CN111408320A - Synthesis device and application thereof, and method for producing thermotropic liquid crystal polymer - Google Patents
Synthesis device and application thereof, and method for producing thermotropic liquid crystal polymer Download PDFInfo
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- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
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- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
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- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/60—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from the reaction of a mixture of hydroxy carboxylic acids, polycarboxylic acids and polyhydroxy compounds
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
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- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
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Abstract
The present invention provides a synthesis apparatus and use thereof and a method for producing a thermotropic liquid crystalline polymer; the synthesis device comprises a reaction kettle (1), a condenser (2) and a liquid storage tank (3); the reaction kettle (1) is communicated with a liquid inlet of the condenser (2) through a first pipeline; the liquid storage tank 3 is communicated with a liquid outlet of the condenser (2) through a second pipeline; a stirrer (11), a sprayer (12) and a temperature sensor are arranged in the reaction kettle (1); the liquid storage tank (3) is communicated with the sprayer (12) through a third pipeline; a metering pump (4) and a first temperature control switch (5) are arranged on the third pipeline; the first temperature control switch (5) is in electrical signal connection with the temperature sensor. The reaction device in the application has a compact structure, can realize the accurate control of the temperature of reaction materials in the reaction kettle, and is very suitable for producing thermotropic liquid crystal polymers.
Description
Technical Field
The invention relates to the field of synthesis of liquid crystal polyester, in particular to a synthesis method and a synthesis device of liquid crystal polyester.
Background
Thermotropic liquid crystal polymer (T L CP) as an engineering plastic with special performance has a series of excellent performances, such as high strength, high modulus, short molding period, heat and chemical resistance, small linear expansion coefficient, low hygroscopicity, low dielectric constant, excellent electric insulation and the like, so that the thermotropic liquid crystal polymer has wide application in the fields of electronic appliances, fiber optical fibers, flexible circuit boards, 5G mobile phone antennas and the like at present.
The melt-process synthesis of thermotropic liquid crystalline polyesters generally comprises the following steps: (1) performing acetylation reaction on the mixed monomers in the reaction kettle; (2) after the acetylation is finished, raising the temperature to carry out polycondensation reaction, and distilling off acetic acid and excessive acetic anhydride; (3) when the reaction system has a certain viscosity, the polymer is discharged from the bottom of the kettle in a strip shape.
The whole reaction process is accompanied with strong heat absorption and release phenomena, which can cause the temperature change of a reaction system in the kettle to be larger, deviate from the set temperature and even generate temperature runaway phenomena. In addition, the excessive temperature causes sublimation and crystallization of reaction monomers, and the reaction monomers are separated out and adhered to the wall of the kettle and the stirring paddle, so that the determined monomer molar ratio is influenced, and the performance of the liquid crystal polymer is finally influenced.
Therefore, how to inhibit the temperature runaway phenomenon and avoid the influence of monomer sublimation crystallization on the molar ratio is a key process for preparing the high-performance liquid crystal polyester.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the present invention aims to provide a synthesis apparatus, its use and a method for producing thermotropic liquid crystalline polymers, which are used to solve the problems of the prior art that the temperature of materials is too high during the reaction of liquid crystalline polymers, and the sublimation of monomers affects the precise molar ratio of the reactants and thus the final properties of the liquid crystalline polymers.
To achieve the above objects and other related objects, the present invention is achieved by the following technical solutions.
The invention provides a synthesis device, which comprises a reaction kettle, a condenser and a liquid storage tank, wherein the reaction kettle is connected with the condenser; the reaction kettle is communicated with a liquid inlet of the condenser through a first pipeline; the liquid storage tank is communicated with a liquid outlet of the condenser through a second pipeline; a stirrer, a sprayer and a temperature sensor are arranged in the reaction kettle; the liquid storage tank is communicated with the sprayer through a third pipeline; a metering pump and a first temperature control switch are arranged on the third pipeline; the first temperature control switch is in electrical signal connection with the temperature sensor.
According to the above synthesis device, the condenser is arranged at the upper part of the reaction kettle.
According to the synthesizer, the outer side wall of the reaction kettle is further wound with a plurality of heat exchange interlayers, and circulating heat conduction oil is arranged in the heat exchange interlayers.
According to the synthesis device, the heat exchange interlayer is also provided with a cooling assembly; the cooling assembly includes a cooling tube that spirals around the reactor.
According to the synthesis device, one or more heat exchange interlayers are provided. More preferably, a plurality of heat exchange interlayers are distributed along the height direction of the reaction kettle in sequence.
According to the synthesis device, the heat exchange interlayer is also internally provided with an ultrasonic generator.
According to the synthesis device, the average molecular weight of the heat conduction oil is 200-400; the kinematic viscosity at 40 ℃ is 25-32 mm2(s) kinematic viscosity at 100 ℃ of 2 to 5mm2/s。
According to the synthesizer, the cooling pipe is provided with a second temperature control switch, and the second temperature control switch is in electrical signal connection with the temperature sensor.
According to the synthesis device, the temperature sensor is arranged in the middle or at the bottom of the reaction kettle; and/or the sprayer is arranged at the top of the reaction kettle; and/or the side surface of the reaction kettle is also provided with an inner window.
According to the synthesis device, along the flowing direction of liquid on the third pipeline, the third pipeline is divided into a manual switch communication channel and an automatic switch communication channel after passing through the first temperature control switch.
The invention also discloses the application of the synthesis device for producing the thermotropic liquid crystal polymer.
The invention also discloses a method for producing the thermotropic liquid crystal polymer, which comprises the following steps: 1) adding a monomer into a reaction kettle, dissolving the monomer with a solvent, adding a certain amount of catalyst, and heating until the temperature of reaction materials reaches 80-150 ℃ and keeping the temperature for acetylation; 2) after the acetylation reaction is finished, heating the reaction materials in the reaction kettle to 200-350 ℃ and keeping the temperature for polymerization deacidification reaction; and in the steps 1) and 2), the produced fraction is extracted and condensed, and then is refluxed and sprayed back to the reaction kettle and/or the temperature is regulated and controlled by a heat exchange interlayer arranged on the wall of the reaction kettle, so that the temperature is kept at 80-150 ℃ or 200-350 ℃.
According to the method, the monomer is one or more of p-hydroxybenzoic acid, 6-hydroxy-2-naphthoic acid, hydroquinone, biphenol, p-hydroxyamine and derivatives thereof; the catalyst is acetate of any one or more of calcium, iron, zinc and selenium.
According to the method, the condensed fraction is automatically controlled to flow back and spray back to the reaction kettle or the temperature of the heat exchange interlayer is automatically controlled through the temperature switch and the temperature sensor arranged in the reaction kettle.
According to the method, the condition of a reaction system in the reaction kettle is observed through the inner window arranged on the reaction kettle, and when white monomers are sublimated and adhered to the kettle wall in the reaction kettle, the distillate after condensation is manually controlled to flow back and spray back to the reaction kettle or the temperature of the heat exchange interlayer is controlled.
According to the method described above, it employs a synthesis apparatus as described above in the present application.
The invention has the beneficial effects that:
reaction unit compact structure in this application can realize the accurate control of reation kettle interior reaction material temperature. Specifically, through the design of spray set and heat transfer intermediate layer in this application, effectively restrained acetylation in-process monomer and appeared the phenomenon, solved simultaneously that high temperature polymerization in-process system is exothermic in a large number, lead to the emergence that the interior actual temperature of cauldron drifted away the settlement temperature, ensure that the reaction is mild controllable, be particularly suitable for producing thermotropic liquid crystal polymer.
Drawings
FIG. 1 is a schematic diagram of the synthesis apparatus of the present invention.
Description of the drawings in FIG. 1
| 1 | |
| 11 | Stirrer |
| 12 | |
| 13 | |
| 14 | |
| 2 | Condenser |
| 3 | |
| 4 | |
| 5 | First temperature control switch |
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
It is to be understood that the processing equipment or apparatus not specifically identified in the following examples is conventional in the art.
Furthermore, it is to be understood that one or more method steps mentioned in the present invention does not exclude that other method steps may also be present before or after the combined steps or that other method steps may also be inserted between these explicitly mentioned steps, unless otherwise indicated; it is also to be understood that a combined connection between one or more devices/apparatus as referred to in the present application does not exclude that further devices/apparatus may be present before or after the combined device/apparatus or that further devices/apparatus may be interposed between two devices/apparatus explicitly referred to, unless otherwise indicated. Moreover, unless otherwise indicated, the numbering of the various method steps is merely a convenient tool for identifying the various method steps, and is not intended to limit the order in which the method steps are arranged or the scope of the invention in which the invention may be practiced, and changes or modifications in the relative relationship may be made without substantially changing the technical content.
Example 1
As shown in fig. 1, the embodiment of the present application provides a liquid crystal polyester synthesizing apparatus, which includes a reaction kettle 1, a condenser 2 and a liquid storage tank 3;
the reaction kettle 1 is communicated with a liquid inlet of the condenser 2 through a first pipeline;
the liquid storage tank 3 is communicated with a liquid outlet of the condenser 2 through a second pipeline;
a stirrer 11, a sprayer 12 and a temperature sensor are arranged in the reaction kettle 1; the liquid storage tank 3 is communicated with the sprayer 12 through a third pipeline;
a metering pump 4 and a first temperature control switch 5 are arranged on the third pipeline; the first temperature control switch 5 is in electrical signal connection with the temperature sensor.
Reaction unit reactant heats to the uniform temperature in reation kettle and keeps and react in this application, and the fraction of production gets into in condenser 2 condensation back gets into liquid storage pot 3 through the second pipeline through first pipeline, then sprays to reation kettle 1 in through third pipeline to sprayer 12.
The liquid storage tank is stored with a spraying solvent.
In the embodiment shown in fig. 1, the condenser 2 is disposed at an upper portion of the reaction vessel 1.
In the specific embodiment shown in fig. 1, a plurality of heat exchange interlayers 13 are further wound on the outer side wall of the reaction kettle 1, and circulating heat conduction oil is arranged in the heat exchange interlayers 13.
The average molecular weight of the heat conduction oil adopted in the application is 200-400; the kinematic viscosity at 40 ℃ is 25-32 mm2(s) kinematic viscosity at 100 ℃ of 2 to 5mm2And s. In the case of producing liquid crystal polyester by using the apparatus as in the example of the present application, modified terphenyl may be used as the heat transfer oil.
In the specific embodiment shown in fig. 1, the heat exchange interlayer 13 is further provided with a cooling assembly 14; the cooling assembly 14 comprises cooling tubes that spiral around the reactor vessel 1. The cooling pipe is a metal pipe.
The number of the heat exchange interlayers 13 is one or more in the present application. In the specific embodiment shown in fig. 1, there is one heat exchange interlayer 13, and one heat exchange interlayer wraps the entire outer side wall of the reaction vessel 1. In another specific embodiment, in order to better control the temperature of each section in the reaction kettle 1, for example, in the synthesis process of thermotropic liquid crystal polyester, in order to avoid monomer and solvent sublimation, too much of the monomer and solvent enter the condenser, the temperature of the upper end in the reaction kettle 1 is properly lower than that of the bottom end, therefore, a plurality of heat exchange interlayers 13 are sequentially distributed on the outer side wall of the reaction kettle 1 from top to bottom, and the temperature of each heat exchange interlayer is controlled to realize the sectional distribution of the temperature in the reaction kettle 1.
In the particular embodiment shown in fig. 1, the cooling module 14 is a cooling water module.
In a specific embodiment, an ultrasonic generator is further disposed in the heat exchange interlayer 13. The heat transfer effect in the reaction process is improved through the oscillation effect of the ultrasonic generator.
In the specific embodiment shown in fig. 1, a second temperature-controlled switch 6 is disposed on the cooling pipe, and the second temperature-controlled switch 6 is electrically connected to the temperature sensor 13. When the temperature of the materials in the reaction kettle is floated from a certain temperature, cooling water is introduced through the cooling pipe to take away the heat of the heat-conducting oil.
In the specific embodiment shown in fig. 1, the temperature sensor is disposed in the middle or at the bottom of the reaction vessel 1. In a more specific embodiment, the temperature sensor 13 is provided at the bottom of the temperature sensor 13. The temperature of the reaction system in the reaction vessel 1 was measured by using the temperature sensor 13. In a more specific embodiment, the gas outlet of the reaction vessel 1 is also provided with a temperature sensor for detecting the temperature of the outlet gas in the reaction vessel.
In the specific embodiment shown in fig. 1, the sparger 12 is provided at the top of the reaction vessel 1. The number of the sprayers 12 is 1 or more. In the specific embodiment shown in fig. 1, the number of the sprayers 12 is 2, and two sprayers are distributed at intervals to ensure that the sprayed solvent can cover the whole space in the reaction kettle 1.
In a more specific embodiment, along the flowing direction of the liquid on the third pipeline, the third pipeline is divided into a manual switch communication channel and an automatic switch communication channel after passing through the first temperature control switch. After the first temperature control switch is manually opened, liquid enters the sprayer 12 from the manual switch communicating channel and is sprayed into the reaction kettle 1, and after the first temperature control switch is automatically opened, liquid enters the sprayer 12 from the automatic switch communicating channel and is sprayed into the reaction kettle 1.
In a specific embodiment, the side of the reaction kettle 1 is further provided with an inner window.
The method for producing a thermotropic liquid crystalline polymer in the present application comprises the steps of: 1) adding a monomer into a reaction kettle, dissolving the monomer with a solvent, adding a certain amount of catalyst, and heating until the temperature of reaction materials reaches 80-150 ℃ and keeping the temperature for acetylation; 2) after the acetylation reaction is finished, heating the reaction materials in the reaction kettle to 200-350 ℃ and keeping the temperature for polymerization deacidification reaction; and in the steps 1) and 2), the produced fraction is extracted and condensed, and then is refluxed and sprayed back to the reaction kettle and/or the temperature is regulated and controlled by a heat exchange interlayer arranged on the wall of the reaction kettle, so that the temperature is kept at 80-150 ℃ or 200-350 ℃.
Preferably, the monomer is one or more selected from p-hydroxybenzoic acid, 6-hydroxy-2-naphthoic acid, hydroquinone, biphenol, p-hydroxyamine and derivatives thereof; the catalyst is acetate of any one or more of calcium, iron, zinc and selenium.
According to the method, the condensed fraction can be automatically controlled to flow back and spray back to the reaction kettle or the temperature of the heat exchange interlayer can be automatically controlled through the temperature switch and the temperature sensor arranged in the reaction kettle.
According to the method, the condition of a reaction system in the reaction kettle can be observed through an inner window arranged on the reaction kettle, and when white monomers are sublimated and adhered to the kettle wall in the reaction kettle, the condensed fraction is manually controlled to flow back and spray back to the reaction kettle or the temperature of the heat exchange interlayer is controlled.
In a further alternative embodiment, the method employs a synthesis apparatus as described herein above.
The production process of thermotropic liquid crystalline polymers using the synthesis apparatus as described above in this application is as follows:
the monomers were added to reaction vessel 1 and dissolved in a solvent while a certain amount of catalyst was added. Wherein the monomer is one or more selected from p-hydroxybenzoic acid, 6-hydroxy-2-naphthoic acid, hydroquinone, biphenol, p-hydroxyamine and derivatives thereof; the catalyst is acetate of any one or more of calcium, iron, zinc and selenium. And (3) heating the reaction materials in the reaction kettle 1 to 80-150 ℃ by adopting heat conduction oil of internal circulation in the heat exchange interlayer 14 to perform acetylation reaction. In the acetylation process, the acetylation process is observed through an inner view window, if the white monomer in the reaction kettle is sublimated and adhered to the kettle wall, the first temperature control switch 5 is manually opened at the moment, the liquid in the liquid storage tank 3 enters the manual switch communication channel through the metering pump 4 and is reserved to the sprayer 12, the sprayed solvent washes the monomer back into the reaction kettle 1 to continue to react, and the accuracy of monomer formula design is guaranteed.
After the acetylation is finished, the temperature of a reaction system in the reaction kettle 1 is raised to 200-350 ℃ for polymerization deacidification reaction, and distilled acetic acid is condensed and refluxed to a liquid storage tank 3 through a condenser 2. Along with the continuous distillation of acetic acid, the concentration of monomers in the system is gradually increased, the polymerization reaction is accelerated, the heat release is severe, the temperature in the reaction kettle 1 is quickly raised, and the accurate temperature control of the reaction system is difficult to realize by simply controlling the temperature of the oil bath. When the temperature of the reaction system detected by the temperature sensor 13 is higher than a set value, the temperature control switch receives a signal and automatically turns on the switch, so that the acetic acid solvent which is stored in the liquid storage tank 3 and cooled by the condenser 2 is sprayed into the reaction kettle 1 through the third pipeline and the sprayer 12 to reduce the reaction temperature; meanwhile, the second temperature control switch on the cooling assembly 15 is turned on after receiving the signal from the temperature sensor 13, and the cooling assembly is enabled to work, so that cooling water is introduced into the cooling pipe, and heat transfer oil is subjected to heat exchange and temperature reduction. In the production of the liquid crystal polyester as described above in the present application, the heat transfer oil is modified terphenyl, and the spraying solvent is preferably acetic acid or acetic anhydride.
Example 2
1657.4g of p-hydroxybenzoic acid, 752.72g of 2-hydroxy-6-naphthoic acid, 220.2g of hydroquinone, 332.2g of terephthalic acid, 8.4g of potassium acetate (polymerization catalyst), 11g of p-toluenesulfonic acid (acetylation catalyst), and 2500g of acetic anhydride were charged into a reaction vessel.
The reactants are mixed and stirred evenly, and then acetylation reaction is carried out for 2.5h under nitrogen atmosphere and reflux at 155 ℃. When the monomer is sublimated and separated out on the kettle wall, cooling water is introduced into the cooling assembly for oil bath cooling, and meanwhile, the sprayer sprays solvent to wash the monomer back into the reaction kettle for continuous reaction. The temperature was then raised further to 350 ℃ over 5h, during which the polymerization was gradually allowed to proceed mildly by controlling the reaction temperature rise rate by means of cooling water flux in the cooling tube and a shower. The viscosity of the reaction system is increased along with the gradual distillation of acetic acid and excessive acetic anhydride, when the system begins to generate a rod climbing or wire drawing phenomenon, the reaction is stopped, and reactants are discharged and granulated from the bottom of the polymerization container in a multi-strand strip shape.
The detection proves that the product has light color, uniform quality, high strength and a melting point of 307.5 ℃.
Comparative example
1657.4g of p-hydroxybenzoic acid, 752.72g of 2-hydroxy-6-naphthoic acid, 220.2g of hydroquinone, 332.2g of terephthalic acid, 8.4g of potassium acetate (polymerization catalyst), 11g of p-toluenesulfonic acid (acetylation catalyst), and 2500g of acetic anhydride were charged into a reaction vessel.
After the reactants are mixed and stirred uniformly, acetylation reaction is carried out for 2.5 hours under the nitrogen atmosphere and at the temperature of 155 ℃, a cooling pipe is not adopted to cool the heat conducting oil or a sprayer is not adopted to spray a solvent, a large amount of crystals are separated out on the wall of the kettle at the moment, and even part of the crystals enter a condenser, so that the mole ratio design of the monomers is directly influenced.
The temperature is increased to 350 ℃ within 5h, in the process, a cooling pipe is not adopted to cool the heat conducting oil or a sprayer is not adopted to spray a solvent, the temperature rising rate of the reaction system is increased along with the increase of the polymerization degree, so that the system generates a large amount of smoke small particles, and low polymer small molecules are sublimated. The reaction is stopped, reactants are taken out from the bottom of the polymerization container, the product is locally carbonized due to overhigh temperature, and a large amount of unreacted monomers are attached to the wall of the kettle or even a condenser, so that the molar ratio of the monomers is extremely unbalanced, and the product quality is seriously influenced. In addition, the polymer had a melting point of 267.65 ℃ and a low strength, indicating a low molecular weight.
Through embodiment 1 and comparative example 1, the design that a sprayer and a reaction kettle heat exchange interlayer are added to a reaction kettle effectively inhibits the monomer precipitation in the acetylation process, and simultaneously solves the problems of material temperature runaway and even carbonization in the high-temperature polymerization process. The preparation method is simple, the polymerization reaction is mild, mild and controllable, and the method is suitable for producing high-performance liquid crystal polymers.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. A synthesis device is characterized by comprising a reaction kettle (1), a condenser (2) and a liquid storage tank (3); the reaction kettle (1) is communicated with a liquid inlet of the condenser (2) through a first pipeline; the liquid storage tank (3) is communicated with a liquid outlet of the condenser (2) through a second pipeline; a stirrer (11), a sprayer (12) and a temperature sensor are arranged in the reaction kettle (1); the liquid storage tank (3) is communicated with the sprayer (12) through a third pipeline; a metering pump (4) and a first temperature control switch (5) are arranged on the third pipeline; the first temperature control switch (5) is in electrical signal connection with the temperature sensor.
2. The synthesis device according to claim 1, characterized in that the condenser (2) is arranged at the upper part of the reaction vessel (1); and/or the outer side wall of the reaction kettle (1) is also provided with a plurality of heat exchange interlayers (13) in a winding manner, and circulating heat conduction oil is arranged in the heat exchange interlayers (13).
3. A synthesis unit according to claim 2, characterized in that the heat exchange sandwich (13) is further provided with a cooling module (14); the cooling assembly (14) comprises a cooling tube that spirals around the reactor vessel (1); and/or the heat exchange interlayer(s) (13) is/are one or more; and/or an ultrasonic generator is also arranged in the heat exchange interlayer (13); and/or the average molecular weight of the heat conduction oil is 200-400; the kinematic viscosity at 40 ℃ is 25-32 mm2(s) kinematic viscosity at 100 ℃ of 2 to 5mm2/s。
4. The synthesizer according to claim 3, wherein a second temperature control switch is disposed on the cooling tube, and the second temperature control switch is electrically connected to the temperature sensor; and/or a plurality of heat exchange interlayers (13) are distributed in sequence along the height direction of the reaction kettle (1).
5. The synthesis device according to claim 1, characterized in that the temperature sensor is arranged in the middle or at the bottom of the reaction kettle (1); and/or the sprayer (12) is arranged at the top of the reaction kettle (1); and/or the side surface of the reaction kettle (1) is also provided with an inner window; and/or along the flowing direction of liquid on the third pipeline, the third pipeline is divided into a manual switch communicating channel and an automatic switch communicating channel after passing through the first temperature control switch (5).
6. Use of a synthesis device according to any one of claims 1 to 5 for the production of thermotropic liquid crystalline polymers.
7. A method for producing a thermotropic liquid crystalline polymer, comprising the steps of: 1) adding a monomer into a reaction kettle, dissolving the monomer with a solvent, adding a certain amount of catalyst, and heating until the temperature of reaction materials reaches 80-150 ℃ and keeping the temperature for acetylation; 2) after the acetylation reaction is finished, heating the reaction materials in the reaction kettle to reach and keep the temperature at 200-350 ℃ for polymerization deacidification reaction; and in the steps 1) and 2), the produced fraction is extracted and condensed, and then is refluxed and sprayed back to the reaction kettle and/or the temperature is regulated and controlled by a heat exchange interlayer arranged on the wall of the reaction kettle, so that the temperature is kept at 80-150 ℃ or 200-350 ℃.
8. The method of claim 7, wherein the monomer is one or more selected from the group consisting of p-hydroxybenzoic acid, 6-hydroxy-2-naphthoic acid, hydroquinone, biphenol, p-hydroxyaniline and derivatives thereof; the catalyst is acetate of any one or more of calcium, iron, zinc and selenium.
9. The method of claim 7, wherein the condensed distillate is automatically controlled to flow back and spray to the reaction kettle or the temperature of the heat exchange interlayer is automatically controlled by a temperature switch and a temperature sensor arranged in the reaction kettle; and/or observing the condition of a reaction system in the reaction kettle through an inner window arranged on the reaction kettle, and manually controlling the temperature of the condensed fraction reflux spray back to the reaction kettle or the heat exchange interlayer when white monomers are sublimated and adhered to the kettle wall in the reaction kettle.
10. A method according to any one of claims 7 to 9, wherein a synthesis apparatus according to any one of claims 1 to 5 is used.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010388189.1A CN111408320A (en) | 2020-05-09 | 2020-05-09 | Synthesis device and application thereof, and method for producing thermotropic liquid crystal polymer |
Applications Claiming Priority (1)
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| CN202010388189.1A CN111408320A (en) | 2020-05-09 | 2020-05-09 | Synthesis device and application thereof, and method for producing thermotropic liquid crystal polymer |
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| CN112191198A (en) * | 2020-11-11 | 2021-01-08 | 北京水木滨华科技有限公司 | Isobutylene oxyacetylation reaction device and method |
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