CN219722837U - Reaction device for preparing biphenol - Google Patents

Reaction device for preparing biphenol Download PDF

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Publication number
CN219722837U
CN219722837U CN202320189006.2U CN202320189006U CN219722837U CN 219722837 U CN219722837 U CN 219722837U CN 202320189006 U CN202320189006 U CN 202320189006U CN 219722837 U CN219722837 U CN 219722837U
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catalyst
main body
reaction
reaction device
reactor
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梅雪
杜庶铭
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Taixing Zhongke Aide Membrane Material Technology Co ltd
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Taixing Zhongke Aide Membrane Material Technology Co ltd
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Abstract

The utility model discloses a reaction device for preparing biphenol, which comprises: the catalyst recycling device is used for inputting a catalyst into the coupling reaction device and recycling the used catalyst; the product purification device comprises: the utility model is provided with the acidification reactor, the product filtering pump and the product filter, the stability of the reaction process is enhanced, the conversion rate of raw materials is effectively improved, the catalyst recycling device is arranged, the catalyst can be recycled, 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 discharged gas after passing through the condenser is basically pollution-free, the whole process is environment-friendly, and the process safety is high.

Description

Reaction device for preparing biphenol
Technical Field
The utility model belongs to the field of fine chemical manufacturing, and particularly relates to a reaction device for preparing biphenol.
Background
4,4' -biphenol is an important fine chemical intermediate, has an anti-aging effect on aging caused by oxygen and heat, can be used as an anti-aging agent for rubber and latex, and can also be used as an additive for petroleum products; the 4,4' -biphenol has a biphenyl conjugated structure and a phenolic hydroxyl group which is easy to chemically modify, and can be used for dye intermediates, synthesis of photosensitive materials and the like.
The 4,4 '-biphenol can be used for manufacturing excellent engineering plastics and composite plastics, such as modified monomers of polyester, polyurethane, polycarbonate, polyphenylsulfone and epoxy resin, and can be used for preparing liquid crystal elements of liquid crystal polymers, and the liquid crystal polymers prepared by using the 4,4' -biphenol as a raw material have various excellent characteristics, such as high temperature resistance, high mechanical strength, excellent electrical performance and processability.
In the prior art, the method for efficiently removing the tertiary butyl by using 2, 6-tertiary butyl phenol as a raw material and using dimethylbenzene as a solvent and p-toluenesulfonic acid as a catalyst is a common method for synthesizing 4,4' -biphenol, and the total product yield of the method is about 80 percent. The method has the problems of long synthetic route, low yield and poor atom economy, so that the manufacturing cost of the 4,4' -biphenol is high, and the expansion of downstream application is limited.
In view of the above, there is a need to provide a device for synthesizing biphenol which can improve the conversion rate of the product by enhancing the stability of the reaction process and can reduce the production cost.
Disclosure of Invention
To this end, an embodiment of the present utility model provides a reaction apparatus for preparing biphenol, including: the device comprises a coupling reaction device for reacting a compound, a catalyst circulating device communicated with the coupling reaction device and a product purifying device connected with the tail end of the catalyst circulating device and used for further purifying a product, wherein the catalyst circulating device is used for inputting the catalyst into the coupling reaction device and recovering the used catalyst;
wherein, the product purification device includes: the device comprises an acidification reactor connected with a catalyst circulating device, a product filter pump arranged at the tail end of the acidification reactor and a product filter arranged at one end of the product filter pump far away from the acidification reactor.
In one embodiment, the catalyst circulation apparatus includes: 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 acidification reactor comprises: the reactor comprises a reactor main body, a feed inlet, a discharge valve and a stirrer, wherein the reactor main body is arranged in a sealing manner, the feed inlet is arranged at the upper part of the reactor main body and is communicated with a catalyst circulating device, the discharge valve is arranged at the lower part of the reactor main body, and the stirrer is arranged inside the reactor main body, wherein the discharge valve is communicated with a catalyst filtering pump.
In one embodiment, the coupling reaction apparatus includes: the reaction device comprises a reaction device main body, a feed inlet, an air outlet, a discharge valve, a stirrer and a heating device, wherein the feed inlet is arranged on the upper part of the reaction device main body, the air inlet is arranged adjacent to the feed inlet, the air outlet is arranged on one side far away from the air inlet, the discharge valve is arranged on the lower part of the reaction device main body, the stirrer is arranged inside the reaction device main body, and the heating device is arranged on the reaction device, wherein the discharge valve is communicated with a catalyst filtering pump.
In one embodiment, the heating device comprises: the device comprises a heater arranged at the bottom of a reaction device main body, a temperature sensor arranged on the outer wall of the reaction device main body and a processor respectively connected with the heater and the temperature sensor.
In one embodiment, a condenser is arranged on the air outlet, one end of the condenser is connected with the air outlet, a reflux channel is arranged at the bottom of the other end of the condenser, the reflux channel is communicated with the coupling reaction device, an exhaust channel 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 by the reflux 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.
The embodiment of the utility model has the following advantages:
the utility model enhances the stability of the reaction process by arranging the systematic arrangement, effectively improves the conversion rate of raw materials, realizes the recycling of the catalyst by arranging the catalyst circulating device, greatly reduces the contact time of the catalyst and air, ensures the service life of the catalyst, ensures that the whole reaction device is sealed, basically causes no pollution to the gas discharged after passing through the condenser, and has the advantages of environment-friendly whole process and high process safety.
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;
FIG. 3 is a schematic diagram of the structure of the acidification reactor of the 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 3, a reaction apparatus for preparing biphenol, comprising: 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 product purification device 3 comprises: an acidification reactor 31 connected with the catalyst circulation device 2, a product filter pump 32 arranged at the end of the acidification reactor 31 and a product filter 33 arranged at the end of the product filter pump 32 away from the acidification reactor.
Further preferably, the acidification reactor 31 comprises: a reactor main body 311 which is arranged in a sealing manner, a reactor feed inlet 312 which is arranged at the upper part of the reactor main body 311 and is communicated with the catalyst circulating device 2, a reactor discharge valve 313 which is arranged at the lower part of the reactor main body 311, and a stirrer 314 which is arranged inside the reactor main body 311, wherein the reactor discharge valve 313 is communicated with the catalyst filtering pump 12.
Preferably, the coupling reaction apparatus 2 includes: the reactor comprises a reactor main body 21 arranged in a sealing manner, a reactor feed inlet 22 arranged at the upper part of the reactor main body 21, a reactor air inlet 24 arranged adjacent to the reactor feed inlet 22, a reactor air outlet 25 arranged at one side far away from the reactor air inlet 24, a reactor discharge valve 23 arranged at the lower part of the reactor main body 21, and a reactor stirrer 26 arranged in the reactor main body 21, wherein the reactor discharge valve 23 is communicated with the catalyst filter pump 12. After the discharge valve 23 of the reaction device is opened, the materials after complete reaction are pumped into the catalyst filter bed 11 through the catalyst filter pump 12 to separate the catalyst in the materials from the required materials, the materials after the catalyst separation are sent to the acidification reactor 31, and the trapped catalyst can be pumped into the reaction device main body 21 from the feed inlet 22 of the reaction device through the back flushing pump 13, so that the contact time of the catalyst and air is greatly reduced, the catalyst can be recycled, the service life of the catalyst is long, and the process is green and environment-friendly.
Preferably, the air outlet 25 of the reaction device is provided with a condenser 27, one end of the condenser 27 is connected with the air outlet 25 of the reaction device, the bottom of the other end is provided with a backflow channel (not shown), the backflow channel is communicated with the feed inlet 22 of the reaction device 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 condensed by the condenser 27 and then flows back by the backflow channel, the uncondensed gas is discharged by the exhaust channel at the top of the condenser 27, the reaction device is integrally sealed, the discharged gas after passing through the condenser 27 is basically pollution-free, the whole process is environment-friendly, and the process safety is high.
Further preferably, a heating device 4 for maintaining the reaction temperature of the reaction device body 21 throughout the reaction process is further provided at the bottom of the reaction device body 21, and the etherification reaction heating device 4 includes: a heater 41 provided at the bottom of the reactor body 21, a temperature sensor 42 provided at the outer wall of the reactor body 21, and a processor 43 connected to the heater 41 and the temperature sensor 42, respectively. The temperature sensor 42 monitors the temperature of the reaction apparatus main body 21 in the operating state, and returns the temperature data to the controller 43, and if the temperature is lower than the minimum threshold value set initially, a signal is sent to the heater 41 to start the heater 41 to operate, so as to perform temperature compensation, until the temperature sensor 42 monitors that the temperature in the reaction is higher than the minimum threshold value set initially, the controller 43 controls the heater 41 to stop heating.
The device is integrally and systematically arranged, the automation degree of operation is improved on the basis of the prior art, the stability of the reaction process is enhanced, the conversion rate of raw materials is effectively improved, and the conversion rate of the raw materials of the device is high and can reach more than 99 percent.
Further preferably, the condenser 27 is one of a tube condenser and a coil condenser, and in this embodiment, a coil condenser is selected.
Further preferably, the reaction device 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 reaction device stirrer 26 is one of a frame stirrer, an anchor stirrer and a hinge stirrer, and in this embodiment, the frame stirrer is selected, and the materials are uniformly mixed by stirring the reaction device stirrer 26, and are heated to the reaction temperature from the outside. Wherein the reaction temperature is 80-100 ℃.
Still further preferably, the reactor stirrer 26 may be configured to be manually driven or motor driven depending on the needs of the use.
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.
Further preferably, the stirring paddle of the coupling reaction device is one of a frame type stirring paddle, an anchor type stirring paddle and a hinge type stirring paddle.
Further preferably, the stirring paddle of the acidification reactor is one of a frame stirring paddle and an anchor stirring paddle.
Further preferably, the product filter pump is one of a centrifugal pump and a screw pump.
Further preferably, the product filter is one of a centrifuge and a plate-and-frame filter press.
In one embodiment, the catalyst is one of granular active carbon supported palladium catalyst and cylindrical active carbon supported palladium catalyst, and the solvent is one or more of deionized water, methanol, ethanol and glycerin.
The working flow of the utility model is as follows:
(1) Adding parachlorophenol and sodium hydroxide into a coupling reaction device 2 according to a certain proportion, and pumping a solvent containing a catalyst;
(2) Introducing nitrogen to discharge air in the reaction system;
(3) Heating the materials in the coupling reaction device 2 to 80-100 ℃, gradually pumping sodium formate aqueous solution in a certain proportion within 1-2h, continuing to react for 10-20h, refluxing steam generated in the kettle through a condenser 27, and discharging non-condensable gas through a top discharge port of the condenser 27;
(4) After the coupling reaction is finished, a discharge valve 23 of the reaction device is opened, the reacted material is filtered by a catalyst filter bed 11 through a catalyst filter pump 12, the catalyst is trapped in the filter bed, and the filtered solution is sent to an acidification reactor 31;
(5) In the next batch of reaction, the catalyst in the catalyst filter bed 11 is pumped into the coupling reaction device 2 for repeated use by a solvent through a back flushing pump 13, the catalyst can be repeatedly used for a plurality of times, and when the reaction yield is reduced to a certain value, the catalyst is replaced;
(6) Adding inorganic acid into the acidification reactor 31, and stirring at normal temperature for reaction;
(7) After the acidification reaction is finished, the material is pumped into a product filter 33 by a product filter pump 32 for filtration, and the product is obtained.
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 from the reaction device air inlet 24 through the nitrogen input device, the nitrogen enters from the reaction device air inlet 24, air is gradually discharged from the reaction device air outlet 25, and the coupling reaction is carried out under the protection of the nitrogen.
And then stirring the materials uniformly by a reaction device stirrer 26, heating to the reaction temperature (80-100 ℃), controlling the reaction speed by the pumping flow of the catalyst, closing a feed inlet 22 of the catalyst reaction device after the catalyst is added, and continuously heating and reacting 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 27 through the air outlet 25 of the reaction device to flow back, and noncondensable gas generated in the reaction process is discharged through the top discharge port of the condenser 27.
After the reaction is finished, a discharge valve 23 of the reaction device is opened, the reacted material is filtered by a catalyst filter pump 12 through a catalyst filter bed 11, the catalyst is trapped in the filter bed, and the filtered product solution is sent to an acidification reactor.
The catalyst is not discharged in the reaction device, is stored in a nitrogen atmosphere, and is pumped into the coupling reaction device 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 (10)

1. A reaction apparatus for producing biphenol, comprising: the device comprises a coupling reaction device for reacting a compound, a catalyst circulating device communicated with the coupling reaction device, and a product purifying device connected with the tail end of the catalyst circulating device and used for further purifying a product, wherein the catalyst circulating device is used for inputting a catalyst into the coupling reaction device and recovering the used catalyst;
wherein, the product purification device includes: the device comprises an acidification reactor connected with the catalyst circulating device, a product filtering pump arranged at the tail end of the acidification reactor and a product filter arranged at one end of the product filtering pump far away from the acidification reactor.
2. The reaction apparatus for producing biphenol according to claim 1, wherein the catalyst circulation apparatus 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.
3. The reaction apparatus for producing biphenol according to claim 2, wherein the acidification reactor comprises: the reactor comprises a reactor main body, a feed inlet, a discharge valve and a stirrer, wherein the reactor main body is arranged in a sealing mode, the feed inlet is arranged on the upper portion of the reactor main body and communicated with the catalyst circulating device, the discharge valve is arranged on the lower portion of the reactor main body, the stirrer is arranged inside the reactor main body, and the discharge valve is communicated with the catalyst filtering pump.
4. The reaction apparatus for producing biphenol according to claim 2, wherein the coupling reaction apparatus comprises: the reaction device comprises a reaction device main body, a feed inlet, an air outlet, a discharge valve, a stirrer and a heating device, wherein the feed inlet is arranged on the upper portion of the reaction device main 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 main body, the stirrer is arranged inside the reaction device main body, and the heating device is arranged on the reaction device, and the discharge valve is communicated with a catalyst filtering pump.
5. The reaction apparatus for producing biphenol according to claim 4, wherein the heating means comprises: the device comprises a heater arranged at the bottom of a reaction device main body, a temperature sensor arranged on the outer wall of the reaction device main body and a processor respectively connected with the heater and the temperature sensor.
6. The reaction apparatus for preparing biphenol according to claim 4, wherein a condenser is provided on the air outlet, one end of the condenser is connected to the air outlet, a reflux passage is provided at the bottom of the other end, the reflux passage is communicated with the coupling reaction apparatus, an exhaust passage is provided at the top of the end, steam generated in the coupling reaction apparatus is condensed by the condenser and then refluxed by the reflux passage, and the gas which is not condensed is exhausted through the exhaust passage at the top of the condenser.
7. The reaction apparatus for producing biphenol according to claim 6, wherein the condenser is one of a tube condenser and a coil condenser.
8. The reaction apparatus for producing biphenol according to claim 4, wherein the inlet port is connected to a nitrogen gas input means for inputting nitrogen gas into the reaction apparatus main body.
9. The reaction apparatus for producing biphenol according to claim 4, wherein the stirrer is one of a frame stirrer, an anchor stirrer and a hinge stirrer.
10. The reaction apparatus for producing biphenol according to claim 2, wherein the catalyst filter bed is one of a microporous filter and a bag filter.
CN202320189006.2U 2023-02-10 2023-02-10 Reaction device for preparing biphenol Active CN219722837U (en)

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Application Number Priority Date Filing Date Title
CN202320189006.2U CN219722837U (en) 2023-02-10 2023-02-10 Reaction device for preparing biphenol

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202320189006.2U CN219722837U (en) 2023-02-10 2023-02-10 Reaction device for preparing biphenol

Publications (1)

Publication Number Publication Date
CN219722837U true CN219722837U (en) 2023-09-22

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