A reaction device for esterification of trimellitic anhydride with dihydric phenol or dihydric alcohol

Abstract

The utility model discloses a reaction device for double partial trimellitic anhydride binary phenol or binary alcohol ester in the field of chemical equipment, and the kettle body is equipped with stirring vane, and the stirring vane includes upper layer stirring vane and lower layer stirring vane, is equipped with upper layer material distributor below upper layer stirring vane, and upper layer material distributor is connected with material import no. 1, is equipped with lower layer material distributor below lower layer stirring vane, and lower layer material distributor is connected with material import no. 2, and the lower part of kettle body is equipped with support, and the lower side of support is installed with the isolation cylinder that is coaxial with stirring shaft, and the isolation cylinder is kept with the inner wall of kettle body and the inner bottom of kettle body liquid flow channel, and the outside of lower layer stirring vane is connected with scraper, and the scraper is close to the inside of isolation cylinder and sets up. Its through the setting of isolation cylinder and scraper, forms homogeneous phase liquid membrane, increases the reaction area, makes material mixing more fully, accelerates the interface reaction rate of trimellitic anhydride and binary phenol or binary alcohol, can reduce the reaction difficulty and improve the reaction conversion rate.

Description

Technical Field

[0001] This utility model relates to a reaction apparatus for chemical production, specifically a production apparatus for synthesizing high-purity bis(triphenyl)-p-butyl trihydric anhydride diphenol (or diol) esters. It belongs to the field of organic chemical equipment. Background Technology

[0002] Diphenyltriglyceride, a diphenol or diol ester (abbreviated as ester anhydride), is an important organic compound mainly used in the synthesis of polymer materials. These compounds are typically prepared by esterification of diphenyltriglyceride with diphenols or diols. Ester anhydrides possess a unique molecular structure, combining the characteristics of both acid anhydrides and esters, thus exhibiting excellent thermal stability, mechanical properties, and chemical inertness.

[0003] In materials science, ester anhydrides are widely used in the manufacture of high-performance polymers, such as polyimide (PI) and polyesterimide (PEI). These polymers possess high strength, high modulus, excellent heat resistance, and electrical insulation properties, making them ideal for manufacturing critical components in high-tech fields such as aerospace, electronics, and automotive parts. Furthermore, ester anhydrides can also be used as crosslinking agents, plasticizers, or modifiers to improve the properties of other polymers. By adjusting the molecular structure and content of ester anhydrides, the physical and chemical properties of polymers can be controlled to meet diverse application requirements.

[0004] In summary, bis(p-phenylene trioxide) anhydride, a diphenol or diol ester (ester anhydride), is a powerful organic compound with broad application prospects in the field of polymer materials. With continuous technological advancements and the ongoing development of novel polymer materials, the importance of ester anhydrides will become increasingly prominent.

[0005] In existing technologies, ester anhydrides are commonly produced using batch reactors equipped with mechanical stirring. This involves placing a stirring shaft inside the reactor, with stirring blades mounted on it. Materials are fed into the reactor and reacted through stirring to produce ester anhydrides. However, this method has several drawbacks. Trimeric trihydric anhydride contains an anhydride group and a carboxyl functional group. The ester formed after reacting with a bisphenol or diol has a rigid benzene ring skeleton and long ester chains. The rigid structure of the benzene ring increases the intermolecular packing density, while the interaction of the ester chains further enhances intermolecular entanglement, leading to increased internal friction and viscosity during fluid flow. The reaction requires multiple solvents and reaction aids, and the solution transforms from a homogeneous phase to a multiphase mixture, affecting the mixing efficiency. Furthermore, during the reaction, lighter, more fluid materials rise, while materials with high viscosity and density accumulate at the bottom of the reactor, further hindering the reaction. Stirring by the blades alone is insufficient to achieve optimal reaction results, resulting in a difficult reaction with a low conversion rate. Utility Model Content

[0006] The purpose of this invention is to provide a reaction apparatus for bis(triphenyl phthalic anhydride) diphenols or diol esters, which allows for more thorough mixing of materials, reduces reaction difficulty, and increases reaction conversion rate.

[0007] The purpose of this invention is achieved as follows: A reaction apparatus for bis(triphenyl phthalic anhydride) diphenols or diol esters includes a vertically arranged vessel body, a motor at the top of the vessel body, and a stirring shaft connected to the output end of the motor. The stirring shaft is inserted downward into the vessel body, and stirring blades are respectively provided in the middle and lower part of the stirring shaft. A discharge port is provided at the bottom of the vessel body, a gas phase outlet is provided at the top of the vessel body, and a material inlet is provided on the side of the vessel body. The material inlet includes material inlet one and material inlet two. The stirring blades include upper stirring blades and lower stirring blades. An upper material distributor is provided below the upper stirring blades and is connected to material inlet one. A lower material distributor is provided below the lower stirring blades and is connected to material inlet two. A support is provided at the bottom of the vessel body, and an isolation cylinder coaxially arranged with the stirring shaft is installed on the lower side of the support. A liquid flow channel is provided between the isolation cylinder and the inner wall and bottom of the vessel body. A scraper is connected to the outer side of the lower stirring blades and is arranged close to the inner side of the isolation cylinder.

[0008] In operation, the reactor is filled with trimellitic anhydride chloride and a solvent. The solvent can be one or more compound solvents selected from THF, acetonitrile, DMF, NMP, and acetone. An acidic catalyst and a co-catalyst are also injected into the reactor. Material inlet one is used to inject diols or diphenols, and material inlet two is used to add a mixed solvent containing diphenols or diols in batches. During the reaction, the reactants are continuously stirred by a stirring device. The stirring blades push the reactants downwards; high-viscosity materials gradually sink after formation, while lighter materials float. A scraper can evenly coat the high-viscosity materials on the inner wall of the isolation cylinder, forming a homogeneous liquid film, increasing the reaction area and thus promoting the forward reaction. Some low-boiling-point liquids rise to the gas phase outlet and then condense and reflux. Compared with the prior art, the beneficial effects of this utility model are as follows: by setting up the isolation cylinder and scraper, a homogeneous liquid film is formed, the reaction area is increased, the material is mixed more thoroughly, the interfacial reaction rate of trimellitic anhydride and diphenol or diol is accelerated, the reaction difficulty is reduced and the reaction conversion rate is improved.

[0009] Furthermore, a jacket is provided on the outer side of the middle of the vessel, facing downwards. The jacket has a hot water inlet and a hot water outlet. Heating with hot water can promote the forward reaction. The reaction temperature is controlled between 20 and 70°C by introducing hot water through the jacket.

[0010] Furthermore, a gas distribution pipe is provided inside the reactor body, and the gas distribution pipe is connected to a gas source via an air inlet pipe; the gas distribution pipe is arranged in a circular shape on the outside of the isolation cylinder, and the surface of the gas distribution pipe has several air holes. Air is introduced through the gas distribution pipe, forming an upward force, which, under the propulsion of the stirring blades, creates convection inside and outside the isolation cylinder, thereby promoting the reaction.

[0011] To facilitate mixing of the reactants, the upper and lower material distributors are circular tubular, and the surfaces of the upper and lower material distributors are provided with several liquid inlet micropores.

[0012] Furthermore, the bottom of the reactor body is equipped with several vertically arranged heaters, which are arranged in a row. Each heater is a U-shaped steam pipe that extends upwards above the lower material distributor. Further heating of the viscous material through the steam pipes reduces the viscosity of the reaction solution, ensuring complete esterification. To ensure stable operation of the stirring shaft, a bearing is provided at the position where the stirring shaft passes through the bracket.

[0013] Furthermore, a gap of 1-3 mm is left between the scraper and the inner wall of the isolation cylinder. Attached Figure Description

[0014] Figure 1 This is a schematic diagram of the structure of this utility model.

[0015] Figure 2 for Figure 1 A magnified view of part A in the image.

[0016] In the diagram, 1 is the temperature measuring port, 2 is the isolation cylinder, 3 is the scraper, 4 is the bracket, 5 is the hot water outlet, 6 is the material inlet 1, 7 is the material inlet 2, 8 is the gas phase outlet, 9 is the motor, 10 is the vessel body, 11 is the upper stirring blade, 12 is the jacket, 13 is the upper material distributor, 14 is the stirring shaft, 15 is the lower stirring blade, 16 is the air distribution pipe, 17 is the air inlet pipe, 18 is the discharge port, 19 is the heater, 20 is the lower material distributor, and 21 is the hot water inlet. Detailed Implementation

[0017] like Figure 1 , 2The diagram shows a reaction apparatus for bis(triphenyl phthalic anhydride) diphenols or diol esters, comprising a vertically arranged vessel body 10, a motor 9 mounted on the top of the vessel body 10, and a stirring shaft 14 connected to the output end of the motor 9. The stirring shaft 14 is inserted downwards into the vessel body 10, and stirring blades are respectively provided in the middle and lower parts of the stirring shaft 14. A discharge port 18 is provided at the bottom of the vessel body 10, a gas phase outlet 8 is provided at the top of the vessel body 10, and a material inlet is provided on the side of the vessel body 10. The material inlet includes material inlet 1 6 and material inlet 2 7. The stirring blades include an upper stirring blade 11 and a lower stirring blade 12. A stirring blade 15 is provided; an upper material distributor 13 is provided below the upper stirring blade 11, and the upper material distributor 13 is connected to the material inlet 6; a lower material distributor 20 is provided below the lower stirring blade 15, and the lower material distributor 20 is connected to the material inlet 7; a support 4 is provided at the lower part of the vessel body 10, and an isolation cylinder 2 is installed on the lower side of the support 4, which is coaxial with the stirring shaft 14. The isolation cylinder 2, the inner wall of the vessel body 10, and the bottom of the vessel body 10 have liquid flow channels. A scraper 3 is connected to the outer side of the lower stirring blade 15, and the scraper 3 is set close to the inner side of the isolation cylinder 2.

[0018] Furthermore, a jacket 12 is provided on the outer side of the middle of the vessel body 10, facing downwards. The jacket 12 has a hot water inlet 21 and a hot water outlet 5. The reaction can be promoted by introducing hot water for heating. The reaction temperature is controlled between 20 and 70°C by introducing hot water through the jacket 12.

[0019] Furthermore, a gas distribution pipe 16 is provided inside the vessel body 10, and the gas distribution pipe 16 is connected to a gas source via an air inlet pipe 17; the gas distribution pipe 16 is generally arranged in a circular shape on the outside of the isolation cylinder 2, and a number of air holes are provided on the surface of the gas distribution pipe 16. Air is introduced through the gas distribution pipe 16 to form an upward force, and under the propulsion action of the stirring blades, convection is formed inside and outside the isolation cylinder 2, which promotes the reaction.

[0020] To facilitate mixing of the reactants, the upper material distributor 13 and the lower material distributor 20 are circular tubular, and the surfaces of the upper material distributor 13 and the lower material distributor 20 are provided with a number of liquid inlet micropores.

[0021] Furthermore, the bottom of the vessel body 10 is provided with several vertically arranged heaters 19, which are arranged in an array. Each heater 19 is a U-shaped steam pipe that extends upwards above the lower material distributor 20. Further heating of the viscous material through the steam pipes reduces the viscosity of the reaction solution, ensuring complete esterification. To ensure stable operation of the stirring shaft 14, a bearing is provided at the position where the stirring shaft 14 passes through the bracket 4.

[0022] Furthermore, a gap of 1-3mm is left between the scraper 3 and the inner wall of the isolation cylinder 2.

[0023] The vessel body 10 is also equipped with a temperature measuring port 1 and a manhole.

[0024] Trimeric trihydride is an aromatic compound containing one anhydride group and one carboxylic acid group, and is commonly produced from trimellitic anhydride acyl chloride as a raw material. Examples of diphenols or diols that provide such trimellitic anhydride diphenols or diol esters (ester anhydrides) include aliphatic diols and aromatic diols or diphenols such as ethylene glycol, propylene glycol, 1,4-butanediol, 1,8-octanediol, 1,12-dodecanediol, cyclohexanediol, hydrogenated bisphenol A, hydroquinone, resorcinol, bisphenol A, bisphenol S, 2,2-bis(4-hydroxyphenyl)hexafluoropropane, and 4,4'-dihydroxydiphenyl ether.

[0025] During operation, the reactor body 10 is filled with trimellitic anhydride chloride and solvent. The solvent can be one or more compound solvents selected from THF, acetonitrile, DMF, NMP, and acetone. Acidic catalyst and co-catalyst are also injected into the reactor body 10. Material inlet 6 is used to inject diols or diphenols, and material inlet 7 is used to add a mixed solvent containing diphenols or diols in batches. During the reaction, the reactants are continuously stirred by a stirring device. The stirring blades push the reactants downwards; high-viscosity materials gradually sink after formation, while lighter materials float. The scraper 3 can evenly coat the high-viscosity materials on the inner wall of the isolation cylinder 2, forming a homogeneous liquid film, increasing the reaction area and thus promoting the forward reaction. Some low-boiling-point liquids rise to the gas phase outlet 8 and then condense and reflux. Compared with the prior art, the beneficial effects of this utility model are as follows: by setting up the isolation cylinder 2 and the scraper 3, a homogeneous liquid film is formed, the reaction area is increased, the material is mixed more thoroughly, the interfacial reaction rate of bis(triphenyl benzoic anhydride) and diphenol or diol is accelerated, the reaction difficulty is reduced and the reaction conversion rate is improved.

[0026] Practice has proven that, after 48 hours of operation using the equipment described in this embodiment, the conversion rate of bis(triphenyl)-triglyceride diphenols or diol esters (ester anhydrides) is >99%, with minimal temperature and pressure fluctuations and a general reduction in energy consumption of 10%. The reaction process is safe and environmentally friendly, with minimal equipment wear and tear, and the operation is simple, demonstrating the reliability and effectiveness of the ester anhydride synthesis device of this invention.

[0027] This utility model is not limited to the above embodiments. Based on the technical solutions disclosed in this utility model, those skilled in the art can make some substitutions and modifications to some of the technical features without creative labor, and these substitutions and modifications are all within the protection scope of this utility model.

Claims

1. A reaction device for esterification of trimellitic anhydride with dihydric phenol or dihydric alcohol, comprising a kettle body arranged vertically, a motor arranged at the top of the kettle body, an output end of the motor being drivingly connected with a stirring shaft, the stirring shaft being inserted into the kettle body downward, stirring blades being arranged at the middle and lower part of the stirring shaft respectively, a discharge port being arranged at the bottom of the kettle body, a gas phase outlet being arranged at the top of the kettle body, and a material inlet being arranged at the side of the kettle body, characterized in that: The material inlets include Material Inlet 1 and Material Inlet 2. The stirring blades include upper stirring blades and lower stirring blades. An upper material distributor is provided below the upper stirring blades and is connected to Material Inlet 1. A lower material distributor is provided below the lower stirring blades and is connected to Material Inlet 2. A support is provided at the bottom of the vessel body. An isolation cylinder coaxially arranged with the stirring shaft is installed on the lower side of the support. Liquid flow channels are left between the isolation cylinder and the inner wall and bottom of the vessel body. A scraper is connected to the outer side of the lower stirring blades and is set close to the inner wall of the isolation cylinder. ​ 2. The reaction apparatus for bis(triphenyl phthalic anhydride) diphenols or diol esters according to claim 1, characterized in that: The outer side of the middle of the vessel body is provided with a jacket, and the jacket is provided with a hot water inlet and a hot water outlet.

3. The reaction apparatus for bis(triphenyl phthalic anhydride) diphenols or diol esters according to claim 1, characterized in that: The vessel body is equipped with a gas distribution pipe, which is connected to a gas source via an air inlet pipe; the gas distribution pipe is arranged in a circular shape on the outside of the isolation cylinder, and the surface of the gas distribution pipe is provided with several air holes.

4. A reaction apparatus for bis(triphenyl phthalic anhydride) diphenols or diol esters according to any one of claims 1-3, characterized in that: The upper and lower material distributors are circular tubular, and the surfaces of the upper and lower material distributors are provided with several liquid inlet micro-holes.

5. A reaction apparatus for bis(triphenyl phthalic anhydride) diphenols or diol esters according to any one of claims 1-3, characterized in that: The bottom of the vessel body is equipped with several vertically installed heaters, which are arranged in a row.

6. The reaction apparatus for bis(triphenyl phthalic anhydride) diphenols or diol esters according to claim 5, characterized in that: The heater is a U-shaped steam pipe that extends upwards above the lower material distributor.

7. A reaction apparatus for bis(triphenyl phthalic anhydride) diphenols or diol esters according to any one of claims 1-3, characterized in that: A bearing is provided at the location where the stirring shaft passes through the support.

8. A reaction apparatus for bis(triphenyl phthalic anhydride) diphenols or diol esters according to any one of claims 1-3, characterized in that: A gap of 1-3 mm is left between the scraper and the inner wall of the isolation cylinder.

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