close to the raw material kettle (1), the feed flow meter (14) is arranged at one end close to the feed pipe (55), a feed heat exchanger (13) is arranged between the feed pump (12) and the feed flow meter (14), and a feed check valve (15) and a feed valve (16) are arranged in sequence between the feed flow meter (14) and the feed pipe (55).

4. The piperonal continuous oxidation device according to claim 2, characterized in that: The air intake device comprises an air supply machine (2), the air supply machine (2) is connected to the main reaction box (5) through an air intake pipeline (61), the inlet of the air intake pipeline (61) is connected to the air outlet of the air supply machine (2), and the outlet of the air intake pipeline (61) is connected to the air intake (51) of the main reaction box (5), and an air intake valve (21), a pressure gauge (22), an air supply check valve (23) and an air outlet valve (24) are sequentially arranged on the air intake pipeline (61) between the air supply machine (2) and the main reaction box (5), wherein the air intake valve (21) and the air outlet valve (24) are respectively arranged at the inlet and outlet of the air intake pipeline (61), the pressure gauge (22) is arranged on the air intake pipeline (61) on a side close to the air intake valve (21), and the air supply check valve (23) is arranged between the pressure gauge (22) and the air outlet valve (24).

5. The piperonal continuous oxidation device according to claim 2, characterized in that: The material storage device comprises a receiving kettle (3), the receiving kettle (3) is connected to the gas-liquid separator (9) via a discharge pipeline (62), the inlet end of the discharge pipeline (62) is connected to the liquid outlet of the gas-liquid separator (9), a corresponding discharge valve (33) is arranged at the inlet end of the discharge pipeline (62), and a discharge flow meter (32) and a discharge heat exchanger (31) are arranged between the discharge valve (33) and the receiving kettle (3).

6. The piperonal continuous oxidation device according to claim 2, characterized in that: The gas-liquid separator (9) is connected to a buffer tank (36) via a buffer pipeline (63); the inlet end of the buffer pipeline (63) is connected to the gas outlet of the gas-liquid separator (9); a pressure reducing valve (34) and a buffer heat exchanger (35) are provided on the buffer pipeline (63) between the gas-liquid separator (9) and the buffer tank (36); the pressure reducing valve (34) is provided at one end of the buffer pipeline (63) close to the gas-liquid separator (9); and the buffer heat exchanger (35) is provided between the pressure reducing valve (34) and the buffer tank (36).

7. The piperonal continuous oxidation device according to claim 2, characterized in that: A reflux pipeline (64) is provided between the gas-liquid separator (9) and the main reaction device. The inlet end of the reflux pipeline (64) is connected to the gas-liquid separator (9). A corresponding reflux port (56) is provided on the feed pipe (55) of the main reaction device. The outlet end of the reflux pipeline (64) is connected to the feed pipe (55) of the main reaction device through the reflux port (56). The reflux pipeline (64) is provided with a corresponding reflux device, including a reflux pump (4), a reflux valve (41), a reflux check valve (42), a reboiler (43) and a reflux flowmeter (44). The above components are arranged in sequence from the inlet end to the outlet end of the reflux pipeline (64) and are connected in series to the reflux pipeline (64).

8. The piperonal continuous oxidation device according to claim 2, characterized in that: The nano bubble disperser (7) is provided with a corresponding dispersion membrane (71), and a plurality of nano passages are provided on the dispersion membrane (71).

9. The piperonal continuous oxidation device according to claim 2, characterized in that: The microchannel reactor (8) comprises a plurality of microchannels which are not interconnected, and the plurality of microchannels are evenly distributed in an array in the inner cavity of a shell (88) of the microchannel reactor (8). An interlayer (83) is provided between the microchannel and the shell (88). An interlayer inlet (86) which is connected to the interlayer (83) is provided at the upper portion of a side wall of the shell (88), and an interlayer outlet (87) which is connected to the interlayer (83) is provided at the lower portion of the side wall opposite thereto. The microchannel reactor (8) is externally connected to a corresponding heat exchange device via the interlayer inlet (86) and the interlayer outlet (87). The microchannel comprises a reaction chamber (81), and the plurality of reaction chambers (81) are connected in series to form a microchannel, and each reaction chamber (81) is provided with a heat exchanger at both upper and lower ends. The corresponding reaction channels (82) are interconnected between two upper and lower adjacent reaction chambers (81) through the corresponding reaction channels (82). In each reaction chamber (81), a pair of channel baffles (84) are provided above the reaction channel (82) at the lower end thereof. A slit channel corresponding to the reaction channel (82) below the lower end thereof is provided between the two channel baffles (84). A corresponding arc-shaped baffle (85) is provided above the slit channel. Side gaps are provided between the two sides of the arc-shaped baffle (85) and the corresponding channel baffle (84). The lower reaction channel (82) of the bottommost reaction chamber (81) is a microchannel inlet, and the upper reaction channel (82) of the topmost reaction chamber (81) is a microchannel outlet.

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