CN218981512U

CN218981512U - Reaction device for preparing biphenyl dianhydride

Info

Publication number: CN218981512U
Application number: CN202223020135.3U
Authority: CN
Inventors: 梅雪; 杜庶铭; 王文宾
Original assignee: Taixing Zhongke Aide Membrane Material Technology Co ltd
Current assignee: Taixing Zhongke Aide Membrane Material Technology Co ltd
Priority date: 2022-11-14
Filing date: 2022-11-14
Publication date: 2023-05-09
Anticipated expiration: 2032-11-14

Abstract

The utility model discloses a reaction device for preparing biphenyl dianhydride, which comprises: the catalyst recycling device is used for inputting a catalyst into the coupling reaction device and recycling the used catalyst; wherein the catalyst circulation device comprises: the catalyst circulating device is arranged, so that the catalyst can be recycled, the contact time of the catalyst and air is greatly reduced, and the service life of the catalyst is long.

Description

Reaction device for preparing biphenyl dianhydride

Technical Field

The embodiment of the utility model relates to the field of preparation of biphenyl dianhydride, in particular to a reaction device for preparing biphenyl dianhydride.

Background

The biphenyl dianhydride is an important fine chemical intermediate and is mainly used for synthesizing biphenyl polyimide. The polyimide is a polymer material mainly composed of aromatic imide structural units in a molecular main chain, and the product prepared from the polyimide has excellent mechanical property, electrical insulation property, high and low temperature resistance, wear resistance and radiation resistance, high strength, high rigidity and dimensional stability, and can be used for a long time at high temperature. The processability of pure polyimide is poor, but the processability can be improved by adjusting the molecular chemical structure of the polymer, such as introducing diphenyl ether groups and bending groups, and the processability is improved on the basis of maintaining higher service performance, so that the improved polyaramid has excellent processability and can be used for injection molding or extrusion molding. In recent years, polyimide special engineering plastics are increasingly widely applied, and the daily demand of the polyimide special engineering plastics is gradually increased.

The method needs to use a carbon-supported noble metal catalyst, the separation, the recycling and the service life of the catalyst have obvious influence on the economy of the preparation process, but the catalyst is easy to be degraded in air due to the performance of oxygen adsorption, the service life is reduced, and the use effect of the catalyst is obviously influenced by the structure of a reaction device and the coupling preparation process.

Disclosure of Invention

To this end, an embodiment of the present utility model provides a reaction apparatus for preparing biphenyl dianhydride, including: the catalyst recycling device is used for inputting a catalyst into the coupling reaction device and recycling the used catalyst;

wherein the catalyst circulation device comprises: the catalyst filter pump is connected with the coupling reaction device, one end of the catalyst filter pump is connected with the catalyst filter bed of the coupling reaction device, and the other end of the catalyst filter bed is connected with the back flush pump.

In one embodiment, the coupling reaction apparatus includes: the reaction device comprises a reaction device body, a feed inlet, an air outlet, a discharge valve and a stirrer, wherein the feed inlet is arranged on the upper portion of the reaction device body, the air inlet is arranged adjacent to the feed inlet, the air outlet is arranged on one side away from the air inlet, the discharge valve is arranged on the lower portion of the reaction device body, the stirrer is arranged inside the reaction device body, and the discharge valve is communicated with a catalyst filtering pump.

In one embodiment, the air outlet is provided with a condenser, one end of the condenser is connected with the air outlet, the bottom of the other end of the condenser is provided with a backflow channel, the backflow channel is communicated with the coupling reaction device, the top of the end of the condenser is provided with an exhaust channel, steam generated in the coupling reaction device is condensed by the condenser and then flows back by the backflow channel, and uncondensed gas is discharged through the exhaust channel at the top of the condenser.

In one embodiment, the condenser is one of a tube-in-tube condenser and a coil condenser.

In one embodiment, the gas inlet is connected to a nitrogen gas inlet device for inputting nitrogen gas into the reaction device body.

In one embodiment, the stirrer is one of a frame stirrer, an anchor stirrer and a hinge stirrer.

In one embodiment, the catalyst filter bed is one of a microporous filter and a bag filter.

In one embodiment, the catalyst filtration pump is one of a centrifugal pump and a screw pump.

In one embodiment, the backwash pump is one of a centrifugal pump, a plunger pump, and a diaphragm pump.

The embodiment of the utility model has the following advantages:

according to the utility model, the catalyst recycling device is arranged, so that the catalyst recycling is realized, the contact time of the catalyst and air is greatly reduced, the service life of the catalyst is long, the reaction device is integrally sealed, the gas exhausted after passing through the condenser is basically pollution-free, the whole process is environment-friendly, and the process safety is high.

Drawings

In order to more clearly illustrate the embodiments of the present utility model or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It will be apparent to those of ordinary skill in the art that the drawings in the following description are exemplary only and that other implementations can be obtained from the extensions of the drawings provided without inventive effort.

The structures, proportions, sizes, etc. shown in the present specification are shown only for the purposes of illustration and description, and are not intended to limit the scope of the utility model, which is defined by the claims, so that any structural modifications, changes in proportions, or adjustments of sizes, which do not affect the efficacy or the achievement of the present utility model, should fall within the ambit of the technical disclosure.

FIG. 1 is a schematic diagram of the overall connection relationship of the present utility model;

FIG. 2 is a schematic diagram of a coupling reaction apparatus according to the present utility model.

Detailed Description

Other advantages and advantages of the present utility model will become apparent to those skilled in the art from the following detailed description, which, by way of illustration, is to be read in connection with certain specific embodiments, but not all embodiments. All other examples, which are obtained by a person of ordinary skill in the art without making any inventive effort based on the examples herein, are within the scope of the present utility model, and the specific conditions are not noted in the examples, and are performed under the conventional conditions or the conditions suggested by the manufacturer. The reagents or apparatus used were conventional products available commercially without the manufacturer's attention.

Example 1

As shown in fig. 1 to 2, a reaction apparatus for preparing biphenyl dianhydride comprises: a coupling reaction device 2 for reacting the compound, a catalyst circulation device 1 communicated with the coupling reaction device 2, wherein the catalyst circulation device 1 is used for inputting the catalyst into the coupling reaction device 2 and recovering the used catalyst;

wherein the catalyst circulation apparatus 1 comprises: the catalyst circulating device 1 is arranged to realize the recycling of the catalyst, so that the contact time of the catalyst and air is greatly reduced, and the service life of the catalyst is long.

Preferably, the coupling reaction apparatus 2 includes: the reactor comprises a reaction device main body 21, a feed inlet 22, an air inlet 24, an air outlet 25, a discharge valve 23 and a stirrer 26, wherein the feed inlet 22 is arranged at the upper part of the reaction device main body 21, the air inlet 24 is arranged adjacent to the feed inlet 22, the air outlet 25 is arranged at one side far away from the air inlet 24, the discharge valve 23 is arranged at the lower part of the reaction device main body 21, the stirrer 26 is arranged in the reaction device main body 21, and the discharge valve 23 is communicated with the catalyst filtering pump 12. After the discharge valve 23 is opened, the material after complete reaction is pumped into the catalyst filter bed 11 through the catalyst filter pump 12 to separate the catalyst in the material from the required material, the material after the catalyst separation is sent to the subsequent separation and purification process, and the trapped catalyst can be pumped into the reaction device main body 21 through the back flush pump 13 from the feed inlet 22, so that the catalyst can be recycled.

Preferably, the air outlet 25 is provided with the condenser 3, one end of the condenser 3 is connected with the air outlet 25, the bottom of the other end is provided with a backflow channel, the backflow channel is communicated with the feed inlet 22 of the coupling reaction device 2, the top of the end is provided with an exhaust channel, steam generated in the coupling reaction device 2 is backflow through the backflow channel after being condensed by the condenser 3, and uncondensed gas is discharged through the exhaust channel at the top of the condenser 3, the reaction device is integrally sealed, the discharged gas after passing through the condenser 3 is basically pollution-free, and the whole process is green and environment-friendly and has high process safety.

Further preferably, the condenser 3 is one of a tube condenser and a coil condenser, and in this embodiment, a coil condenser is selected.

Further preferably, the gas inlet 24 is connected to a nitrogen gas input device (not shown) for inputting nitrogen gas into the reaction device main body 21, discharging air in the reaction device through the nitrogen gas, and the coupling reaction is performed under the protection of the nitrogen gas.

Further preferably, the stirrer 26 is one of a frame stirrer, an anchor stirrer and a hinge stirrer, and in this embodiment, the frame stirrer is used to uniformly mix the materials by stirring with the stirrer 26, and the materials are heated to the reaction temperature from the outside. Wherein the reaction temperature is 80-100 ℃.

Still further preferably, the agitator 26 may be configured to be manually driven or motor driven depending on the needs of the application.

Further preferably, the catalyst filter bed 11 is one of a microporous filter and a bag filter, and in this embodiment, a microporous filter is selected.

Further preferably, the catalyst filtration pump 12 is one of a centrifugal pump and a screw pump, and in this embodiment, a centrifugal pump is selected.

Further preferably, the backwash pump 13 is one of a centrifugal pump, a plunger pump, and a diaphragm pump, and in this embodiment, a centrifugal pump is selected.

In one embodiment, the catalyst is one of a granular active carbon supported palladium catalyst and a cylindrical active carbon supported palladium catalyst, and the solvent is one or more of deionized water, methanol, ethanol and glycerin.

The working principle of the utility model is as follows:

adding materials (chlorophthalic anhydride and sodium hydroxide) into the coupling reaction device 2 according to a certain proportion, and simultaneously pumping aqueous dispersion containing a catalyst into the coupling reaction device 2 through a back flushing pump 13; nitrogen is introduced through the nitrogen input device from the air inlet 24, the nitrogen enters through the air inlet 24, air is gradually discharged through the air outlet 25, and the coupling reaction is carried out under the protection of the nitrogen.

And then stirring the materials by a stirrer 26 to uniformly mix, heating to the reaction temperature (80-100 ℃), controlling the reaction speed by pumping flow of the catalyst, closing a catalyst feed inlet 22 after the catalyst is added, and continuing to heat the reaction for 10-20 hours to ensure that the raw materials are completely converted.

In the reaction process, steam generated in the coupling reaction device 2 enters the condenser 3 for backflow through the air outlet 25, and noncondensable gas generated in the reaction process is discharged through a top discharge port of the condenser 3.

After the reaction is finished, the discharge valve 23 is opened, the reacted material is filtered by the catalyst filter pump 12 through the catalyst filter bed 11, the catalyst is trapped in the filter bed, and the filtered product solution is sent to the subsequent separation and purification process.

The catalyst is not discharged in the reaction device, is stored in a nitrogen atmosphere, and is pumped into the coupling reactor for repeated use by a solvent and a back flushing pump 13 in the next batch reaction, and when the reaction yield is reduced to a certain value, the catalyst is replaced, and precious metal components in the replaced catalyst can be recovered for preparing a new catalyst.

While the utility model has been described in detail in the foregoing general description and specific examples, it will be apparent to those skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the utility model and are intended to be within the scope of the utility model as claimed.

Claims

1. A reaction apparatus for producing biphenyl dianhydride, comprising: the catalyst recycling device is used for inputting a catalyst into the coupling reaction device and recycling the used catalyst;

2. The reaction apparatus for producing biphenyl dianhydride according to claim 1, wherein the coupling reaction apparatus comprises: the reaction device comprises a reaction device body, a feed inlet, an air outlet, a discharge valve and a stirrer, wherein the feed inlet is arranged on the upper portion of the reaction device body, the air inlet is arranged adjacent to the feed inlet, the air outlet is arranged on one side of the reaction device body, which is far away from the air inlet, the discharge valve is arranged on the lower portion of the reaction device body, the stirrer is arranged inside the reaction device body, and the discharge valve is communicated with a catalyst filtering pump.

3. The reaction device for preparing biphenyl dianhydride according to claim 2, wherein a condenser is arranged on the air outlet, one end of the condenser is connected with the air outlet, a reflux passage is arranged at the bottom of the other end of the condenser, the reflux passage is communicated with the coupling reaction device, an exhaust passage is arranged at the top of the end of the condenser, steam generated in the coupling reaction device is condensed by the condenser and then flows back through the reflux passage, and uncondensed gas is discharged through the exhaust passage at the top of the condenser.

4. The reaction apparatus for producing biphenyl dianhydride according to claim 3, wherein the condenser is one of a tube condenser and a coil condenser.

5. The reaction apparatus for preparing biphenyl dianhydride according to claim 2, wherein the gas inlet is connected to a nitrogen gas input device for inputting nitrogen gas into the reaction apparatus main body.

6. The reaction apparatus for producing biphenyl dianhydride according to claim 2, wherein the stirrer is one of a frame stirrer, an anchor stirrer and a hinge stirrer.

7. The reaction apparatus for producing biphenyl dianhydride according to claim 1, wherein the catalyst filter bed is one of a microporous filter and a bag filter.

8. The reaction apparatus for producing biphenyl dianhydride according to claim 1, wherein the catalyst filter pump is one of a centrifugal pump and a screw pump.

9. The reaction apparatus for producing biphenyl dianhydride according to claim 1, wherein the backwash pump is one of a centrifugal pump, a plunger pump and a diaphragm pump.