Method and device for continuously synthesizing antioxidant 168

Abstract

The invention discloses a method and a device for continuously synthesizing an antioxidant 168, and relates to the technical field of antioxidant 168 synthesis, and the method comprises the following steps: a, injecting a raw material mixed solution into a material box 1, injecting a phosphorus trichloride solution into a material box 2, and injecting a basic catalyst into a catalyst box 3; b, heating and mixing in a heating mixing barrel 4; c, carrying out a reaction in a reaction tube 5; d, the hydrogen chloride gas upwards enters a tail gas tank 18 through an exhaust pipe 17; e, the solution passing through the gas-liquid separation baffle 10 enters a distillation tank 6, and then the organic solution and the basic catalyst in the solution are distilled to enter a neutralization tank 7 through heating distillation; and f, heat of the neutralization tank 7 is transmitted to a second heat conducting plate 14 through a heat exchanger 13. According to the invention, materials enter the long reaction tube for reaction, and the generated hydrogen chloride can be quickly discharged through the exhaust pipe, so that the reaction speed of the balance reaction and the delay antioxidant 168 is reduced.

Description

Technical Field

[0001] The present invention relates to the technical field of synthesizing antioxidant 168, and specifically to a method and apparatus for continuously synthesizing antioxidant 168. Background Art

[0002] Antioxidant 168 is generally used to protect polymers exposed to oxidative environments. Antioxidant 168 is generally prepared by reacting 2,4-di-tert-butylphenol and phosphorus trichloride with an alkaline catalyst. In some preparation methods, the reactants are reacted in a stirring drum. The hydrogen chloride produced during the reaction leads to a reversible equilibrium reaction. Generally, it is necessary to discharge the hydrogen chloride to cause the reaction to proceed to the right in order to increase the yield of antioxidant 168.

[0003] The defects of the existing method for synthesizing antioxidant 168 are: 1. Prior art JP2012170948A discloses a stirring tank equipped with multiple agitators. This technology discloses a stirring tank equipped with multiple agitators inside. It can fully stir within a wide range inside with a simple structure. However, when synthesizing antioxidant 168, hydrogen chloride generated inside this reaction device is discharged slowly. Hydrogen chloride and products also react to form a reversible equilibrium reaction, which affects the reaction rate of antioxidant 168. Therefore, a method and device for continuously synthesizing antioxidant 168 that can quickly discharge hydrogen chloride are needed to solve this problem.

[0004] 2. Prior art JP2010058027A discloses a stirring device and a stirring tank. This technology can form a satisfactory circulation flow to effectively stir a high-viscosity fluid in the stirring tank. However, when the device uses a pipeline to transport the reaction liquid during the reaction, the reaction liquid is easily transported together with the gas, resulting in low separation efficiency of hydrogen chloride gas and solution. Therefore, a method and device for continuously synthesizing antioxidant 168 that can effectively separate hydrogen chloride from the solution is needed to solve this problem.

[0005] 3. The prior art KR101373626B1 discloses a multi-layer stirring tank. When heating the solution, this technology cannot recover the heat of the solution when the solution is discharged, resulting in waste of heat of the solution and further waste of electrical energy. Therefore, a method and device for continuously synthesizing antioxidant 168 that can recover the heat of the reaction solution is needed to solve this problem.

[0006] 4. Prior art CN115819451A discloses a method for continuously synthesizing antioxidant 168. This technology cannot absorb hydrogen chloride escaping from the air during the reaction. If hydrogen chloride escapes into the air, it is easy to pollute the environment. Therefore, a method and device for continuously synthesizing antioxidant 168 that can absorb hydrogen chloride escaping from the air are needed to solve this problem. Summary of the Invention

[0007] One purpose of the present application is to provide a method and apparatus for continuously synthesizing antioxidant 168, which can solve the technical problems raised in the prior art.

[0008] To achieve the above object, the present invention provides the following technical solution: a method for continuously synthesizing antioxidant 168, comprising the following steps: a: Inject the raw material mixture of 2,4-di-tert-butylphenol and organic solution into material box one, inject the phosphorus trichloride solution into material box two, and inject the alkaline catalyst into the catalyst box; b: The raw material mixed liquid in the material tank 1 and the phosphorus trichloride solution in the material tank 2 are respectively transferred into the heating mixing drum through a pump and a pipeline for heating and mixing; c. The liquid in the heated mixing drum is transferred into the reaction tube through a pump and a pipe for reaction. At the same time, the alkaline catalyst in the catalyst box is transferred into the inlet of the reaction tube through a pipe and a pump. Then, the motor drives the rotating rod to rotate slowly. The raised stirring rod on the rotating rod stirs the mixed liquid to ensure that the 2,4-di-tert-butylphenol and phosphorus trichloride solution are fully in contact and react. d: The hydrogen chloride gas generated by the reaction escapes upward through the gas-liquid separation valve, exhaust pipe and connected pipes as it is stirred by the rotating rod and enters the tail gas tank. The gas-liquid separation baffle allows the reacted liquid to be transmitted backward through the air holes, and the hydrogen chloride gas is blocked on the side of the gas-liquid separation baffle facing the motor; e: The solution that passes through the gas-liquid separation baffle enters the distillation tank through the output end of the reaction tube and the pipe between the reaction tube and the distillation tank. Then, the organic solution and alkaline catalyst in the solution are distilled into the neutralization tank through heating distillation. Then, sodium hydroxide solution is added to the neutralization tank to neutralize the hydrogen chloride in the solution produced by distillation. At the same time, the fan works to absorb the hydrogen chloride escaping into the air during the reaction process and transfers it to the neutralization tank for neutralization and absorption; f: Before the solution in the neutralization tank is discharged, the hydraulic cylinder drives the heat transfer plate 1 to move backward toward the neutralization tank and contact the neutralization tank, so that the heat of the neutralization tank is transferred to the heat transfer plate 1, and then to the heat exchanger, and then the heat is transferred to the heat transfer plate 2 through the heat exchanger, thereby transferring the heat to the reaction liquid in the reaction tube, realizing heat recovery and reuse.

[0009] Preferably, the organic solution is at least one of ethyl acetate, toluene, xylene, diethyl ether and acetonitrile, preferably ethyl acetate and diethyl ether, and the mass ratio of ethyl acetate to diethyl ether is 1:(0.2-0.3).

[0010] Preferably, the content of 2,4-di-tert-butylphenol in the raw material mixture is 20-30wt%.

[0011] Preferably, the alkaline catalyst is selected from at least one of triethylamine, tripropylamine, diazabicyclo and hexamethylenetetramine, preferably tripropylamine and diazabicyclo, and preferably the mass ratio thereof is 1:(5-6).

[0012] Preferably, the molar ratio of 2,4-di-tert-butylphenol, phosphorus trichloride and alkaline catalyst in the material box 1, the material box 2 and the catalyst box is 3:1:0.2-0.3.

[0013] Preferably, in step b, the temperature of heating and mixing is 40-50°C.

[0014] Preferably, in step c, the temperature of the solution inside the reaction tube (5) increases from the inlet end to the outlet end, and the temperature range is 40 to 150°C.

[0015] Preferably, the solution inside the reaction tube (5) is evenly divided into three sections from the inlet end to the outlet end, and the temperature of the first section of the reaction tube is controlled to be 40-50°C, the temperature of the second section of the reaction tube is controlled to be 100-120°C, and the temperature of the third section of the reaction tube is controlled to be 140-150°C.

[0016] Preferably, in step c, when the contact reaction is sufficient, the residence time is 260-300s.

[0017] The inventors have discovered that the synergistic effect of hexamethylenetetramine and diazabicyclo in the present invention not only avoids the instability of the triethylamine system, but also uses a specific solvent and alkaline catalyst combination to better increase the yield of antioxidant 168. This is presumably because in the early stage of the reaction, the reaction temperature set by the present invention is relatively low, and a large amount of raw materials are reacted in the reaction. At this time, hexamethylenetetramine and diazabicyclo can better play a catalytic role in the specific solvent system. At the same time, the present invention continuously discharges HCl during the reaction, which can promote the forward progress of the reaction and reduce the occurrence of side reactions. In the later stage of the reaction, the temperature is relatively high, and there are very few raw materials reacted in the reaction. The fact that diazabicyclo is a heat-sensitive amine catalyst can better increase the synthesis of the target product.

[0018] The conditions for heating and distillation in step e are not particularly limited, as long as the organic solution and the alkaline catalyst can be distilled off. This invention will not elaborate on this in detail.

[0019] A second aspect of the present invention provides a device for continuously synthesizing an antioxidant 168, the device comprising: A material box 1 for providing a raw material mixture of 2,4-di-tert-butylphenol and an organic solution, a material box 2 for providing a phosphorus trichloride solution, and a catalyst box 3 for providing an alkaline catalyst; A heating mixing cylinder 4 connected to the material box 1 and the material box 2 2 through a pump and a pipeline; The liquid is transferred into the reaction tube 5 through the pump and the pipeline connected to the heating mixing cylinder 4; The catalyst box 3 is connected to the inlet of the reaction tube 5 through a pipeline and a pump; A rotating rod 9 with a parallel end penetrating the front inner wall of the reaction tube 5; The device also includes a motor 8, a fan 19, an air intake pipe 20, a neutralization tank 7, a hydraulic cylinder 15, a heat conducting plate 12, a heat conducting plate 2 14, and a heat exchanger 13; The output end of the motor 8 is connected to one end of a rotating rod 9, and one end of the rotating rod 9 passes through the front inner wall of the reaction tube 5; The input end of the fan 19 is connected to the bottom output end of the air intake pipe 20 through a pipe. The top of the air intake pipe 20 is provided with a plurality of holes. The output end of the fan (19) is connected to the front input end of the neutralization tank 7 through a pipe. A plurality of gas-liquid separation baffles 10 are arranged at equal intervals on the outer side of the rotating rod 9, and air holes 11 are arranged through the gas-liquid separation baffles 10 at positions close to the rotating rod 9; One end of the piston rod at the output end of the hydraulic cylinder 15 is connected to the front surface of the heat conducting plate 12, and the material of the heat conducting plate 12 and the heat conducting plate 2 14 is one of iron, aluminum and copper; The heat exchanger 13 is in mobile contact with the heat exchanger neutralization tank 7 and the hot plate 12 respectively; The surface of the rotating rod 9 is provided with protrusions.

[0020] Preferably, a heating rod and a temperature sensor are provided on the inner wall of the reaction tube 5 .

[0021] Preferably, the reaction tube 5 is evenly divided into three sections along the material flow direction, and a heating rod and a temperature sensor are respectively provided on the inner wall of the first section reaction tube, the second section reaction tube and the third section reaction tube.

[0022] Compared with the prior art, the present invention has the following beneficial effects: 1. The present invention arranges for 2,4-di-tert-butylphenol, phosphorus trichloride and an alkaline catalyst to be mixed and reacted in an elongated reaction tube, and the generated hydrogen chloride can be quickly discharged through an exhaust pipe, thereby reducing the equilibrium reaction and delaying the reaction rate of the antioxidant 168. The reaction apparatus is simple and the production cost is low. The method for continuously synthesizing the antioxidant 168 is arranged for 2,4-di-tert-butylphenol, phosphorus trichloride and an alkaline catalyst to be mixed and reacted in an elongated reaction tube, and the reaction apparatus is simple and the production cost is low.

[0023] 2. In the present invention, the motor drives the rotating rod to rotate, and then the stirring rod on the rotating rod stirs the material, so that the material is fully mixed and the reaction speed is fast. At the same time, the gas-liquid separation baffle can separate the gaseous hydrogen chloride and the liquid in the reaction tube, so that the hydrogen chloride is squeezed by the liquid upward into the exhaust pipe and is transmitted into the tail gas tank, so that the separation process of hydrogen chloride and the liquid is simple and efficient, so that the method for continuously synthesizing antioxidant 168 is simple and efficient. The motor drives the rotating rod to rotate, and then the stirring rod on the rotating rod stirs the material, so that the material is fully mixed and the reaction speed is fast. At the same time, the gas-liquid separation baffle can separate the gaseous hydrogen chloride and the liquid in the reaction tube, so that the hydrogen chloride is squeezed by the liquid upward into the exhaust pipe and is transmitted into the tail gas tank, so that the separation process of hydrogen chloride and the liquid is simple and efficient.

[0024] 3. The present invention can effectively transfer the heat of the high-temperature product in the neutralization tank to the front low-temperature part of the reaction tube by arranging the heat conducting plate 1, the heat exchanger and the heat conducting plate 2, thereby realizing heat recovery and saving energy. The method for continuously synthesizing antioxidant 168 can effectively transfer the heat of the high-temperature product in the neutralization tank to the front low-temperature part of the reaction tube by arranging the heat conducting plate 1, the heat exchanger and the heat conducting plate 2, thereby realizing heat recovery and saving energy.

[0025] 4. The present invention can absorb the hydrogen chloride leaked during the reaction into the intake pipe by providing a blower and an intake pipe, and then transmit it into the neutralization tank to be neutralized, thereby reducing the pollution of hydrogen chloride to the environment. The method for continuously synthesizing antioxidant 168 can absorb the hydrogen chloride leaked during the reaction into the intake pipe by providing a blower and an intake pipe, and then transmit it into the neutralization tank to be neutralized, thereby reducing the pollution of hydrogen chloride to the environment. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 A flow chart of the method of using the present invention; Figure 2 Schematic diagram of the device structure of the present invention; Figure 3 Schematic diagram of the rotating rod structure of the present invention; Figure 4 It is a structural schematic diagram of location A of the present invention.

[0028] In the figure: 1. Material box 1; 2. Material box 2; 3. Catalyst box; 4. Heating mixing cylinder; 5. Reaction tube; 6. Distillation tank; 7. Neutralization tank; 8. Motor; 9. Rotating rod; 10. Gas-liquid separation baffle; 11. Air hole; 12. Heat transfer plate 1; 13. Heat exchanger; 14. Heat transfer plate 2; 15. Hydraulic cylinder; 16. Gas-liquid separation valve; 17. Exhaust pipe; 18. Tail gas tank; 19. Fan; 20. Intake pipe. DETAILED DESCRIPTION

[0029] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0030] In the description of the present invention, it should be noted that the terms "upper," "lower," "inner," "outer," "front end," "rear end," "both ends," "one end," "the other end," and the like, indicating orientations or positional relationships, are based on the orientations or positional relationships shown in the accompanying drawings and are intended solely to facilitate and simplify the description of the present invention. They are not intended to indicate or imply that the devices or components referred to must have, be constructed, or operate in a specific orientation, and therefore should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0031] In the description of the present invention, it should be noted that, unless otherwise expressly specified or limited, the terms "installed," "provided with," "connected," etc., should be understood in a broad sense. For example, "connected" may refer to a fixed connection, a detachable connection, or an integral connection; it may refer to a mechanical connection or an electrical connection; it may refer to a direct connection or an indirect connection through an intermediate medium; it may refer to internal communication between two components. Those skilled in the art will be able to understand the specific meanings of the above terms in the present invention based on the specific circumstances.

[0032] See also Figure 1 、 Figure 2 、 Figure 3 and Figure 4 The present invention provides an embodiment of a method for continuously synthesizing antioxidant 168, comprising the following steps: a: Inject the organic solution of 2,4-di-tert-butylphenol into material box 1, inject the phosphorus trichloride solution into material box 2, and inject the alkaline catalyst into catalyst box 3; b: The 2,4-di-tert-butylphenol organic solution in the material tank 1 and the phosphorus trichloride solution in the material tank 2 are respectively transferred into the heating mixing cylinder 4 through a pump and a pipeline for heating and mixing; c. The liquid in the heated mixing drum 4 is transferred to the reaction tube 5 through a pump and a pipeline for reaction. At the same time, the alkaline catalyst in the catalyst box 3 is transferred to the inlet of the reaction tube 5 through a pipeline and a pump. Then, the motor 8 drives the rotating rod 9 to rotate. The raised stirring rod on the rotating rod 9 stirs the mixed liquid to ensure that the 2,4-di-tert-butylphenol and the phosphorus trichloride solution are fully contacted and reacted; d: The hydrogen chloride gas generated by the reaction escapes upward through the gas-liquid separation valve 16, the exhaust pipe 17 and the connected pipe into the tail gas tank 18 as it is stirred by the rotating rod 9. The gas-liquid separation baffle 10 allows the reacted liquid to be transmitted backward through the air holes 11, and the hydrogen chloride gas is blocked on the side of the gas-liquid separation baffle 10 facing the motor 8; e: The solution passing through the gas-liquid separation baffle 10 enters the distillation tank 6 through the output end of the reaction tube 5 and the pipeline between the reaction tube 5 and the distillation tank 6, and then the organic solution and the alkaline catalyst in the solution are distilled into the neutralization tank 7 by heating distillation. The output end of the top of the neutralization tank 7 is equipped with an outlet pipe. Subsequently, sodium hydroxide solution is added to the neutralization tank 7 to neutralize the hydrogen chloride in the solution produced by the distillation. At the same time, the fan 19 is operated to absorb the hydrogen chloride escaping into the air during the reaction and transfer it to the neutralization tank 7 for neutralization and absorption; f: Before the solution in the neutralization tank 7 is discharged, the hydraulic cylinder 15 drives the heat conducting plate 12 to move backward toward the neutralization tank 7 and contact the neutralization tank 7, so that the heat of the neutralization tank 7 is transferred to the heat conducting plate 12, and then to the heat exchanger 13, and then the heat is transferred to the heat conducting plate 2 14 through the heat exchanger 13, thereby transferring the heat to the reaction liquid in the reaction tube 5, realizing heat recovery and reuse.

[0033] The organic solution is ethyl acetate and diethyl ether, and the mass ratio of ethyl acetate to diethyl ether is 1: (0.2-0.3).

[0034] The content of 2,4-di-tert-butylphenol in the raw material mixture is 20-30wt%.

[0035] The basic catalyst is tripropylamine and diazabicyclo, the mass ratio of which is 1: (5-6) The molar ratio of 2,4-di-tert-butylphenol, phosphorus trichloride and alkaline catalyst in material box 1, material box 2 and catalyst box 3 is 3:1:0.2-0.3.

[0036] In step b, the temperature of heating and mixing is 40-50°C.

[0037] The solution inside the reaction tube 5 is evenly divided into three sections from the inlet end to the outlet end. The temperature of the first section of the reaction tube is controlled at 40-50°C, the temperature of the second section of the reaction tube is controlled at 100-120°C, and the temperature of the third section of the reaction tube is controlled at 140-150°C.

[0038] The residence time is 260-300s.

[0039] Example 1 1. As Figure 2-4As shown, 2,4-di-tert-butylphenol and an organic solution (ethyl acetate and diethyl ether in a mass ratio of 1:0.25) are injected into material box 1 as a raw material mixture, phosphorus trichloride solution is injected into material box 2, and an alkaline catalyst (tripropylamine and diazabicyclic in a mass ratio of 1:5) is injected into catalyst box 3. The liquid volumes of material box 1, material box 2, and catalyst box 3 are the same, and the molar ratio of 2,4-di-tert-butylphenol, phosphorus trichloride and alkaline catalyst is 3:1:0.2. 2. The raw material mixture in the material tank 1 and the phosphorus trichloride solution in the material tank 2 are respectively transferred into the heating mixing drum 4 through a pump and a pipeline for heating and mixing (the heating temperature is 45°C); 3. The liquid in the heated mixing drum 4 is transferred to the reaction tube 5 for reaction through a pump and a pipeline. At the same time, the alkaline catalyst 3 in the catalyst box 3 is transferred to the inlet of the reaction tube 5 through a pipeline and a pump. The solution inside the reaction tube 5 is evenly divided into three sections from the inlet end to the outlet end. The temperature of the first section of the reaction tube is controlled to 45° C., the temperature of the second section of the reaction tube is 115° C., and the temperature of the third section of the reaction tube is 145° C. by a heating rod. Then, the motor 8 drives the rotating rod 9 to rotate. The raised stirring rod on the rotating rod 9 stirs the mixed liquid in the reaction tube 5 to ensure sufficient contact and reaction between 2,4-di-tert-butylphenol and phosphorus trichloride. The residence time of the materials in the reaction tube 5 is 300 seconds. Fourth, the hydrogen chloride gas generated by the reaction escapes upward through the gas-liquid separation valve 16, the exhaust pipe 17 and the connected pipe into the tail gas tank 18 as it is stirred by the rotating rod 9. The gas-liquid separation baffle 10 allows the reacted liquid to be transmitted backward through the air holes 11, and the hydrogen chloride gas is blocked on the side of the gas-liquid separation baffle 10 facing the motor 8; 5. The solution passing through the gas-liquid separation baffle 10 enters the distillation tank 6 through the output end of the reaction tube 5 and the pipeline between the reaction tube 5 and the distillation tank 6. Then, the organic solution and the alkaline catalyst in the solution are distilled into the neutralization tank 7 by heating distillation. Subsequently, sodium hydroxide solution is added to the neutralization tank 7 to neutralize the hydrogen chloride in the solution produced by the distillation to obtain a phosphorus trichloride solution. At the same time, the fan 19 is operated to absorb the hydrogen chloride escaping into the air during the reaction process and transfer it to the neutralization tank 7 for neutralization and absorption; 6. Before the solution in the neutralization tank 7 is discharged, the hydraulic cylinder 15 drives the heat conducting plate 12 to move backward toward the neutralization tank 7 and contact the neutralization tank 7, so that the heat of the neutralization tank 7 is transferred to the heat conducting plate 12, and then to the heat exchanger 13, and then the heat is transferred to the heat conducting plate 2 14 through the heat exchanger 13, thereby transferring the heat to the reaction liquid in the reaction tube 5, realizing heat recovery and reuse.

[0040] Example 2 1. As Figure 2-4As shown, 2,4-di-tert-butylphenol and an organic solution (ethyl acetate and diethyl ether in a mass ratio of 1:0.2) are injected into material box 1 as a raw material mixture, phosphorus trichloride solution is injected into material box 2, and an alkaline catalyst (tripropylamine and diazabicyclic in a mass ratio of 1:6) is injected into catalyst box 3. The liquid volumes of material box 1, material box 2, and catalyst box 3 are the same, and the molar ratio of 2,4-di-tert-butylphenol, phosphorus trichloride and alkaline catalyst is 3:1:0.25. 2. The raw material mixture in the material tank 1 and the phosphorus trichloride solution in the material tank 2 are respectively transferred into the heating mixing drum 4 through a pump and a pipeline for heating and mixing (the heating temperature is 50°C); 3. The liquid in the heated mixing drum 4 is transferred to the reaction tube 5 for reaction via a pump and a pipeline. At the same time, the alkaline catalyst in the catalyst box 3 is transferred to the inlet of the reaction tube 5 via a pipeline and a pump. The solution inside the reaction tube 5 is evenly divided into three sections from the inlet end to the outlet end. The temperature of the first section of the reaction tube is controlled by a heating rod to be 50° C., the temperature of the second section of the reaction tube is 100° C., and the temperature of the third section of the reaction tube is 150° C. Then, the motor 8 drives the rotating rod 9 to rotate. The raised stirring rod on the rotating rod 9 stirs the mixed liquid in the reaction tube 5 to ensure sufficient contact and reaction between 2,4-di-tert-butylphenol and phosphorus trichloride. The residence time of the materials in the reaction tube 5 is 280 seconds. Fourth, the hydrogen chloride gas generated by the reaction escapes upward through the gas-liquid separation valve 16, the exhaust pipe 17 and the connected pipe into the tail gas tank 18 as it is stirred by the rotating rod 9. The gas-liquid separation baffle 10 allows the reacted liquid to be transmitted backward through the air holes 11, and the hydrogen chloride gas is blocked on the side of the gas-liquid separation baffle 10 facing the motor 8; 5. The solution passing through the gas-liquid separation baffle 10 enters the distillation tank 6 through the output end of the reaction tube 5 and the pipeline between the reaction tube 5 and the distillation tank 6. Then, the organic solution and the alkaline catalyst in the solution are distilled into the neutralization tank 7 by heating distillation. Subsequently, sodium hydroxide solution is added to the neutralization tank 7 to neutralize the hydrogen chloride in the solution produced by the distillation to obtain a phosphorus trichloride solution. At the same time, the fan 19 is operated to absorb the hydrogen chloride escaping into the air during the reaction process and transfer it to the neutralization tank 7 for neutralization and absorption; 6. Before the solution in the neutralization tank 7 is discharged, the hydraulic cylinder 15 drives the heat conducting plate 12 to move backward toward the neutralization tank 7 and contact the neutralization tank 7, so that the heat of the neutralization tank 7 is transferred to the heat conducting plate 12, and then to the heat exchanger 13, and then the heat is transferred to the heat conducting plate 2 14 through the heat exchanger 13, thereby transferring the heat to the reaction liquid in the reaction tube 5, realizing heat recovery and reuse.

[0041] Example 3 1. As Figure 2-4As shown, 2,4-di-tert-butylphenol and an organic solution (ethyl acetate and diethyl ether in a mass ratio of 1:0.3) are injected into material box 1 as a raw material mixture, phosphorus trichloride solution is injected into material box 2, and an alkaline catalyst (tripropylamine and diazabicyclic in a mass ratio of 1:6) is injected into catalyst box 3. The liquid volumes of material box 1, material box 2, and catalyst box 3 are the same, and the molar ratio of 2,4-di-tert-butylphenol, phosphorus trichloride and alkaline catalyst is 3:1:0.30. 2. Transfer the 2,4-di-tert-butylphenol organic solution in the raw material mixture in material box 1 and the phosphorus trichloride solution in material box 2 into the heating mixing drum 4 through a pump and a pipeline for heating and mixing (the heating temperature is 40°C); 3. The liquid in the heated mixing drum 4 is transferred to the reaction tube 5 for reaction via a pump and a pipeline. At the same time, the alkaline catalyst in the catalyst box 3 is transferred to the inlet of the reaction tube 5 via a pipeline and a pump. The solution in the reaction tube 5 is evenly divided into three sections from the inlet end to the outlet end. The temperature of the first section of the reaction tube is controlled by a heating rod to be 40° C., the temperature of the second section of the reaction tube is 120° C., and the temperature of the third section of the reaction tube is 150° C. Then, the motor 8 drives the rotating rod 9 to rotate. The raised stirring rod on the rotating rod 9 stirs the mixed liquid in the reaction tube 5 to ensure sufficient contact and reaction between the 2,4-di-tert-butylphenol and the phosphorus trichloride. The residence time of the materials in the reaction tube 5 is 260 seconds. Fourth, the hydrogen chloride gas generated by the reaction escapes upward through the gas-liquid separation valve 16, the exhaust pipe 17 and the connected pipe into the tail gas tank 18 as it is stirred by the rotating rod 9. The gas-liquid separation baffle 10 allows the reacted liquid to be transmitted backward through the air holes 11, and the hydrogen chloride gas is blocked on the side of the gas-liquid separation baffle 10 facing the motor 8; 5. The solution passing through the gas-liquid separation baffle 10 enters the distillation tank 6 through the output end of the reaction tube 5 and the pipeline between the reaction tube 5 and the distillation tank 6. Then, the organic solution and the alkaline catalyst in the solution are distilled into the neutralization tank 7 by heating distillation. Subsequently, sodium hydroxide solution is added to the neutralization tank 7 to neutralize the hydrogen chloride in the solution produced by the distillation to obtain a phosphorus trichloride solution. At the same time, the fan 19 is operated to absorb the hydrogen chloride escaping into the air during the reaction process and transfer it to the neutralization tank 7 for neutralization and absorption; 6. Before the solution in the neutralization tank 7 is discharged, the hydraulic cylinder 15 drives the heat conducting plate 12 to move backward toward the neutralization tank 7 and contact the neutralization tank 7, so that the heat of the neutralization tank 7 is transferred to the heat conducting plate 12, and then to the heat exchanger 13, and then the heat is transferred to the heat conducting plate 2 14 through the heat exchanger 13, thereby transferring the heat to the reaction liquid in the reaction tube 5, realizing heat recovery and reuse.

[0042] Example 4 1. As Figure 2-4As shown, 2,4-di-tert-butylphenol and an organic solution (ethyl acetate and diethyl ether in a mass ratio of 1:0.25) are injected into material box 1 as a raw material mixture, phosphorus trichloride solution is injected into material box 2, and an alkaline catalyst (tripropylamine and diazabicyclic in a mass ratio of 1:5) is injected into catalyst box 3. The liquid volumes of material box 1, material box 2, and catalyst box 3 are the same, and the molar ratio of 2,4-di-tert-butylphenol, phosphorus trichloride and alkaline catalyst is 3:1:0.2. 2. The raw material mixture in the material tank 1 and the phosphorus trichloride solution in the material tank 2 are respectively transferred into the heating mixing drum 4 through a pump and a pipeline for heating and mixing (the heating temperature is 45°C); 3. The liquid in the heated mixing drum 4 is transferred to the reaction tube 5 for reaction via a pump and a pipeline. At the same time, the alkaline catalyst in the catalyst box 3 is transferred to the inlet of the reaction tube 5 via a pipeline and a pump. The solution in the reaction tube 5 is evenly divided into two sections from the inlet end to the outlet end by a heating rod. The temperature of the first section of the reaction tube is controlled to 115° C. and the temperature of the second section of the reaction tube is controlled to 145° C. by the heating rod. Then, the motor 8 drives the rotating rod 9 to rotate. The raised stirring rod on the rotating rod 9 stirs the mixed solution in the reaction tube 5 to ensure sufficient contact and reaction between the 2,4-di-tert-butylphenol and the phosphorus trichloride. The residence time of the materials in the reaction tube 5 is 300 seconds. Fourth, the hydrogen chloride gas generated by the reaction escapes upward through the gas-liquid separation valve 16, the exhaust pipe 17 and the connected pipe into the tail gas tank 18 as it is stirred by the rotating rod 9. The gas-liquid separation baffle 10 allows the reacted liquid to be transmitted backward through the air holes 11, and the hydrogen chloride gas is blocked on the side of the gas-liquid separation baffle 10 facing the motor 8; 5. The solution passing through the gas-liquid separation baffle 10 enters the distillation tank 6 through the output end of the reaction tube 5 and the pipeline between the reaction tube 5 and the distillation tank 6. Then, the organic solution and the alkaline catalyst in the solution are distilled into the neutralization tank 7 by heating distillation. Subsequently, sodium hydroxide solution is added to the neutralization tank 7 to neutralize the hydrogen chloride in the solution produced by the distillation to obtain a phosphorus trichloride solution. At the same time, the fan 19 is operated to absorb the hydrogen chloride escaping into the air during the reaction process and transfer it to the neutralization tank 7 for neutralization and absorption; 6. Before the solution in the neutralization tank 7 is discharged, the hydraulic cylinder 15 drives the heat conducting plate 12 to move backward toward the neutralization tank 7 and contact the neutralization tank 7, so that the heat of the neutralization tank 7 is transferred to the heat conducting plate 12, and then to the heat exchanger 13, and then the heat is transferred to the heat conducting plate 2 14 through the heat exchanger 13, thereby transferring the heat to the reaction liquid in the reaction tube 5, realizing heat recovery and reuse.

[0043] Example 5 1. Inject 2,4-di-tert-butylphenol and an organic solution (ethyl acetate and diethyl ether in a mass ratio of 1:0.25) as a raw material mixture into material box 1, inject phosphorus trichloride solution into material box 2, and inject an alkaline catalyst (tripropylamine and diazabicyclic in a mass ratio of 1:5) into catalyst box 3. The liquid volumes of material box 1, material box 2, and catalyst box 3 are the same. At the same time, the molar ratio of 2,4-di-tert-butylphenol, phosphorus trichloride, and alkaline catalyst is 3:1:0.2; 2. The raw material mixture in the material tank 1 and the phosphorus trichloride solution in the material tank 2 are respectively transferred into the heating mixing drum 4 through a pump and a pipeline for heating and mixing (the heating temperature is 45°C); 3. The liquid in the heated mixing drum 4 is transferred to the reaction tube 5 for reaction through a pump and a pipeline. At the same time, the alkaline catalyst 3 in the catalyst box 3 is transferred to the inlet of the reaction tube 5 through a pipeline and a pump. The solution inside the reaction tube 5 is evenly divided into three sections from the inlet end to the outlet end. The temperature of the first section of the reaction tube is controlled to 45° C., the temperature of the second section of the reaction tube is 115° C., and the temperature of the third section of the reaction tube is 145° C. by a heating rod. Then, the motor 8 drives the rotating rod 9 to rotate. The raised stirring rod on the rotating rod 9 stirs the mixed liquid in the reaction tube 5 to ensure sufficient contact and reaction between 2,4-di-tert-butylphenol and phosphorus trichloride. The residence time of the materials in the reaction tube 5 is 300 seconds. Fourth, the hydrogen chloride gas generated by the reaction escapes upward through the gas-liquid separation valve 16, the exhaust pipe 17 and the connected pipe into the tail gas tank 18 as it is stirred by the rotating rod 9. The gas-liquid separation baffle 10 allows the reacted liquid to be transmitted backward through the air holes 11, and the hydrogen chloride gas is blocked on the side of the gas-liquid separation baffle 10 facing the motor 8; 5. The solution passing through the gas-liquid separation baffle 10 enters the distillation tank 6 through the output end of the reaction tube 5 and the pipeline between the reaction tube 5 and the distillation tank 6. Then, the organic solution and the alkaline catalyst in the solution are distilled into the neutralization tank 7 by heating distillation. Subsequently, sodium hydroxide solution is added to the neutralization tank 7 to neutralize the hydrogen chloride in the solution produced by the distillation to obtain a phosphorus trichloride solution. At the same time, the fan 19 is operated to absorb the hydrogen chloride escaping into the air during the reaction process and transfer it to the neutralization tank 7 for neutralization and absorption.

[0044] Example 6 1. As Figure 2-4 As shown, 2,4-di-tert-butylphenol and an organic solution (ethyl acetate and diethyl ether in a mass ratio of 1:0.25) are injected into material box 1 as a raw material mixture, phosphorus trichloride solution is injected into material box 2, and alkaline catalyst triethylamine is injected into catalyst box 3. The liquid volumes of material box 1, material box 2, and catalyst box 3 are the same, and the molar ratio of 2,4-di-tert-butylphenol, phosphorus trichloride and alkaline catalyst is 3:1:0.2. 2. The raw material mixture in the material tank 1 and the phosphorus trichloride solution in the material tank 2 are respectively transferred into the heating mixing drum 4 through a pump and a pipeline for heating and mixing (the heating temperature is 45°C); 3. The liquid in the heated mixing drum 4 is transferred to the reaction tube 5 for reaction through a pump and a pipeline. At the same time, the alkaline catalyst 3 in the catalyst box 3 is transferred to the inlet of the reaction tube 5 through a pipeline and a pump. The solution inside the reaction tube 5 is evenly divided into three sections from the inlet end to the outlet end. The temperature of the first section of the reaction tube is controlled to 45° C., the temperature of the second section of the reaction tube is 115° C., and the temperature of the third section of the reaction tube is 145° C. by a heating rod. Then, the motor 8 drives the rotating rod 9 to rotate. The raised stirring rod on the rotating rod 9 stirs the mixed liquid in the reaction tube 5 to ensure sufficient contact and reaction between 2,4-di-tert-butylphenol and phosphorus trichloride. The residence time of the materials in the reaction tube 5 is 300 seconds. Fourth, the hydrogen chloride gas generated by the reaction escapes upward through the gas-liquid separation valve 16, the exhaust pipe 17 and the connected pipe into the tail gas tank 18 as it is stirred by the rotating rod 9. The gas-liquid separation baffle 10 allows the reacted liquid to be transmitted backward through the air holes 11, and the hydrogen chloride gas is blocked on the side of the gas-liquid separation baffle 10 facing the motor 8; 5. The solution passing through the gas-liquid separation baffle 10 enters the distillation tank 6 through the output end of the reaction tube 5 and the pipeline between the reaction tube 5 and the distillation tank 6. Then, the organic solution and the alkaline catalyst in the solution are distilled into the neutralization tank 7 by heating distillation. Subsequently, sodium hydroxide solution is added to the neutralization tank 7 to neutralize the hydrogen chloride in the solution produced by the distillation to obtain a phosphorus trichloride solution. At the same time, the fan 19 is operated to absorb the hydrogen chloride escaping into the air during the reaction process and transfer it to the neutralization tank 7 for neutralization and absorption; 6. Before the solution in the neutralization tank 7 is discharged, the hydraulic cylinder 15 drives the heat conducting plate 12 to move backward toward the neutralization tank 7 and contact the neutralization tank 7, so that the heat of the neutralization tank 7 is transferred to the heat conducting plate 12, and then to the heat exchanger 13, and then the heat is transferred to the heat conducting plate 2 14 through the heat exchanger 13, thereby transferring the heat to the reaction liquid in the reaction tube 5, realizing heat recovery and reuse.

[0045] Example 7 1. As Figure 2-4 As shown, 2,4-di-tert-butylphenol and an organic solution (ethyl acetate and ether in a mass ratio of 1:0.25) are injected into material box 1 as a raw material mixture, phosphorus trichloride solution is injected into material box 2, and the alkaline catalyst diazabicyclo is injected into catalyst box 3. The liquid volumes of material box 1, material box 2, and catalyst box 3 are the same, and the molar ratio of 2,4-di-tert-butylphenol, phosphorus trichloride and alkaline catalyst is 3:1:0.2; 2. The raw material mixture in the material tank 1 and the phosphorus trichloride solution in the material tank 2 are respectively transferred into the heating mixing drum 4 through a pump and a pipeline for heating and mixing (the heating temperature is 45°C); 3. The liquid in the heated mixing drum 4 is transferred to the reaction tube 5 for reaction through a pump and a pipeline. At the same time, the alkaline catalyst 3 in the catalyst box 3 is transferred to the inlet of the reaction tube 5 through a pipeline and a pump. The solution inside the reaction tube 5 is evenly divided into three sections from the inlet end to the outlet end. The temperature of the first section of the reaction tube is controlled to 45° C., the temperature of the second section of the reaction tube is 115° C., and the temperature of the third section of the reaction tube is 145° C. by a heating rod. Then, the motor 8 drives the rotating rod 9 to rotate. The raised stirring rod on the rotating rod 9 stirs the mixed liquid in the reaction tube 5 to ensure sufficient contact and reaction between 2,4-di-tert-butylphenol and phosphorus trichloride. The residence time of the materials in the reaction tube 5 is 300 seconds. Fourth, the hydrogen chloride gas generated by the reaction escapes upward through the gas-liquid separation valve 16, the exhaust pipe 17 and the connected pipe into the tail gas tank 18 as it is stirred by the rotating rod 9. The gas-liquid separation baffle 10 allows the reacted liquid to be transmitted backward through the air holes 11, and the hydrogen chloride gas is blocked on the side of the gas-liquid separation baffle 10 facing the motor 8; 5. The solution passing through the gas-liquid separation baffle 10 enters the distillation tank 6 through the output end of the reaction tube 5 and the pipeline between the reaction tube 5 and the distillation tank 6. Then, the organic solution and the alkaline catalyst in the solution are distilled into the neutralization tank 7 by heating distillation. Subsequently, sodium hydroxide solution is added to the neutralization tank 7 to neutralize the hydrogen chloride in the solution produced by the distillation to obtain a phosphorus trichloride solution. At the same time, the fan 19 is operated to absorb the hydrogen chloride escaping into the air during the reaction process and transfer it to the neutralization tank 7 for neutralization and absorption; 6. Before the solution in the neutralization tank 7 is discharged, the hydraulic cylinder 15 drives the heat conducting plate 12 to move backward toward the neutralization tank 7 and contact the neutralization tank 7, so that the heat of the neutralization tank 7 is transferred to the heat conducting plate 12, and then to the heat exchanger 13, and then the heat is transferred to the heat conducting plate 2 14 through the heat exchanger 13, thereby transferring the heat to the reaction liquid in the reaction tube 5, realizing heat recovery and reuse.

[0046] Example 8 1. As Figure 2-4 As shown, 2,4-di-tert-butylphenol and an organic solution (ethyl acetate and diethyl ether in a mass ratio of 1:0.25) are injected into material box 1 as a raw material mixture, phosphorus trichloride solution is injected into material box 2, and alkaline catalyst tripropylamine is injected into catalyst box 3. The liquid volumes of material box 1, material box 2, and catalyst box 3 are the same, and the molar ratio of 2,4-di-tert-butylphenol, phosphorus trichloride and alkaline catalyst is 3:1:0.2. 2. The raw material mixture in the material tank 1 and the phosphorus trichloride solution in the material tank 2 are respectively transferred into the heating mixing drum 4 through a pump and a pipeline for heating and mixing (the heating temperature is 45°C); 3. The liquid in the heated mixing drum 4 is transferred to the reaction tube 5 for reaction through a pump and a pipeline. At the same time, the alkaline catalyst 3 in the catalyst box 3 is transferred to the inlet of the reaction tube 5 through a pipeline and a pump. The solution inside the reaction tube 5 is evenly divided into three sections from the inlet end to the outlet end. The temperature of the first section of the reaction tube is controlled to 45° C., the temperature of the second section of the reaction tube is 115° C., and the temperature of the third section of the reaction tube is 145° C. by a heating rod. Then, the motor 8 drives the rotating rod 9 to rotate. The raised stirring rod on the rotating rod 9 stirs the mixed liquid in the reaction tube 5 to ensure sufficient contact and reaction between 2,4-di-tert-butylphenol and phosphorus trichloride. The residence time of the materials in the reaction tube 5 is 300 seconds. Fourth, the hydrogen chloride gas generated by the reaction escapes upward through the gas-liquid separation valve 16, the exhaust pipe 17 and the connected pipe into the tail gas tank 18 as it is stirred by the rotating rod 9. The gas-liquid separation baffle 10 allows the reacted liquid to be transmitted backward through the air holes 11, and the hydrogen chloride gas is blocked on the side of the gas-liquid separation baffle 10 facing the motor 8; 5. The solution passing through the gas-liquid separation baffle 10 enters the distillation tank 6 through the output end of the reaction tube 5 and the pipeline between the reaction tube 5 and the distillation tank 6. Then, the organic solution and the alkaline catalyst in the solution are distilled into the neutralization tank 7 by heating distillation. Subsequently, sodium hydroxide solution is added to the neutralization tank 7 to neutralize the hydrogen chloride in the solution produced by the distillation to obtain a phosphorus trichloride solution. At the same time, the fan 19 is operated to absorb the hydrogen chloride escaping into the air during the reaction process and transfer it to the neutralization tank 7 for neutralization and absorption; 6. Before the solution in the neutralization tank 7 is discharged, the hydraulic cylinder 15 drives the heat conducting plate 12 to move backward toward the neutralization tank 7 and contact the neutralization tank 7, so that the heat of the neutralization tank 7 is transferred to the heat conducting plate 12, and then to the heat exchanger 13, and then the heat is transferred to the heat conducting plate 2 14 through the heat exchanger 13, thereby transferring the heat to the reaction liquid in the reaction tube 5, realizing heat recovery and reuse.

[0047] Example 9 1. As Figure 2-4 As shown, 2,4-di-tert-butylphenol and organic solvent toluene are injected into material box 1 as a raw material mixture, phosphorus trichloride solution is injected into material box 2, and alkaline catalyst (tripropylamine and diazabicyclic with a mass ratio of 1:5) is injected into catalyst box 3. The liquid volumes of material box 1, material box 2 and catalyst box 3 are the same, and the molar ratio of 2,4-di-tert-butylphenol, phosphorus trichloride and alkaline catalyst is 3:1:0.2; 2. The raw material mixture in the material tank 1 and the phosphorus trichloride solution in the material tank 2 are respectively transferred into the heating mixing drum 4 through a pump and a pipeline for heating and mixing (the heating temperature is 45°C); 3. The liquid in the heated mixing drum 4 is transferred to the reaction tube 5 for reaction through a pump and a pipeline. At the same time, the alkaline catalyst 3 in the catalyst box 3 is transferred to the inlet of the reaction tube 5 through a pipeline and a pump. The solution inside the reaction tube 5 is evenly divided into three sections from the inlet end to the outlet end. The temperature of the first section of the reaction tube is controlled to 45° C., the temperature of the second section of the reaction tube is 115° C., and the temperature of the third section of the reaction tube is 145° C. by a heating rod. Then, the motor 8 drives the rotating rod 9 to rotate. The raised stirring rod on the rotating rod 9 stirs the mixed liquid in the reaction tube 5 to ensure sufficient contact and reaction between 2,4-di-tert-butylphenol and phosphorus trichloride. The residence time of the materials in the reaction tube 5 is 300 seconds. Fourth, the hydrogen chloride gas generated by the reaction escapes upward through the gas-liquid separation valve 16, the exhaust pipe 17 and the connected pipe into the tail gas tank 18 as it is stirred by the rotating rod 9. The gas-liquid separation baffle 10 allows the reacted liquid to be transmitted backward through the air holes 11, and the hydrogen chloride gas is blocked on the side of the gas-liquid separation baffle 10 facing the motor 8; 5. The solution passing through the gas-liquid separation baffle 10 enters the distillation tank 6 through the output end of the reaction tube 5 and the pipeline between the reaction tube 5 and the distillation tank 6. Then, the organic solution and the alkaline catalyst in the solution are distilled into the neutralization tank 7 by heating distillation. Subsequently, sodium hydroxide solution is added to the neutralization tank 7 to neutralize the hydrogen chloride in the solution produced by the distillation to obtain a phosphorus trichloride solution. At the same time, the fan 19 is operated to absorb the hydrogen chloride escaping into the air during the reaction process and transfer it to the neutralization tank 7 for neutralization and absorption; 6. Before the solution in the neutralization tank 7 is discharged, the hydraulic cylinder 15 drives the heat conducting plate 12 to move backward toward the neutralization tank 7 and contact the neutralization tank 7, so that the heat of the neutralization tank 7 is transferred to the heat conducting plate 12, and then to the heat exchanger 13, and then the heat is transferred to the heat conducting plate 2 14 through the heat exchanger 13, thereby transferring the heat to the reaction liquid in the reaction tube 5, realizing heat recovery and reuse.

[0048] Performance Testing 1. Product solution component analysis: Use gas chromatography to test the content of antioxidant 168 in the solution passing through the gas-liquid separation baffle 10. After deducting the peaks of the solvent, catalyst and organic solvent used to prepare the sample, the content of antioxidant 168 is analyzed according to the area normalization method.

[0049] 2. Power consumption detection: Detect the power consumed in each embodiment within the same period of time.

[0050] Performance test data table of each embodiment Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 Example 8 Embodiment 9 Gas chromatography content of antioxidants (%) 95.31 96.23 94.16 90.56 95.29 86.45 88.35 81.72 88.92 Power consumption (kwh) 4.5 4.6 4.3 4.5 6.4 4.8 4.6 4.5 4.4 As can be seen from the chart, when the alkaline catalyst is within a suitable range and the dosage increases, the catalytic effect on 2,4-di-tert-butylphenol and phosphorus trichloride becomes better, the phosphorus trichloride conversion effect becomes higher, and thus the yield of antioxidant 168 becomes higher. At the same time, the heat conducting plate 12, heat exchanger 13 and heat conducting plate 2 14 provided can transfer the heat in the neutralization tank 7 to the lower temperature area in the front section of the reaction tube 5, thereby increasing the heat utilization efficiency and saving electricity.

[0051] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims rather than the foregoing description. It is intended that all variations within the meaning and range of equivalents of the claims be embraced herein, and any reference signs in the claims should not be construed as limiting the rights involved.

Claims

1. A method for continuously synthesizing antioxidant 168, characterized in that: The following steps are involved: a: injecting the raw material mixture of 2,4-di-tert-butylphenol and organic solution into material box one (1), injecting phosphorus trichloride solution into material box two (2), and injecting alkaline catalyst into catalyst box (3); b: The raw material mixed liquid in the material box 1 (1) and the phosphorus trichloride solution in the material box 2 (2) are respectively transferred into the heating mixing cylinder (4) through a pump and a pipeline for heating and mixing; c: The liquid in the heating mixing cylinder (4) is transferred into the reaction tube (5) through a pump and a pipeline for reaction, and the alkaline catalyst in the catalyst box (3) is transferred into the inlet of the reaction tube (5) through a pipeline and a pump, and then the motor (8) drives the rotating rod (9) to rotate, and the protruding stirring rod on the rotating rod (9) stirs the mixed liquid, so that the 2,4-di-tert-butylphenol and the phosphorus trichloride solution are fully contacted and reacted; d: The hydrogen chloride gas generated by the reaction escapes upward through the gas-liquid separation valve (16), the exhaust pipe (17) and the connected pipe into the tail gas tank (18) as the rotating rod (9) stirs. The gas-liquid separation baffle (10) allows the liquid after the reaction to be transmitted backward through the air hole (11). The hydrogen chloride gas is blocked on the side of the gas-liquid separation baffle (10) facing the motor (8); e: the solution passing through the gas-liquid separation baffle (10) enters the distillation tank (6) through the output end of the reaction tube (5) and the pipeline between the reaction tube (5) and the distillation tank (6), and then the organic solution and the alkaline catalyst in the solution are distilled into the neutralization tank (7) by heating distillation, and then sodium hydroxide solution is added to the neutralization tank (7) to neutralize the hydrogen chloride in the solution produced by the distillation, and at the same time, the fan (19) is operated to absorb the hydrogen chloride escaping into the air during the reaction process and transfer it to the neutralization tank (7) for neutralization and absorption; f: Before the solution in the neutralization tank (7) is discharged, the hydraulic cylinder (15) drives the heat transfer plate 1 (12) to move backward toward the neutralization tank (7) and contact the neutralization tank (7), so that the heat of the neutralization tank (7) is transferred to the heat transfer plate 1 (12), and then to the heat exchanger (13), and then the heat is transferred to the heat transfer plate 2 (14) through the heat exchanger (13), thereby transferring the heat to the reaction liquid in the reaction tube (5), thereby realizing the recovery and reuse of heat.

2. The method for continuously synthesizing antioxidant 168 according to claim 1, characterized in that: The organic solvent is at least one of ethyl acetate, toluene, xylene, ether and acetonitrile.

3. The method for continuously synthesizing antioxidant 168 according to claim 1, characterized in that: The alkaline catalyst is selected from at least one of triethylamine, tripropylamine, diazabicyclo and hexamethylenetetramine.

4. The method for continuously synthesizing antioxidant 168 according to claim 1, characterized in that: The molar ratio of 2,4-di-tert-butylphenol, phosphorus trichloride and alkaline catalyst in the material box 1 (1), the material box 2 (2) and the catalyst box (3) is 3:1:0.2-0.

3.

5. The method for continuously synthesizing antioxidant 168 according to claim 1, characterized in that: In step b, the temperature of heating and mixing is 40-50°C.

6. The method for continuously synthesizing antioxidant 168 according to claim 1, characterized in that: In step c, the temperature of the solution inside the reaction tube (5) increases from the inlet end to the outlet end, and the temperature ranges from 40 to 150°C.

7. The method for continuously synthesizing antioxidant 168 according to claim 6, characterized in that: The solution inside the reaction tube (5) is evenly divided into three sections from the inlet end to the outlet end, and the temperature of the first section of the reaction tube is controlled to be 40-50°C, the temperature of the second section of the reaction tube is controlled to be 100-120°C, and the temperature of the third section of the reaction tube is controlled to be 140-150°C.

8. The method for continuously synthesizing antioxidant 168 according to claim 6, characterized in that: In step c, when the contact reaction is sufficient, the residence time is 260-300s.

9. A device for continuously synthesizing an antioxidant 168, characterized in that: The device includes: A material box (1) for providing a raw material mixed solution of 2,4-di-tert-butylphenol and an organic solution, a material box (2) for providing a phosphorus trichloride solution, and a catalyst box (3) for providing an alkaline catalyst; A heating mixing cylinder (4) connected to the material box 1 (1) and the material box 2 (2) respectively through a pump and a pipeline; The liquid is transmitted into the reaction tube (5) through a pump and a pipeline connected to the heating mixing cylinder (4); A catalyst box (3) connected to the inlet of the reaction tube (5) through a pipeline and a pump; A rotating rod (9) having a parallel end penetrating the front inner wall of the reaction tube (5); The device also includes a motor (8), a fan (19), an air intake pipe (20), a neutralization tank (7), a hydraulic cylinder (15), a first heat conducting plate (12), a second heat conducting plate (14), and a heat exchanger (13); The output end of the motor (8) is connected to one end of a rotating rod (9), and one end of the rotating rod (9) penetrates the front inner wall of the reaction tube (5); The input end of the fan (19) is connected to the bottom output end of the air intake pipe (20) through a pipeline, a plurality of holes are formed through the top of the air intake pipe (20), and the output end of the fan (19) is connected to the front input end of the neutralization tank (7) through a pipeline; A plurality of gas-liquid separation baffles (10) are arranged at equal intervals on the outer side of the rotating rod (9), and the air holes (11) are arranged through the gas-liquid separation baffles (10) at positions close to the rotating rod (9); One end of the piston rod at the output end of the hydraulic cylinder (15) is connected to the front surface of the heat conducting plate 1 (12), and the material of the heat conducting plate 1 (12) and the heat conducting plate 2 (14) is one of iron, aluminum and copper; The heat exchanger (13) is in movable contact with the heat exchanger neutralization tank (7) and the hot plate 1 (12) respectively; The surface of the rotating rod (9) is provided with a protrusion.

10. The device for continuously synthesizing antioxidant 168 according to claim 9, characterized in that: A heating rod and a temperature sensor are arranged on the inner wall of the reaction tube (5); Along the material flow direction, the reaction tube (5) is evenly divided into three sections, and a heating rod and a temperature sensor are respectively arranged on the inner walls of the first section reaction tube, the second section reaction tube and the third section reaction tube.

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