CN113072734A - Thermotropic liquid crystal polymer microporous foam material and preparation method thereof - Google Patents
Thermotropic liquid crystal polymer microporous foam material and preparation method thereof Download PDFInfo
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- CN113072734A CN113072734A CN202110287188.2A CN202110287188A CN113072734A CN 113072734 A CN113072734 A CN 113072734A CN 202110287188 A CN202110287188 A CN 202110287188A CN 113072734 A CN113072734 A CN 113072734A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/122—Hydrogen, oxygen, CO2, nitrogen or noble gases
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/06—CO2, N2 or noble gases
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/08—Supercritical fluid
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2300/00—Characterised by the use of unspecified polymers
- C08J2300/12—Polymers characterised by physical features, e.g. anisotropy, viscosity or electrical conductivity
Abstract
The invention provides a thermotropic liquid crystal polymer microporous foam material and a preparation method thereof, wherein the preparation method comprises the following steps: placing a thermotropic liquid crystal polymer in a reaction kettle, introducing a supercritical fluid foaming agent, keeping high temperature and high pressure in the reaction kettle, and then quickly reducing the pressure; or, the thermotropic liquid crystal polymer is placed in a reaction kettle, then a supercritical fluid foaming agent is introduced, the high temperature and the high pressure in the reaction kettle are kept, then the pressure is slowly released, and then the foaming is carried out at the temperature of 180-330 ℃; or placing the thermotropic liquid crystal polymer in a reaction kettle, introducing a supercritical fluid foaming agent, keeping the high temperature and the high pressure in the reaction kettle, slowly releasing the pressure, and foaming in a mold of a vulcanizing machine; according to the preparation method, the supercritical fluid is used as the foaming agent, the thermotropic liquid crystal polymer microporous foam can be prepared at a lower temperature, the foaming temperature is generally between the glass transition temperature and the melting point of the thermotropic liquid crystal polymer, and the microporous foam material with high cell density, small cell aperture and uniformity can be prepared.
Description
Technical Field
The invention relates to the field of polymer materials, in particular to a thermotropic liquid crystal polymer microporous foam material and a preparation method thereof.
Background
The polymer foam material is a solid/gas composite material, has excellent properties such as light weight, high specific strength, large specific surface area, sound and heat insulation, damping and shock absorption and the like, and is widely applied to industrial production and daily life. With the development and progress of the technology, the requirements on the performance of the polymer foam material in the fields of national defense and military industry, aerospace, ships, rail traffic and the like are higher and higher, such as high strength, high temperature resistance, radiation resistance, chemical corrosion resistance, flame retardance and the like. Thermotropic liquid crystal polymer has a series of excellent properties such as high strength and high modulus, outstanding heat resistance, extremely small linear expansion coefficient, excellent flame resistance, electric insulation, chemical corrosion resistance, weather aging resistance and microwave permeability, and excellent molding processability, and has wide application in the fields of electronic and electrical manufacturing, automobile and mechanical industry, aerospace and military apparatus, chemical equipment and the like.
Thermotropic liquid crystalline polymer foams have great market potential, however, applicants have found that thermotropic liquid crystalline polymers with high processing temperatures are difficult to use with conventional physical and chemical blowing agents.
Because the current thermotropic liquid crystal polymers have high processing temperature and are difficult to foam, improvement on the thermotropic liquid crystal polymers is needed.
Disclosure of Invention
In view of the above, the present invention provides a thermotropic liquid crystal polymer microporous foam material and a preparation method thereof, so as to solve or at least partially solve the technical problems in the prior art.
In a first aspect, the present invention provides a method for preparing a thermotropic liquid crystalline polymer microcellular foam material, 1, comprising the steps of:
placing a thermotropic liquid crystal polymer into a reaction kettle, introducing a supercritical fluid foaming agent to ensure that the pressure in the reaction kettle is 3.3-25 MPa, keeping the temperature in the reaction kettle at 0-280 ℃ for a certain time, heating to 200-330 ℃, keeping for 5-25 min, and relieving the pressure in the reaction kettle to normal pressure within 5-100 s to prepare the thermotropic liquid crystal polymer microporous foam material;
or placing the thermotropic liquid crystal polymer into a reaction kettle, introducing a supercritical fluid foaming agent to ensure that the pressure in the reaction kettle is 3.3-25 MPa, keeping the temperature in the reaction kettle at 20-250 ℃ for a certain time, relieving the pressure in the reaction kettle to normal pressure within 2-10 min, and then placing a sample in the reaction kettle at 180-330 ℃ for foaming to obtain the thermotropic liquid crystal polymer microporous foam material;
or placing the thermotropic liquid crystal polymer into a reaction kettle, introducing a supercritical fluid foaming agent to ensure that the pressure in the reaction kettle is 3.3-25 MPa, keeping the temperature in the reaction kettle at 20-250 ℃ for a certain time, relieving the pressure in the reaction kettle to normal pressure within 2-10 min, and placing a sample in the reaction kettle into a mold of a vulcanizing machine for foaming to obtain the thermotropic liquid crystal polymer microporous foam material;
based on the above technical solution, preferably, in the preparation method of the thermotropic liquid crystal polymer microcellular foam material, the supercritical fluid foaming agent includes carbon dioxide and/or nitrogen.
On the basis of the technical scheme, preferably, the preparation method of the thermotropic liquid crystal polymer microporous foam material comprises the steps of placing the thermotropic liquid crystal polymer in a reaction kettle, and simultaneously adding a foaming nucleating agent and/or an antioxidant into the reaction kettle.
On the basis of the technical scheme, preferably, the preparation method of the thermotropic liquid crystal polymer microporous foam material comprises the step of preparing the foaming nucleating agent, wherein the foaming nucleating agent comprises one or more of nano silicon dioxide, nano clay, nano montmorillonite, nano molybdenum disulfide, nano kaolin, a carbon nano tube and microcrystalline cellulose.
On the basis of the technical scheme, preferably, the preparation method of the thermotropic liquid crystal polymer microporous foam material further comprises the step of carrying out heat treatment on the obtained thermotropic liquid crystal polymer microporous foam material under the protection of inert gas.
Further preferably, in the preparation method of the thermotropic liquid crystal polymer microporous foam material, the heat treatment temperature is 230-250 ℃ and the time is 6-10 hours; the inert gas comprises one of nitrogen and helium.
On the basis of the above technical solution, preferably, the method for preparing the thermotropic liquid crystal polymer microcellular foam material, wherein the step of placing the sample in the reaction kettle in a mold of a vulcanizer for foaming specifically comprises: and (3) placing the sample in the reaction kettle in a mold of a vulcanizing machine, keeping the pressure of the mold at 3-25 MPa and the temperature at 200-330 ℃ for 5-10 min, and then opening the mold for 5-10 mm.
On the basis of the technical scheme, the preferable preparation method of the thermotropic liquid crystal polymer microporous foam material is that in the step of keeping the temperature in the reaction kettle at 0-280 ℃ for a certain time, the maintaining time is 5-10 hours; in the step of maintaining the temperature in the reaction kettle at 20-250 ℃ for a certain time, the maintaining time is 15-25 h.
In a second aspect, the invention also provides a thermotropic liquid crystal polymer microporous foam material prepared by the preparation method.
On the basis of the technical scheme, preferably, the thermotropic liquid crystal polymer microporous foam material has the average cell diameter of 0.8-200 mu m and the cell density of more than 3.0 multiplied by 106Per cm3。
Compared with the prior art, the preparation method of the thermotropic liquid crystal polymer microporous foam material has the following beneficial effects:
(1) in order to overcome the technical problem that the conventional physical and chemical foaming agents are difficult to use due to the fact that the processing temperature of the thermotropic liquid crystal polymer is high, the thermotropic liquid crystal polymer microporous foam can be prepared at a lower temperature by using the supercritical fluid as the foaming agent, the foaming temperature is generally between the glass transition temperature and the melting point of the thermotropic liquid crystal polymer, and the microporous foam material with high foam hole density, small and uniform cell aperture can be prepared.
(2) The preparation method of the thermotropic liquid crystal polymer microporous foam material also comprises the step of carrying out heat treatment on the foam material, and the melting point of the foam material can be further improved by carrying out heat treatment on the foam material.
Detailed Description
In the following, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The embodiment of the application provides a preparation method of a thermotropic liquid crystal polymer microporous foam material, which comprises the following steps:
placing a thermotropic liquid crystal polymer into a reaction kettle, introducing a supercritical fluid foaming agent to ensure that the pressure in the reaction kettle is 3.3-25 MPa, keeping the temperature in the reaction kettle at 0-280 ℃ for a certain time, heating to 200-330 ℃, keeping for 5-25 min, and relieving the pressure in the reaction kettle to normal pressure within 5-100 s to prepare the thermotropic liquid crystal polymer microporous foam material;
or placing the thermotropic liquid crystal polymer into a reaction kettle, introducing a supercritical fluid foaming agent to ensure that the pressure in the reaction kettle is 3.3-25 MPa, keeping the temperature in the reaction kettle at 20-250 ℃ for a certain time, relieving the pressure in the reaction kettle to normal pressure within 2-10 min, and then placing a sample in the reaction kettle at 180-330 ℃ for foaming to obtain the thermotropic liquid crystal polymer microporous foam material;
or placing the thermotropic liquid crystal polymer into a reaction kettle, introducing a supercritical fluid foaming agent to ensure that the pressure in the reaction kettle is 3.3-25 MPa, keeping the temperature in the reaction kettle at 20-250 ℃ for a certain time, relieving the pressure in the reaction kettle to normal pressure within 2-10 min, and placing a sample in the reaction kettle into a mold of a vulcanizing machine for foaming to obtain the thermotropic liquid crystal polymer microporous foam material.
In the present application, the thermotropic liquid crystal polymer is an aromatic copolyester liquid crystal polymer, and a high molecular substance having both liquid fluidity and crystal physical property anisotropy state can appear under certain physical conditions. Specifically, this application embodiment is last to be installed discharge valve, controls the pressure release time of reation kettle internal pressure through discharge valve.
In order to overcome the technical problem that the conventional physical and chemical foaming agents with high processing temperature of thermotropic liquid crystal polymers are difficult to use, the preparation method of the thermotropic liquid crystal polymer microporous foam material uses the supercritical fluid as the foaming agent, the supercritical fluid has good diffusivity and solubility, and has a plasticizing effect on the polymer, the polymer can be foamed under the condition of being lower than a melting point or a processing temperature, the thermotropic liquid crystal polymer microporous foam can be prepared at a lower temperature, the foaming temperature is generally between the glass transition temperature and the melting point of the thermotropic liquid crystal polymer, and the microporous foam material with high cell density, small cell aperture and uniformity can be prepared.
In some embodiments, the supercritical fluid blowing agent comprises carbon dioxide and/or nitrogen.
In some embodiments, the thermotropic liquid crystalline polymer is placed in a reaction kettle while a foam nucleating agent and/or an antioxidant is also added to the reaction kettle.
In the above examples, if the foam nucleating agent and/or the antioxidant are added, the thermotropic liquid crystal polymer, the foam nucleating agent and/or the antioxidant are mixed and then thermally pressed into a sheet sample, and then the sheet sample is placed in the reaction kettle.
In some embodiments, the foam nucleating agent comprises one or more of nano-silica, nano-clay, nano-montmorillonite, nano-molybdenum disulfide, nano-kaolin, carbon nanotubes, and microcrystalline cellulose.
In some embodiments, the antioxidant includes, but is not limited to, one or more of phosphite type antioxidants, phenolic ester type antioxidants, thioether type sterically hindered phenolic antioxidants, and the like.
In some embodiments, the method further comprises the step of carrying out heat treatment on the thermotropic liquid crystal polymer microporous foam material under the protection of inert gas.
In some embodiments, the temperature of the heat treatment is 230-250 ℃ and the time is 6-10 h; the inert gas comprises one of nitrogen and helium. The melting point of the foam material can be further improved by subjecting the foam material to a heat treatment.
In some embodiments, further placing the sample in the autoclave into a mold of a vulcanizer for foaming specifically comprises: and (3) placing the sample in the reaction kettle in a mold of a vulcanizing machine, keeping the pressure of the mold at 3-25 MPa and the temperature at 200-330 ℃ for 5-10 min, and then opening the mold for 5-10 mm. In the examples of the present application, thermotropic liquid crystalline polymer microcellular foams of high expansion ratios were prepared by combining a supercritical fluid foaming agent and compression molding foaming.
In some embodiments, the step of maintaining the temperature in the reaction kettle at 0-280 ℃ for a certain time is performed for 5-10 hours; and keeping the temperature in the reaction kettle at 20-250 ℃ for a certain time, wherein the keeping time is 15-25 h.
Based on the same invention concept, the application also provides a thermotropic liquid crystal polymer microporous foam material which is prepared by the preparation method, and the thermotropic liquid crystal polymer microporous foam material has the average cell diameter of 0.8-200 mu m and the cell density of more than 3.0 multiplied by 106Per cm3。
The following further illustrates, in specific examples, the preparation of thermotropic liquid crystalline polymer microcellular foams of the present application.
Example 1
The embodiment of the application provides a preparation method of a thermotropic liquid crystal polymer microporous foam material, which comprises the following steps:
s1, mixing 100 parts by weight of thermotropic liquid crystal polymer and 0.5 part by weight of nano montmorillonite, and then hot-pressing to form a sheet sample with the thickness of 1 mm;
s2, placing the sheet sample in a reaction kettle, introducing supercritical fluid foaming agent carbon dioxide into the reaction kettle to enable the pressure in the reaction kettle to be 15MPa, keeping the temperature in the reaction kettle at 100 ℃, keeping the temperature and pressure for 6 hours, then heating the reaction kettle to 270 ℃, continuing to keep the pressure at 15MPa, keeping the temperature and pressure for 5 minutes again, relieving the pressure in the reaction kettle to normal pressure within 40 seconds, and inducing the foaming agent to nucleate and foam through pressure drop to obtain a foamed product;
s3, placing the foamed product in a heat treatment furnace under nitrogen protection for heat treatment at 230 ℃ for 10h to obtain the thermotropic liquid crystal polymer microporous foam material.
Tests show that the foaming multiplying power of the thermotropic liquid crystal polymer microporous foam material prepared by the method is about 1.2 times, and the cell density is 8.6 multiplied by 108Per cm3The average cell diameter was 1 μm.
Example 2
The embodiment of the application provides a preparation method of a thermotropic liquid crystal polymer microporous foam material, which comprises the following steps:
s1, mixing 100 parts by weight of thermotropic liquid crystal polymer, 1 part by weight of nano silicon dioxide and 0.2 part by weight of phosphite antioxidant, and then carrying out hot pressing on the mixture to form a sheet sample with the thickness of 2 mm;
s2, placing the flaky sample in a reaction kettle, introducing carbon dioxide serving as a supercritical fluid foaming agent into the reaction kettle to enable the pressure in the reaction kettle to be 8MPa, keeping the temperature in the reaction kettle at 80 ℃, keeping the temperature and the pressure for 16 hours, then relieving the pressure in the reaction kettle to normal pressure within 2.5 minutes, taking out the sample in the reaction kettle, placing the sample in an oil bath at 300 ℃, inducing the foaming agent to nucleate and foam at high temperature, and obtaining a foamed product after foaming is completed;
and S3, placing the foamed product in a heat treatment furnace under the protection of nitrogen for heat treatment for 6 hours at 250 ℃, and obtaining the thermotropic liquid crystal polymer microporous foam material.
Tests show that the thermotropic liquid crystal polymer microporous foam material prepared by the method has the foaming multiplying power of about 2 times and the cell density of 1.6 multiplied by 108Per cm3And the average cell diameter was 12 microns.
Example 3
The embodiment of the application provides a preparation method of a thermotropic liquid crystal polymer microporous foam material, which comprises the following steps:
s1, mixing 100 parts by weight of thermotropic liquid crystal polymer, 0.5 part by weight of nano silicon dioxide and 0.1 part by weight of phosphite antioxidant, and then carrying out hot pressing on the mixture to form a sheet sample with the thickness of 2 mm;
s2, placing the flaky sample in a reaction kettle, introducing nitrogen serving as a supercritical fluid foaming agent into the reaction kettle to enable the pressure in the reaction kettle to be 15MPa, keeping the temperature in the reaction kettle at 60 ℃, keeping the temperature and the pressure for 24 hours, then relieving the pressure in the reaction kettle to normal pressure within 3 minutes, taking out the sample in the reaction kettle, placing the sample in an oil bath at 280 ℃, inducing the foaming agent to nucleate and foam at high temperature, and obtaining a foamed product after foaming is completed;
and S3, placing the foamed product in a heat treatment furnace under the protection of nitrogen for heat treatment at 250 ℃ for 10 hours to obtain the thermotropic liquid crystal polymer microporous foam material.
Tests show that the thermotropic liquid crystal polymer microporous foam material prepared by the method has the foaming multiplying power of about 1.5 times and the cell density of 9.0 multiplied by 107Per cm3And the average cell diameter was 8 μm.
Example 4
The embodiment of the application provides a preparation method of a thermotropic liquid crystal polymer microporous foam material, which comprises the following steps:
s1, placing 100 parts by weight of thermotropic liquid crystal polymer with the average particle size of 2nm into a reaction kettle;
s2, introducing supercritical fluid foaming agent carbon dioxide into the reaction kettle to enable the pressure in the reaction kettle to be 20MPa, keeping the temperature in the reaction kettle at 45 ℃, keeping the temperature and the pressure for 20 hours, then relieving the pressure in the reaction kettle to normal pressure within 5 minutes, taking out a sample in the reaction kettle, putting the sample into a mold between flat vulcanizing machines, pressurizing the mold for 15MPa, rapidly heating the mold to 320 ℃, opening the mold for 6mm after keeping the temperature and the pressure for 5 minutes, foaming thermotropic liquid crystal polymer particles and mutually bonding the particles at high temperature and high pressure, and completely opening the mold after the temperature of the mold is reduced to be below 100 ℃ to obtain a foamed product;
and S3, placing the foamed product in a heat treatment furnace under the protection of nitrogen for heat treatment at 245 ℃ for 8 hours to obtain the thermotropic liquid crystal polymer microporous foam material.
Tests show that the thermotropic liquid crystal polymer microporous foam material prepared by the method has the foaming multiplying power of about 4 times and the cell density of 6.2 multiplied by 107Per cm3And the average cell diameter was 32 μm.
Comparative example 1
The comparative example provides a method for preparing a thermotropic liquid crystalline polymer microcellular foam, which is the same as that of example 1, except that the heat treatment of the heat treatment furnace in step S3 is not performed, and the remaining processes are the same.
The melting points and initial decomposition temperatures of the thermotropic liquid crystalline polymer microcellular foams prepared in the above examples 1 to 4 and comparative example 1 were measured, and the results are shown in the following table 1. Wherein, a differential scanning calorimeter is adopted to test the melting point of the material, the heating rate is 10 ℃/min, and the atmosphere is nitrogen; the initial decomposition temperature of the material is tested by a thermal gravimetric analyzer, the heating rate is 10 ℃/min, the temperature is increased from 40 ℃ to 800 ℃, and the atmosphere is nitrogen.
TABLE 1-melting Point (. degree. C.) and initial decomposition temperature (. degree. C.) of microcellular foams prepared in different examples
As can be seen from the comparison of example 1 and comparative example 1 in Table 1 above, the thermotropic liquid crystalline polymer microcellular foam obtained after heat treatment had a slightly higher melting point and initial decomposition than those obtained without heat treatment.
The invention is not to be considered as limited to the particular embodiments shown and described, but is to be accorded the widest scope consistent with the principles and novel features herein disclosed.
Claims (10)
1. A preparation method of thermotropic liquid crystal polymer microcellular foam material is characterized by comprising the following steps:
placing a thermotropic liquid crystal polymer into a reaction kettle, introducing a supercritical fluid foaming agent to ensure that the pressure in the reaction kettle is 3.3-25 MPa, keeping the temperature in the reaction kettle at 0-280 ℃ for a certain time, heating to 200-330 ℃, keeping for 5-25 min, and relieving the pressure in the reaction kettle to normal pressure within 5-100 s to prepare the thermotropic liquid crystal polymer microporous foam material;
or placing the thermotropic liquid crystal polymer into a reaction kettle, introducing a supercritical fluid foaming agent to ensure that the pressure in the reaction kettle is 3.3-25 MPa, keeping the temperature in the reaction kettle at 20-250 ℃ for a certain time, relieving the pressure in the reaction kettle to normal pressure within 2-10 min, and then placing a sample in the reaction kettle at 180-330 ℃ for foaming to obtain the thermotropic liquid crystal polymer microporous foam material;
or placing the thermotropic liquid crystal polymer into a reaction kettle, introducing a supercritical fluid foaming agent to ensure that the pressure in the reaction kettle is 3.3-25 MPa, keeping the temperature in the reaction kettle at 20-250 ℃ for a certain time, relieving the pressure in the reaction kettle to normal pressure within 2-10 min, and placing a sample in the reaction kettle into a mold of a vulcanizing machine for foaming to obtain the thermotropic liquid crystal polymer microporous foam material.
2. The method of preparing a thermotropic liquid crystalline polymer microcellular foam material of claim 1, wherein the supercritical fluid blowing agent comprises carbon dioxide and/or nitrogen.
3. The process for preparing a thermotropic liquid crystalline polymer microcellular foam material according to claim 1, wherein the thermotropic liquid crystalline polymer is placed in a reaction vessel while adding a foam nucleating agent and/or an antioxidant to the reaction vessel.
4. The method for preparing thermotropic liquid crystal polymer microporous foam material of claim 3, wherein the foaming nucleating agent comprises one or more of nano silicon dioxide, nano clay, nano montmorillonite, nano molybdenum disulfide, nano kaolin, carbon nanotube and microcrystalline cellulose.
5. The method of claim 1, further comprising heat treating the thermotropic liquid crystalline polymer microcellular foam obtained under an inert gas atmosphere.
6. The method for preparing a thermotropic liquid crystalline polymer microcellular foam material according to claim 5, wherein the heat treatment is performed at a temperature of 230 to 250 ℃ for 6 to 10 hours; the inert gas comprises one of nitrogen and helium.
7. The method of claim 1, wherein the step of placing the sample in the autoclave into a mold of a vulcanizer for foaming comprises: and (3) placing the sample in the reaction kettle in a mold of a vulcanizing machine, keeping the pressure of the mold at 3-25 MPa and the temperature at 200-330 ℃ for 5-10 min, and then opening the mold for 5-10 mm.
8. The method for preparing the thermotropic liquid crystal polymer microporous foam material of claim 1, wherein in the step of maintaining the temperature in the reaction vessel at 0 to 280 ℃ for a certain period of time, the maintaining time is 5 to 10 hours; in the step of maintaining the temperature in the reaction kettle at 20-250 ℃ for a certain time, the maintaining time is 15-25 h.
9. A thermotropic liquid crystalline polymer microcellular foam material, which is prepared by the preparation method as claimed in any one of claims 1 to 8.
10. The thermotropic liquid crystalline polymer microcellular foam material of claim 9, having an average cell diameter of 0.8 to 200 μm and a cell density of more than 3.0 x 106Per cm3。
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| WO2022209618A1 (en) * | 2021-03-31 | 2022-10-06 | 日東電工株式会社 | Method for producing porous liquid crystal polymer and porosity-imparting agent |
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