A TMBP reaction device and synthesis method thereof

Abstract

The present invention relates to the technical field of TMBP preparation, and in particular to a TMBP reaction device and a synthesis method thereof. The reaction device comprises a sealed tank body, a heating mechanism is arranged inside the tank body, and the tank body is divided into a gas phase area and a liquid phase area from top to bottom. A hollow rotating shaft is arranged at the center of the tank body, a motor is connected to the top of the hollow rotating shaft, an air intake mechanism is arranged inside, an air intake hole connected to the gas phase area is arranged above the side wall, a gas distribution mechanism is arranged below the side wall, and the gas distribution mechanism comprises a plurality of hollow and horizontally arranged spiral blades, the spiral blades are sealed and connected to the hollow rotating shaft, an outer side wall is provided with an outlet pipe perpendicular to its normal, and a one-way nozzle is arranged on the outlet pipe. The overall structure of the present invention is compact, the footprint is small, the stirring effect is good, the oxygen in the gas phase area can be dispersed into the liquid phase area, the gas distribution mechanism has both gas distribution and stirring effects, greatly improves the oxygen content and dispersion uniformity in the liquid phase, improves the reaction efficiency, and shortens the reaction time.

Description

Technical Field

[0001] The invention relates to the technical field of TMBP preparation, and in particular to a TMBP reaction device and a synthesis method thereof. Background Art

[0002] Liquid crystal intermediate 3,3',5,5'-tetramethylbiphenol (TMBP) can be used as a modified monomer for polyester, polyurethane, polycarbonate, polysulfone, epoxy resin and many other products to manufacture excellent engineering plastics and composite materials; it can also be used as rubber, emulsion antioxidant and plastic antioxidant, as well as dye intermediate or stabilizer for petroleum products. For example, 3,3',5,5'-tetramethylbiphenol diglycidyl ether synthesized from TMBP has low melt viscosity, good sealing, wide operating temperature, no cracking, good operability and fluidity, and is an excellent integrated circuit packaging material.

[0003] Liquid crystal polymer (LCP) synthesized from 3,3',5,5'-tetramethylbiphenol is a high-performance special engineering plastic that has developed rapidly in recent years. It has comprehensive properties such as high strength, high modulus, excellent dimensional stability, insulation, flame retardancy, low linear expansion rate, radiation resistance, and chemical corrosion resistance. It is widely used in electronic parts, home appliance accessories, medical equipment, precision machinery parts, automotive components, and chemical equipment parts. The reported TMBP synthesis methods are mainly the following five according to the different oxidants.

[0004] One is to use hydrogen peroxide as an oxidant. Sagar Sharma et al. synthesized tris(3,5-dimethylpyrazole) copper nitrate, which can catalyze the DMP reaction in the presence of hydrogen peroxide. Zhu Jie from Sichuan University synthesized four metal copper-tetranitrogen complexes to study the kinetics of the reaction of 2,6-dimethylphenol to 3,3',5,5'-tetramethylbiphenylquinone under hydrogen peroxide conditions, proving that the metal complex can catalyze DMP for carbon-carbon coupling. Foreign scholars have used 2,4-di-tert-butylphenol and hydrogen peroxide as raw materials, and obtained 2,2-dihydroxy-3,3',5,5'-tetra-tert-butylbiphenyl through an oxidative condensation reaction at 80°C, alkaline and lauric acid as a catalyst. This method is easy to operate in industry and has low equipment requirements. It has a wide range of sources and has good industrial application prospects.

[0005] The second method is to use inorganic salts such as CuSO4, FeCl3, VOCl3, etc. as oxidants, with a yield of about 45%. The Guangzhou Institute of Chemistry, Chinese Academy of Sciences, uses salt oxidants (CuCl2, Ag2CO3, Fe2SO4, etc.) to first oxidatively couple and synthesize DPQ, and then uses cheap and efficient inorganic reducing agents to reduce TMBP under acidic conditions. This method has mild reaction conditions, fewer by-products, simple synthesis process, no need for oxygen, no special reaction equipment, less equipment investment, and cost savings.

[0006] The third method is oxidation in an organic oxidation system, such as Christophe Boldron et al. oxidized TMBP in the presence of iodobenzene diacetate (PIDA), but the synthesis of organic oxidants is relatively complicated.

[0007] The fourth is to use the light-induced method, such as Mohamed Sarakha and Michele Bolte in France who excited [Co(NH3)5N5] under 365nm ultraviolet light. 2+ , thereby achieving the photoinduction of 2,6-dimethylphenol to produce diphenoquinone and TMBP, but this technology is not yet mature.

[0008] Fifth, using oxygen as an oxidant requires special pressure-resistant reaction equipment. Shigeru Tsuruya et al. introduced oxygen into the copper nitrate-acetonitrile system to obtain an appropriate amount of quinone, and studied the effects of pyridine, piperidine and diethylamine on the oxidative coupling reaction. They found that pyridine is conducive to CC bond coupling, while piperidine and diethylamine promote CO coupling. Jiang Zhongliang from Tongji University in Shanghai used 2,6-di-tert-butylphenol as a raw material for oxidative coupling and reduction to obtain TMBP. This method is simple to operate, has a high yield, and is suitable for industrial production. Another method is to dissolve 2,6-dimethylphenol in an aqueous solution containing a surfactant, introduce oxygen, add a catalyst, and obtain TMBP after post-treatment.

[0009] In general, the process of synthesizing 3,3',5,5'-tetramethylbiphenol using oxygen as an oxidant has certain advantages, but the process requires the use of dedicated reaction equipment in the process of synthesizing 3,3',5,5'-tetramethylbiphenol.

[0010] The patent with application number 202211096016.8 discloses a liquid crystal intermediate 3,3',5,5'-tetramethylbiphenol synthesis process and device thereof. The oxidative coupling reaction is carried out in a reaction tank, and an agitator and a temperature control component are provided in the reaction tank. A reaction liquid outlet is provided at the bottom, and the reaction liquid outlet is connected to a filter tank; the reaction liquid is cleaned and filtered in the filter tank, and the solid after cleaning and filtration is dried to obtain the target product. The above technical scheme has the following problems: First, the reaction tank has a simple structure, oxygen stays above the reaction tank, the oxygen content in the liquid phase is low and the dispersion uniformity is poor, which reduces the reaction efficiency of the oxidative coupling and prolongs the reaction time of the oxidative coupling reaction; secondly, the agitator has a simple structure and poor stirring effect, resulting in different oxidation degrees of the oxidative coupling reaction in different regions of the tank. The region with less contact with oxygen has a low degree of oxidation, while the region with more contact with oxygen is prone to peroxidation, which prolongs the reaction time of the subsequent reduction reaction.

[0011] The patent with application number CN215429056U has developed a gas-liquid reaction device, including a reactor, the reactor is provided with a gas phase inlet pipe and a liquid phase inlet pipe, the gas phase inlet pipe extends into the inner side of the bottom of the reactor and is connected to a gas phase distributor, the gas phase distributor is provided with a plurality of gas outlet holes in the circumference; the stirring shaft of the reactor is provided with a plurality of spirally arranged auger blades, the auger blades are arranged above the gas phase distributor. The gas phase distributor sends the gas out from the gas outlet evenly and contacts and mixes with the liquid in the reactor, the auger blades make the gas rise along the spiral path, extend the gas stroke, increase the contact time between the gas and the liquid, and at the same time the auger blades can make the lower liquid move upward, increase the mixing between the gas and the liquid, the mixing effect is good, and the reaction is thorough. The above technical scheme has the following problems: first, the gas phase distributor is a traditional independent fixed structure, which only has a gas distribution effect but not a stirring effect; second, the gas phase inlet pipe of the gas phase distributor is arranged outside the reactor, which increases the volume of the equipment. Summary of the invention

[0012] In order to solve at least one of the above problems, the present invention provides a TMBP reaction device, including a sealed tank body, a heating mechanism is provided inside the tank body, and the tank body is divided into a gas phase area and a liquid phase area from top to bottom, a hollow rotating shaft is provided at the center of the tank body, the top of the hollow rotating shaft is connected to a motor, an air intake mechanism is provided inside, an air inlet hole connected to the gas phase area is provided above the side wall, a gas distribution mechanism is provided below the side wall, the gas distribution mechanism includes a plurality of hollow and horizontally arranged spiral blades, the spiral blades are sealed and connected to the hollow rotating shaft, the outer side wall is provided with an outlet pipe perpendicular to the normal thereof, and the outlet pipe is provided with a one-way nozzle.

[0013] Preferably, the tank body includes a tank body, a tank cover is provided on the top of the tank body, a bracket, a discharge port and a liquid temperature sensor is provided on the bottom, the tank cover is provided with a liquid feed port, a gas feed port, a gas pressure sensor and the motor, and the liquid feed port, the gas feed port and the discharge port are all provided with switch valves; the hollow rotating shaft includes a rotating shaft body with an opening at the top and a rotating shaft cover fixedly provided at the opening, the air inlet is provided above the rotating shaft body, the rotating shaft cover is sealed and rotatably connected to the tank cover, and is fixedly connected to the output end of the motor.

[0014] Preferably, the air intake mechanism includes a fixed shaft fixed in the tank body, the fixed shaft is coaxially sealed and rotatably connected to the hollow rotating shaft, the fixed shaft is provided with a piston capable of vertically guided sliding, the piston divides the hollow rotating shaft into an upper air intake chamber and a lower sealing chamber connected to the gas distribution mechanism, the piston is axially provided with a one-way air valve for intake of air into the lower sealing chamber, the upper end surface is provided with a cam mechanism capable of vertical reciprocating sliding, the cam mechanism includes a cylindrical cam coaxially fixed to the upper end surface of the piston and a push rod fixed to the inner wall of the hollow rotating shaft.

[0015] Preferably, the piston includes an inner annular plug capable of vertically guiding and sliding along the fixed axis, and an outer annular plug capable of vertically guiding and sliding along the hollow rotating axis, the bottom of the inner annular plug is provided with a first flange rotatably abutting against the inner side wall of the outer annular plug, the top of the outer annular plug is provided with a second flange rotatably abutting against the outer side wall of the inner annular plug, a first sealing bearing is provided between the first flange and the second flange, a first sealing ring is provided on the first flange, a second sealing ring is provided on the second flange, an axial air hole is provided on the inner annular plug, and a one-way air valve is provided in the axial air hole.

[0016] Preferably, the gas distribution mechanism also includes a first connecting ring fixed on the hollow rotating shaft, and a plurality of circular tubes connected to the inner cavity of the hollow rotating shaft are equidistantly arranged on the side wall circumference of the first connecting ring. One end of the spiral blade is close to the inner wall of the tank body, and the other end is provided with an end cover. The end cover is rotatably connected to the circular tube through a second sealing bearing, and the spiral blade is sealed and rotatably connected to the circular tube.

[0017] Preferably, the hollow rotating shaft is provided with a first stirring mechanism, the first stirring mechanism includes a second connecting ring connected to the hollow rotating shaft, a plurality of inclined paddle blades are equidistantly arranged on the circumference of the second connecting ring, a plurality of filter holes are evenly arranged on the inclined paddle blades, and the free ends are close to the inner wall of the tank body, the inclined paddle blades are arranged directly above the spiral blades and correspond one to one with the spiral blades, and the gas distribution mechanism and the first stirring mechanism are axially staggered in multiple arrangements.

[0018] Preferably, a second stirring mechanism is provided at the interface between the gas phase zone and the liquid phase zone, and the second stirring mechanism includes a third connecting ring connected to the hollow rotating shaft, and a plurality of sleeves are equidistantly provided on the circumference of the third connecting ring, and the sleeves can be rotatably connected to the horizontal rotating shaft, and a plurality of flat paddle blades are equidistantly provided on the circumference of one end of the horizontal rotating shaft, and the other end can be rotatably passed through the hollow rotating shaft and connected to the first bevel gear, and a plurality of groups of flat paddle blades are equidistantly laid along the axial direction of the horizontal rotating shaft, and a second bevel gear meshing with the first bevel gear is provided on the fixed shaft.

[0019] The present invention provides a TMBP synthesis method, comprising the following steps:

[0020] Step S100. After dissolving 2,6-dimethylphenol in an organic solvent, add the 2,6-dimethylphenol together with the catalyst into the liquid phase region of the reaction device, introduce oxygen into the gas phase region of the reaction device, maintain the oxygen pressure in the gas phase region at 0.1-2MPa, turn on the motor, drive the hollow shaft and the gas distribution mechanism to rotate, the air intake mechanism draws the oxygen in the gas phase region from the air intake hole of the hollow shaft into the spiral blade of the gas distribution mechanism, and then flows out from the air outlet pipe of the spiral blade into the liquid phase region, the spiral blade rotates with the flow of oxygen inside it, and at the same time revolves with the rotation of the hollow shaft, the spiral blade efficiently stirs and mixes the reaction materials in the liquid phase region through rotation and revolution, heats the reaction materials in the liquid phase region through the heating mechanism, performs oxidative coupling reaction at 120-200°C for 30-120min, discharges the material after the reaction is completed, and obtains a reaction completed liquid;

[0021] Step S200. Add deionized water to the reaction solution, stir and mix well, then add the mixture together with the reducing agent into the jacketed reactor, start stirring and heat, and perform reduction reaction at 20-80° C. for 1-6 hours. After the reaction is completed, obtain a reaction product;

[0022] Step S300: Filter the reaction product and wash with water to remove the reducing agent, then cool it down to crystallize solid particles, and recrystallize the solid particles to obtain TMBP.

[0023] Preferably, in step S100, the organic solvent is at least one of methanol, ethanol, tetrahydrofuran, dichloromethane, ethyl acetate, dioxane, isopropanol, acetonitrile, cyclohexanol, butanol, isobutanol, pentanol, octanol, toluene, and xylene; the catalyst is at least one of potassium hydroxide, sodium hydroxide, sodium carbonate, potassium carbonate, lithium hydroxide, cesium carbonate, potassium bicarbonate, sodium bicarbonate, sodium methoxide, sodium ethoxide, sodium tert-butoxide, potassium tert-butoxide, diisopropylamine, triethylamine, and tetramethylethylenediamine; in step S200, the reducing agent is at least one of sodium dithionite, sodium borohydride, hydrogen, and sodium bisulfite.

[0024] Preferably, in step S100, the mass ratio of 2,6-dimethylphenol to the organic solvent is 1:(0.5-5); the mass ratio of 2,6-dimethylphenol to the catalyst is 1:(0.005-0.1); in step S200, the mass ratio of the reaction completion liquid, deionized water and the reducing agent is 25:(20-50):(0.5-10).

[0025] Compared with the prior art, the present invention has the following beneficial technical effects:

[0026] 1. A gas distribution mechanism is provided in the tank body. The spiral blades on the gas distribution mechanism can rotate and revolve with the rotation of the hollow shaft, which can not only evenly distribute the oxygen in the liquid phase, but also efficiently stir the reaction materials. It has the dual functions of gas distribution and stirring, which improves the reaction efficiency and shortens the reaction time of the oxidative coupling reaction. At the same time, it also avoids overoxidation of the coupling reaction and shortens the reaction time of the subsequent reduction reaction.

[0027] 2. The air inlet mechanism of the gas phase distribution mechanism is arranged inside the hollow rotating shaft, and the overall structure is compact and occupies a small area;

[0028] 3. The air intake mechanism uses a cam mechanism and a piston to intermittently inject air into the gas distribution mechanism, which can increase the oxygen ejection intensity and further improve the stirring and dispersion effect of oxygen in the liquid phase; the piston is decomposed into an inner annular plug and an outer annular plug that can be rotatably connected, which can eliminate the rotational friction between the piston and the hollow shaft, reduce the wear of the piston, and increase the service life of the piston;

[0029] 4. The first stirring mechanism can further improve the stirring effect of the reaction materials in the liquid phase region, and at the same time can refine the oxygen bubbles in the liquid phase region, thereby improving the reaction efficiency of the oxidative coupling reaction, avoiding overoxidation, and shortening the reaction time;

[0030] 5. The second stirring mechanism can increase the oxygen exchange rate at the gas-liquid interface, further improve the reaction efficiency of the coupling reaction and avoid overoxidation, thus shortening the reaction time;

[0031] In summary, the overall structure of the present invention is compact, occupies a small area, has a good stirring effect, can disperse the oxygen in the gas phase into the liquid phase, and the gas distribution mechanism has both gas distribution and stirring effects, which greatly improves the oxygen content and dispersion uniformity in the liquid phase, improves the reaction efficiency, and shortens the reaction time. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1 It is a structural schematic diagram of the present invention;

[0033] Figure 2 It is a schematic diagram of the structure of the tank;

[0034] Figure 3 It is a structural schematic diagram of a hollow shaft;

[0035] Figure 4 It is a structural schematic diagram of the air intake mechanism;

[0036] Figure 5 It is a schematic diagram of the structure of the piston;

[0037] Figure 6 is a schematic diagram of the structure of the gas distribution mechanism;

[0038] Figure 7 is a structural schematic diagram of a first stirring mechanism;

[0039] Figure 8 It is a structural schematic diagram of the second stirring mechanism.

[0040] 1. Tank body, 11. Tank body, 12. Tank cover, 13. Bracket, 14. Discharge port, 15. Liquid phase temperature sensor, 16. Liquid phase feed port, 17. Gas phase feed port, 18. Gas phase pressure sensor, 2. Heating mechanism, 3. Hollow shaft, 31. Shaft body, 311. Air inlet, 32. Shaft cover, 4. Motor, 5. Air inlet mechanism, 51. Fixed shaft, 52. Piston, 521. Inner annular plug, 5211. First flange, 5212. First sealing ring, 5213. Axial air hole, 522. Outer annular plug, 5221. Second flange, 5222. Second sealing ring, 523. First sealing bearing, 53 .One-way air valve, 54. Cam mechanism, 541. Cylindrical cam, 542. Push rod, 6. Gas distribution mechanism, 61. First connecting ring, 62. Round tube, 63. Second sealed bearing, 64. End cover, 65 Spiral blade, 66. Air outlet pipe, 67. One-way nozzle, 7. First stirring mechanism, 71. Second connecting ring, 72. Oblique paddle blade, 721. Filter hole, 8. Second stirring mechanism, 81. Third connecting ring, 82. Bushing, 83. Horizontal rotating shaft, 84. Flat paddle blade, 85. First bevel gear, 86. Second bevel gear, 10. Gas phase region, 20. Liquid phase region, 30. Upper air inlet chamber, 40. Lower sealing chamber. DETAILED DESCRIPTION

[0041] In order to more clearly understand the above-mentioned purpose, features and advantages of the present invention, the present invention is further described in detail below in conjunction with specific embodiments. It should be noted that the embodiments of the present application and the features in the embodiments can be combined with each other without conflict.

[0042] In the following description, many specific details are set forth to facilitate a full understanding of the present invention. However, the present invention may also be implemented in other ways different from those described herein. Therefore, the protection scope of the present invention is not limited to the specific embodiments disclosed below.

[0043] Example 1-1

[0044] Combined with Figure 1-8 The present embodiment provides a TMBP reaction device, comprising a sealed tank body 1, wherein the tank body 1 is divided into a gas phase region 10 and a liquid phase region 20 from top to bottom, and is provided with a heating mechanism 2, a hollow rotating shaft 3 is provided at the center of the tank body 1, the top of the hollow rotating shaft 3 is connected to a motor 4, an air intake mechanism 5 is provided inside, an air intake hole 311 connected to the gas phase region 10 is provided above the side wall, a gas distribution mechanism 6 is provided below the side wall, the gas distribution mechanism 6 comprises a plurality of hollow and horizontally arranged spiral blades 65, the spiral blades 65 are sealed and connected to the hollow rotating shaft 3, an outer side wall is provided with an outlet pipe 66 perpendicular to its normal, and a one-way nozzle 67 is provided on the outlet pipe 66.

[0045] In the above technical solution, the heating mechanism 2 can adopt a conventional heating structure such as a heating coil or a heating jacket; the hollow shaft 3 has a closed inner cavity, and the oxygen in the gas phase region 10 can enter the closed inner cavity of the hollow shaft 3 from the air inlet 311, and then the oxygen in the hollow shaft 3 is transported to the gas distribution mechanism 6 through the air intake mechanism 5, and finally the oxygen is sprayed from the one-way nozzle 67 of the gas distribution mechanism 6 to the liquid phase region 20. The air intake mechanism 5 can adopt any suitable gas delivery structure in the prior art, including but not limited to a turbine and an axial flow blade. The spiral blade 65 refers to a blade twisted in a spiral shape, which can be in the shape of a spiral ribbon or a spiral bond as in the present embodiment. The spiral structure of the spiral blade 65 enables it to rotate under the impetus of the internal airflow. The spiral blade 65 will stir the reaction materials during the rotation process. The air outlet pipe 66 will enhance the stirring effect on the reaction materials during the up and down rotation of the spiral blade 65. The one-way nozzle 67 sprays oxygen in a rotating state, which will further enhance the stirring effect on the reaction materials on the one hand, and improve the uniformity of oxygen dispersion in the liquid reaction materials on the other hand. The one-way nozzle 67 refers to a nozzle with a one-way valve structure arranged inside it, which has the function of preventing liquid backflow. Most of the nozzles available on the market have this functional structure. The rotation of the spiral blade 65 driven by the internal airflow is called self-rotation, and the rotation of the spiral blade 65 along with the hollow shaft 3 is called revolution. The self-rotation and revolution of the spiral blade 65 can not only evenly distribute the oxygen in the liquid phase 20, but also efficiently stir the reaction materials, and have the dual functions of gas distribution and stirring, thereby improving the reaction efficiency, shortening the reaction time of the oxidative coupling reaction, and also avoiding the overoxidation of the coupling reaction, shortening the reaction time of the subsequent reduction reaction. In addition, the air intake mechanism 5 is arranged inside the hollow shaft 3, so that the overall structure of the device is compact and occupies a small area.

[0046] In a specific technical scheme, the tank body 1 includes a tank body 11, a tank cover 12 is provided on the top of the tank body 11, and a bracket 13, a discharge port 14 and a liquid temperature sensor 15 are provided on the bottom; the tank cover 12 is provided with a liquid feed port 16, a gas feed port 17, a gas pressure sensor 18 and the motor 4, and the liquid feed port 16, the gas feed port 17 and the discharge port 14 are all provided with a switch valve (not shown in the figure); the hollow rotating shaft 3 includes a rotating shaft body 31 with a top opening and a rotating shaft cover 32 fixedly arranged at the opening, the rotating shaft body 31 is provided with the air inlet 311 above the rotating shaft body 31, the rotating shaft cover 32 is sealed and rotatably connected to the tank cover 12, and is fixedly connected to the output end of the motor 4.

[0047] In the above technical solution, the shaft body 31 of the hollow shaft 3 may not contact the bottom of the tank body 1, or may be rotatably connected to the bottom of the tank body 1 as in the present embodiment.

[0048] In a specific technical scheme, the air intake mechanism 5 includes a fixed shaft 51 fixed in the tank body 1, and the fixed shaft 51 is coaxially sealed and rotatably connected with the hollow rotating shaft 3. The fixed shaft 51 is provided with a piston 52 capable of vertically guiding sliding. The piston 52 divides the hollow rotating shaft 3 into an upper air intake chamber 30 and a lower sealing chamber 40 connected to the gas distribution mechanism 6. The piston 52 is axially provided with a one-way air valve 53 for intake air into the lower sealing chamber 40, and the upper end surface is provided with a cam mechanism 54 capable of vertical reciprocating sliding. The cam mechanism 54 includes a cylindrical cam 541 coaxially fixed to the upper end surface of the piston 52 and a push rod 542 fixed to the inner wall of the hollow rotating shaft 3.

[0049] In the above technical scheme, the fixed shaft 51 can be fixed in the tank body 1 in any suitable manner under the premise of being compatible with the structure of the hollow rotating shaft 3. In this embodiment, the bottom of the hollow rotating shaft 3 is in a closed state and a tank cover 12 is provided on the top. Therefore, the lower end face seal of the fixed shaft 51 can be rotatably passed through the bottom of the hollow rotating shaft 3 and fixedly connected with the bottom of the tank body 1, and the upper end face can be rotatably connected with the lower end face seal of the tank cover 12 of the hollow rotating shaft 3; the cam mechanism 54 is a commonly used reciprocating displacement driving structure, and the cylindrical cam 541 refers to a closed curved groove (an elliptical groove is used in this embodiment) arranged axially on the outer wall of the cylinder, and the push rod 542 slides in the curved groove. When the push rod 542 rotates with the hollow rotating shaft 3, the cylindrical cam 541 is driven to reciprocate up and down through the curved groove; the piston 52 can slide along the vertical guide of the fixed shaft 51, which means that the inner ring wall of the piston 52 is circumferentially locked with the fixed shaft 51 and can only slide reciprocally along the axial direction of the fixed shaft 51. When the hollow shaft 3 rotates, the cam mechanism 54 drives the piston 52 connected thereto to move reciprocatingly up and down. When the piston 52 moves upward, the volume of the lower sealed chamber 40 increases, generating negative pressure. The oxygen in the upper air inlet chamber 30 enters the lower sealed chamber 40 through the one-way air valve 53. When the piston 52 moves downward, the volume of the lower sealed chamber 40 decreases, and the oxygen in the lower sealed chamber 40 is sprayed from the gas distribution mechanism 6 connected thereto to the liquid phase region 20. This intermittent gas injection structure can increase the spraying intensity of oxygen and further improve the stirring and dispersion effect of oxygen in the liquid phase region 20.

[0050] In a specific technical solution, the piston 52 includes an inner annular plug 521 capable of vertically guiding and sliding along the fixed shaft 51 and an outer annular plug 522 capable of vertically guiding and sliding along the hollow rotating shaft 3, the bottom of the inner annular plug 521 is provided with a first flange 5211 that can rotatably abut against the inner side wall of the outer annular plug 522, the top of the outer annular plug 522 is provided with a second flange 5221 that can rotatably abut against the outer side wall of the inner annular plug 521, a first sealing bearing 523 is provided between the first flange 5211 and the second flange 5221, a first sealing ring 5212 is provided on the first flange 5211, a second sealing ring 5222 is provided on the second flange 5221, an axial air hole 5213 is provided on the inner annular plug 521, and a one-way air valve 53 is provided in the axial air hole 5213.

[0051] In the above technical solution, the piston 52 is decomposed into an inner annular plug 521 and an outer annular plug 522 which are rotatably connected, which can eliminate the rotational friction between the piston 52 and the hollow shaft 3, reduce the wear of the piston 52, and increase the service life of the piston 52. The first sealing bearing 523, the first flange 5211, the second flange 5221, the first sealing ring 5212 and the second sealing ring 5222 are used in combination to improve the sealing effect of the inner annular plug 521 and the outer annular plug 522. The vertical guide sliding structure of the inner annular plug 521 and the fixed shaft 51 and the outer annular plug 522 and the hollow shaft 3 is not limited, and can achieve circumferential locking and axial sliding. In this embodiment, the inner ring wall of the inner annular plug 521 is vertically provided with a first slide groove, the side wall of the fixed shaft 51 is provided with a first guide rod matched with the first slide groove, the outer ring wall of the outer annular plug 522 is vertically provided with a second slide groove, and the inner side wall of the hollow shaft 3 is provided with a second guide rod matched with the second slide groove.

[0052] In a specific technical solution, the gas distribution mechanism 6 also includes a first connecting ring 61 fixed on the hollow rotating shaft 3, and a plurality of circular tubes 62 connected to the inner cavity of the hollow rotating shaft 3 are equidistantly arranged on the side wall circumference of the first connecting ring 61. One end of the spiral blade 65 is close to the inner wall of the tank body 1, and the other end is provided with an end cover 64. The end cover 64 is rotatably connected to the circular tube 62 through a second sealing bearing 63, and the spiral blade 65 is sealed and rotatably connected to the circular tube 62.

[0053] The working principle and working process of this embodiment are as follows: liquid material is added into the liquid phase zone 20 of the reaction device, oxygen is introduced into the gas phase zone 10 of the reaction device, the motor 4 is turned on, the motor 4 drives the hollow shaft 3 and the gas distribution mechanism 6 to rotate, the air intake mechanism 5 draws the oxygen in the gas phase zone 10 from the air intake hole 311 of the hollow shaft 3 into the spiral blade 65 of the gas distribution mechanism 6, and then sprays it into the liquid phase zone 20 from the one-way nozzle 67, the spiral blade 65 rotates with the flow of oxygen inside it, and at the same time revolves with the rotation of the hollow shaft 3, the spiral blade 65 efficiently stirs and mixes the liquid material in the liquid phase zone 20 through rotation and revolution, and at the same time makes the oxygen evenly dispersed in the liquid material, and the reaction material in the liquid phase zone 20 is heated by the heating mechanism 2 to carry out oxidative coupling reaction.

[0054] Example 1-2

[0055] Combined with Figure 1-8 This embodiment provides a TMBP reaction device, which adds a first stirring mechanism 7 on the basis of embodiment 1-1. The specific technical scheme is as follows:

[0056] The hollow rotating shaft 3 is provided with a first stirring mechanism 7, which includes a second connecting ring 71 connected to the hollow rotating shaft 3, and a plurality of inclined paddle blades 72 are equidistantly arranged on the circumference of the second connecting ring 71, and a plurality of filter holes 721 are evenly laid on the inclined paddle blades 72, and the free ends are close to the inner wall of the tank body 1, and the inclined paddle blades 72 are arranged directly above the spiral blades 65 and correspond one to one with the spiral blades 65, and a plurality of the gas distribution mechanism 6 and the first stirring mechanism 7 are axially staggered.

[0057] In this embodiment, the first stirring mechanism 7 can further improve the stirring effect of the reaction material in the liquid phase region 20, and at the same time can refine the oxygen bubbles in the liquid phase region 20, improve the efficiency of the oxidative coupling reaction, and shorten the reaction time. When the hollow shaft 3 rotates, oxygen is ejected from the one-way nozzle 67 to form bubbles, and the filter holes 721 on the oblique paddle blade 72 can refine the oxygen bubbles, improve the uniformity of oxygen distribution in the liquid phase region 20, and at the same time, due to the reduction of the bubble volume, the floating speed is reduced, so the residence time of oxygen in the liquid phase region 20 can be increased, the reaction efficiency of the oxidative coupling reaction is improved, overoxidation is avoided, and the reaction time is shortened. The oblique paddle blade 72 is arranged directly above the spiral blade 65, which can not only better refine the oxygen bubbles, but also can be sprayed and washed by the one-way nozzle 67 on the spiral blade 65 during the subsequent equipment cleaning, thereby improving the cleaning effect. The gas distribution mechanism 6 and the first stirring mechanism 7 are arranged in multiple axial staggered positions, which can further improve the stirring effect and reaction efficiency of the liquid phase region 20.

[0058] Examples 1-3

[0059] Combined with Figure 1-8 This embodiment provides a TMBP reaction device, which adds a second stirring mechanism 8 on the basis of Embodiment 1-2. The specific technical solution is as follows:

[0060] A second stirring mechanism 8 is provided at the interface between the gas phase region 10 and the liquid phase region 20, and the second stirring mechanism 8 includes a third connecting ring 81 connected to the hollow rotating shaft 3, and a plurality of shaft sleeves 82 are equidistantly provided on the circumference of the third connecting ring 81, and the shaft sleeves 82 can be rotatably connected to a horizontal rotating shaft 83. A plurality of flat paddle blades 84 are equidistantly provided on the circumference of one end of the horizontal rotating shaft 83, and the other end can be rotatably passed through the hollow rotating shaft 3 and then connected to a first bevel gear 85. A plurality of flat paddle blades 84 are equidistantly laid axially along the horizontal rotating shaft 83, and a second bevel gear 86 meshing with the first bevel gear 85 is provided on the fixed shaft 51.

[0061] In this embodiment, the second stirring mechanism 8 can improve the oxygen exchange rate at the gas-liquid interface, further improve the coupling reaction efficiency, and shorten the reaction time. When the hollow shaft 3 rotates, the horizontal shaft 83 revolves with it, and the first bevel gear 85 on the horizontal shaft 83 rotates around the second bevel gear 86 on the fixed shaft 51. Since the first bevel gear 85 and the second bevel gear 86 are in a meshing state, the horizontal shaft 83 will rotate. When the horizontal shaft 83 rotates, the flat paddle blade 84 rotates therewith, stirring the interface between the gas phase region 10 and the liquid phase region 20, thereby improving the oxygen exchange rate, further improving the reaction efficiency of the coupling reaction, avoiding overoxidation, and shortening the reaction time.

[0062] Example 2-1

[0063] This embodiment provides a TMBP synthesis method, using the TMBP reaction device in Example 1-1 to carry out the reaction, comprising the following steps:

[0064] Step S100. After dissolving 30 parts by mass of 2,6-dimethylphenol in 30 parts by mass of tetrahydrofuran, the mixture is added together with 3 parts by mass of potassium hydroxide into the liquid phase region 20 of the reaction device, oxygen is introduced into the gas phase region 10 of the reaction device, and the oxygen pressure in the gas phase region 10 is maintained at 1 MPa. The motor 4 is turned on, and the motor 4 drives the hollow shaft 3 and the gas distribution mechanism 6 to rotate. The air intake mechanism 5 draws the oxygen in the gas phase region 10 from the air intake hole 311 of the hollow shaft 3 to the spiral of the gas distribution mechanism 6. The oxygen in the spiral blade 65 flows out of the outlet pipe 66 of the spiral blade 65 into the liquid phase region 20. The spiral blade 65 rotates with the flow of oxygen inside it, and at the same time, it revolves with the rotation of the hollow shaft 3. The spiral blade 65 efficiently stirs and mixes the reaction materials in the liquid phase region 20 through rotation and revolution. The reaction materials in the liquid phase region 20 are heated by the heating mechanism 2, and the oxidative coupling reaction is carried out at 120° C. for 60 minutes. After the reaction is completed, the material is discharged to obtain a reaction completed liquid.

[0065] Step S200. Add 20 parts by mass of deionized water to 25 parts by mass of the reaction solution, stir and mix well, and then add the mixture together with 1 part by mass of sodium dithionite into a jacketed reactor, start stirring and heating, and perform a reduction reaction at 60° C. for 4 hours. After the reaction is completed, a reaction product is obtained;

[0066] Step S300: Filter the reaction product and wash it with water to remove the reducing agent, then cool it down to crystallize solid particles, and recrystallize the solid particles to obtain TMBP. The purity of TMBP is 99.62%, and the yield is 84.65%.

[0067] Example 2-2

[0068] This embodiment provides a TMBP synthesis method, using the TMBP reaction device in Example 1-2 to carry out the reaction, comprising the following steps:

[0069] Step S100. After dissolving 30 parts by mass of 2,6-dimethylphenol in 30 parts by mass of tetrahydrofuran, the mixture is added together with 3 parts by mass of potassium hydroxide into the liquid phase region 20 of the reaction device, oxygen is introduced into the gas phase region 10 of the reaction device, and the oxygen pressure in the gas phase region 10 is maintained at 1 MPa. The motor 4 is turned on, and the motor 4 drives the hollow shaft 3 and the gas distribution mechanism 6 to rotate. The air intake mechanism 5 draws the oxygen in the gas phase region 10 from the air intake hole 311 of the hollow shaft 3 into the spiral blade 65 of the gas distribution mechanism 6, and then the oxygen flows out from the air outlet pipe 66 of the spiral blade 65 into the liquid phase region 20. The spiral blade 65 rotates with the flow of oxygen inside it, and at the same time, it revolves with the rotation of the hollow shaft 3. The spiral blade 65 efficiently stirs and mixes the reaction materials in the liquid phase region 20 through rotation and revolution. At the same time, the first stirring mechanism 7 further stirs the reaction materials. The filter holes 721 on the oblique paddle blade 72 refine the oxygen bubbles in the liquid phase region 20 and further disperse them evenly. The reaction materials in the liquid phase region 20 are heated by the heating mechanism 2, and the oxidative coupling reaction is carried out at 120° C. for 40 minutes. After the reaction is completed, the material is discharged to obtain a reaction completion liquid;

[0070] Step S200. Add 20 parts by mass of deionized water to 25 parts by mass of the reaction solution, stir and mix well, and then add it together with 1 part by mass of sodium dithionite into a jacketed reactor, start stirring and heating, and carry out reduction reaction at 60° C. for 3.5 hours to complete the reaction and obtain a reaction product;

[0071] Step S300: Filter the reaction product and wash it with water to remove the reducing agent, then cool it down to crystallize solid particles, and recrystallize the solid particles to obtain TMBP. The purity of TMBP is 99.68%, and the yield is 85.13%.

[0072] Example 2-3

[0073] This embodiment provides a TMBP synthesis method, using the TMBP reaction device in Embodiment 1-3 to carry out the reaction, comprising the following steps:

[0074] Step S100. After dissolving 30 parts by mass of 2,6-dimethylphenol in 30 parts by mass of tetrahydrofuran, add the mixture together with 3 parts by mass of potassium hydroxide into the liquid phase region 20 of the reaction device, introduce oxygen into the gas phase region 10 of the reaction device, maintain the oxygen pressure of the gas phase region 10 at 1 MPa, turn on the motor 4, the motor 4 drives the hollow shaft 3 and the gas distribution mechanism 6 to rotate, the air intake mechanism 5 draws the oxygen in the gas phase region 10 from the air intake hole 311 of the hollow shaft 3 into the spiral blade 65 of the gas distribution mechanism 6, and then the oxygen flows out from the air outlet pipe 66 of the spiral blade 65 into the liquid phase region 20, and the spiral blade 65 is sucked along with the flow of oxygen inside the spiral blade 65. The hollow shaft 3 rotates and revolves with the rotation of the hollow shaft 3. The spiral blade 65 efficiently stirs and mixes the reaction materials in the liquid phase region 20 through rotation and revolution. At the same time, the first stirring mechanism 7 further stirs the reaction materials. The filter holes 721 on the oblique paddle blades 72 refine the oxygen bubbles in the liquid phase region 20 and further disperse them evenly. The second stirring mechanism 8 stirs at the gas-liquid interface to improve the oxygen exchange rate at the gas-liquid interface. The reaction materials in the liquid phase region 20 are heated by the heating mechanism 2, and the oxidative coupling reaction is carried out at 120°C for 30 minutes. After the reaction is completed, the material is discharged to obtain a reaction-completed liquid.

[0075] Step S200. Add 20 parts by mass of deionized water to 25 parts by mass of the reaction solution, stir and mix well, and then add it together with 1 part by mass of sodium dithionite into a jacketed reactor, start stirring and heating, and carry out reduction reaction at 60° C. for 3 hours to complete the reaction and obtain a reaction product;

[0076] Step S300: Filter the reaction product and wash it with water to remove the reducing agent, then cool it down to crystallize solid particles, and recrystallize the solid particles to obtain TMBP. The purity of TMBP is 99.78%, and the yield is 86.01%.

[0077] Embodiment 2-4

[0078] This embodiment provides a method for synthesizing TMBP. The difference from Embodiment 2-3 is that in step S100, an oxidative coupling reaction is carried out at 150° C. for 30 min; in step S200, a reduction reaction is carried out at 80° C. for 4 h; the purity of the obtained TMBP is 99.31%, and the yield is 85.42%.

[0079] Embodiment 2-5

[0080] This embodiment provides a method for synthesizing TMBP. The difference from Embodiment 2-3 is that in step S100, an oxidative coupling reaction is carried out at 200° C. for 30 min; in step S200, a reduction reaction is carried out at 80° C. for 5 h; the purity of the obtained TMBP is 98.49%, and the yield is 84.61%.

[0081] Embodiment 2-6

[0082] This embodiment provides a method for synthesizing TMBP. The difference from Embodiment 2-3 is that in step S100, an oxidative coupling reaction is carried out at 120° C. for 60 min; in step S200, a reduction reaction is carried out at 80° C. for 4 h; the purity of the obtained TMBP is 99.15%, and the yield is 85.07%.

[0083] Embodiment 2-7

[0084] This embodiment provides a method for synthesizing TMBP. The difference from Embodiment 2-3 is that in step S100, an oxidative coupling reaction is carried out at 120° C. for 120 min; in step S200, a reduction reaction is carried out at 80° C. for 6 h; the purity of the obtained TMBP is 98.41%, and the yield is 84.61%.

[0085] Embodiment 2-8

[0086] This embodiment provides a method for synthesizing TMBP. The difference from Embodiment 2-3 is that in step S100, the organic solvent is 100 parts by mass of tetrahydrofuran, the catalyst is 1.5 parts by mass of potassium hydroxide, and the oxidative coupling reaction is 60 minutes; in step S200, the deionized water is 45 parts by mass, the reducing agent is 2 parts by mass of sodium dithionite, and the reaction time is 4 hours; the purity of the obtained TMBP is 99.58%, and the yield is 85.32%.

[0087] Embodiment 2-9

[0088] This embodiment provides a method for synthesizing TMBP. The difference from Embodiment 2-3 is that in step S100, the organic solvent is 150 parts by mass of tetrahydrofuran, the catalyst is 2.5 parts by mass of potassium hydroxide, and the oxidative coupling reaction is 40 minutes; in step S200, the deionized water is 50 parts by mass, the reducing agent is 3 parts by mass of sodium dithionite, and the reaction time is 2 hours; the purity of the obtained TMBP is 99.61%, and the yield is 85.16%.

[0089] Embodiment 2-10

[0090] This embodiment provides a method for synthesizing TMBP. The difference from Embodiment 2-3 is that in step S100, the organic solvent is 60 parts by mass of ethyl acetate, the catalyst is 2 parts by mass of sodium carbonate, and the oxidative coupling reaction is 40 minutes; in step S200, the deionized water is 50 parts by mass, the reducing agent is 3 parts by mass of sodium borohydride, and the reaction time is 2.5 hours; the purity of the obtained TMBP is 99.68%, and the yield is 85.21%.

[0091] Example 2-11

[0092] This embodiment provides a TMBP synthesis method. The difference from Embodiment 2-3 is that in step S100, the organic solvent is 20 parts by mass of methanol, the catalyst is 1.5 parts by mass of sodium methoxide, and the oxidative coupling reaction is 50 minutes; in step S200, the deionized water is 30 parts by mass, the reducing agent is 5 parts by mass of sodium borohydride, and the reaction time is 1.5 hours; the purity of the obtained TMBP is 99.48%, and the yield is 85.11%.

[0093] Example 2-12

[0094] This embodiment provides a TMBP synthesis method. The difference from Embodiment 2-3 is that in step S100, the organic solvent is 40 parts by mass of toluene, the catalyst is 2.5 parts by mass of triethylamine, and the oxidative coupling reaction takes 35 minutes; in step S200, the deionized water is 30 parts by mass, the reducing agent is 2 parts by mass of sodium bisulfite, and the reaction time is 2 hours; the purity of the obtained TMBP is 99.58%, and the yield is 85.39%.

[0095] Example 2-13

[0096] This embodiment provides a method for synthesizing TMBP. The difference from Embodiment 2-3 is that in step S100, the organic solvent is 30 parts by mass of isopropanol, the catalyst is 3 parts by mass of diisopropylamine, and the oxidative coupling reaction takes 35 minutes; in step S200, the deionized water is 25 parts by mass, the reducing agent is 0.5 parts by mass of sodium dithionite, and the reaction time is 5 hours; the purity of the obtained TMBP is 99.45%, and the yield is 84.97%.

[0097] Example 2-14

[0098] This embodiment provides a method for synthesizing TMBP. The difference from Embodiment 2-3 is that in step S100, the organic solvent is 30 parts by mass of ethanol, the catalyst is 3 parts by mass of sodium ethoxide, and the oxidative coupling reaction takes 30 minutes; in step S200, the deionized water is 25 parts by mass, the reducing agent is 3 parts by mass of sodium dithionite, and the reaction time is 3 hours; the purity of the obtained TMBP is 99.55%, and the yield is 85.32%.

[0099] Example 2-15

[0100] This embodiment provides a method for synthesizing TMBP. The difference from Embodiment 2-3 is that in step S100, the organic solvent is 150 parts by mass of dichloromethane, the catalyst is 2.5 parts by mass of tetramethylethylenediamine, and the oxidative coupling reaction takes 40 minutes. In step S200, the deionized water is 50 parts by mass, the reducing agent is 2 parts by mass of sodium borohydride, and the reaction time is 4 hours. The purity of the obtained TMBP is 99.39%, and the yield is 85.13%.

[0101] Comparative Example

[0102] In this comparative example, a conventional high-pressure reactor is used as a reaction apparatus to synthesize TMBP, and the process parameters in Example 2-3 are used for the reaction. The difference from Example 2-3 is that in step S100, the oxidative coupling reaction is carried out at 200° C. for 150 min; in step S200, the reduction reaction is carried out at 80° C. for 8 h; the purity of the obtained TMBP is only 97.82%, and the yield is only 82.35%.

[0103] The above embodiments are preferred implementation modes of the present invention, but the implementation modes of the present invention are not limited to the above embodiments. Any other changes, modifications, substitutions, combinations, and simplifications made without departing from the spirit and principles of the present invention shall be equivalent replacement modes and shall be included in the protection scope of the present invention.

Claims

1. A TMBP reaction device, comprising a sealed tank (1), wherein the tank (1) is divided from top to bottom into a gas phase region (10) and a liquid phase region (20), and is provided with a heating mechanism (2), characterized in that: A hollow rotating shaft (3) is provided at the center of the tank body (1), the top of the hollow rotating shaft (3) is connected to a motor (4), an air intake mechanism (5) is provided inside, an air intake hole (311) communicating with the gas phase region (10) is provided above the side wall, a gas distribution mechanism (6) is provided below the side wall, the gas distribution mechanism (6) comprises a plurality of hollow and horizontally arranged spiral blades (65), the spiral blades (65) are sealed and communicated with the hollow rotating shaft (3), an outer side wall is provided with an air outlet pipe (66) perpendicular to the normal line thereof, and a one-way nozzle (67) is provided on the air outlet pipe (66); The air intake mechanism (5) comprises a fixed shaft (51) fixed in the tank body (1), the fixed shaft (51) being coaxially sealed and rotatably connected to the hollow rotating shaft (3), a piston (52) capable of vertically guiding and sliding being provided on the fixed shaft (51), the piston (52) dividing the hollow rotating shaft (3) into an upper air intake chamber (30) and a lower sealing chamber (40) communicating with the gas distribution mechanism (6), a one-way air valve (53) for intake of air into the lower sealing chamber (40) being axially provided on the piston (52), and a cam mechanism (54) capable of vertically reciprocating sliding being provided on the upper end surface, the cam mechanism (54) comprising a cylindrical cam (541) coaxially fixed to the upper end surface of the piston (52) and a push rod (542) fixed to the inner side wall of the hollow rotating shaft (3); The piston (52) comprises an inner annular plug (521) capable of vertically guiding and sliding along the fixed shaft (51) and an outer annular plug (522) capable of vertically guiding and sliding along the hollow rotating shaft (3); a first flange (5211) is provided at the bottom of the inner annular plug (521) and can rotatably abut against the inner side wall of the outer annular plug (522); a second flange (5221) is provided at the top of the outer annular plug (522) and can rotatably abut against the outer side wall of the inner annular plug (521); a first sealing bearing (523) is provided between the first flange (5211) and the second flange (5221); a first sealing ring (5212) is provided on the first flange (5211); a second sealing ring (5222) is provided on the second flange (5221); an axial air hole (5213) is provided on the inner annular plug (521); a one-way air valve (53) is provided in the axial air hole (5213).

2. A TMBP reaction device according to claim 1, characterized in that: The tank body (1) comprises a tank body (11), the top of the tank body (11) is provided with a tank cover (12), the bottom of the tank body (11) is provided with a bracket (13), a discharge port (14) and a liquid temperature sensor (15), the tank cover (12) is provided with a liquid feed port (16), a gas feed port (17), a gas pressure sensor (18) and the motor (4), and the liquid feed port (16), the gas feed port (17) and the discharge port (14) are all provided with switch valves; the hollow shaft (3) comprises a shaft body (31) with an opening at the top and a shaft cover (32) fixedly arranged at the opening, the shaft body (31) is provided with the air inlet hole (311), the shaft cover (32) is rotatably connected to the tank cover (12) in a sealed manner, and is fixedly connected to the output end of the motor (4).

3. A TMBP reaction device according to claim 2, characterized in that: The gas distribution mechanism (6) further comprises a first connecting ring (61) fixed on the hollow rotating shaft (3); a plurality of circular tubes (62) connected to the inner cavity of the hollow rotating shaft (3) are equidistantly arranged on the circumference of the side wall of the first connecting ring (61); one end of the spiral blade (65) is close to the inner wall of the tank body (1); the other end is provided with an end cover (64); the end cover (64) is rotatably connected to the circular tube (62) via a second sealing bearing (63); and the spiral blade (65) is rotatably connected to the circular tube (62) in a sealed manner.

4. A TMBP reaction device according to claim 3, characterized in that: The hollow rotating shaft (3) is provided with a first stirring mechanism (7), the first stirring mechanism (7) comprising a second connecting ring (71) connected to the hollow rotating shaft (3), a plurality of inclined paddle blades (72) being equidistantly arranged on the circumference of the second connecting ring (71), a plurality of filter holes (721) being evenly arranged on the inclined paddle blades (72), the free ends of which are close to the inner side walls of the tank body (1), the inclined paddle blades (72) being arranged directly above the spiral blades (65) and corresponding one to one with the spiral blades (65), and a plurality of the gas distribution mechanisms (6) and the first stirring mechanisms (7) being staggered in the axial direction.

5. A TMBP reaction device according to claim 4, characterized in that: A second stirring mechanism (8) is provided at the interface between the gas phase region (10) and the liquid phase region (20), the second stirring mechanism (8) comprising a third connecting ring (81) connected to the hollow rotating shaft (3), a plurality of shaft sleeves (82) being equidistantly provided on the circumference of the third connecting ring (81), the shaft sleeves (82) being rotatably connected to a horizontal rotating shaft (83), a plurality of flat paddle blades (84) being equidistantly provided on one end of the horizontal rotating shaft (83), the other end of the horizontal rotating shaft (83) being rotatably connected to a first bevel gear (85) after passing through the hollow rotating shaft (3), a plurality of groups of flat paddle blades (84) being equidistantly provided along the axial direction of the horizontal rotating shaft (83), and a second bevel gear (86) meshing with the first bevel gear (85) being provided on the fixed shaft (51).

6. A method for synthesizing TMBP, characterized in that: The reaction is carried out using the TMBP reaction device according to any one of claims 1 to 5, comprising the following steps: Step S100. After dissolving 2,6-dimethylphenol in an organic solvent, the 2,6-dimethylphenol is added together with a catalyst into the liquid phase region (20) of the reaction device, oxygen is introduced into the gas phase region (10) of the reaction device, and the oxygen pressure in the gas phase region (10) is maintained at 0.1-2 MPa. The motor (4) is turned on, and the motor (4) drives the hollow shaft (3) and the gas distribution mechanism (6) to rotate. The air intake mechanism (5) draws the oxygen in the gas phase region (10) from the air intake hole (311) of the hollow shaft (3) into the spiral blade (65) of the gas distribution mechanism (6). , and then flows out from the outlet pipe (66) of the spiral blade (65) into the liquid phase region (20). The spiral blade (65) rotates with the flow of oxygen inside it, and simultaneously revolves with the rotation of the hollow shaft (3). The spiral blade (65) efficiently stirs and mixes the reaction materials in the liquid phase region (20) through rotation and revolution. The reaction materials in the liquid phase region (20) are heated by the heating mechanism (2), and an oxidative coupling reaction is carried out at 120 to 200° C. for 30 to 120 minutes. After the reaction is completed, the material is discharged to obtain a reaction-completed liquid; Step S200. Add deionized water to the reaction solution, stir and mix well, then add the mixture together with the reducing agent into the jacketed reactor, start stirring and heat, and perform reduction reaction at 20-80° C. for 1-6 hours. After the reaction is completed, obtain a reaction product; Step S300: Filter the reaction product and wash with water to remove the reducing agent, then cool it down to crystallize solid particles, and recrystallize the solid particles to obtain TMBP.

7. A TMBP synthesis method according to claim 6, characterized in that: In step S100, the organic solvent is at least one of methanol, ethanol, tetrahydrofuran, dichloromethane, ethyl acetate, dioxane, isopropanol, acetonitrile, cyclohexanol, butanol, isobutanol, pentanol, octanol, toluene, and xylene; the catalyst is at least one of potassium hydroxide, sodium hydroxide, sodium carbonate, potassium carbonate, lithium hydroxide, cesium carbonate, potassium bicarbonate, sodium bicarbonate, sodium methoxide, sodium ethoxide, sodium tert-butoxide, potassium tert-butoxide, diisopropylamine, triethylamine, and tetramethylethylenediamine; In step S200, the reducing agent is at least one of sodium dithionite, sodium borohydride, hydrogen and sodium bisulfite.

8. A TMBP synthesis method according to claim 6, characterized in that: In step S100, the mass ratio of 2,6-dimethylphenol to the organic solvent is 1:(0.5-5); the mass ratio of 2,6-dimethylphenol to the catalyst is 1:(0.005-0.1); In step S200, the mass ratio of the reaction completion liquid, deionized water and reducing agent is 25: (20-50): (0.5-10).

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