阅读说明：本技术 一种易于成型加工的高耐热lcp材料及其制备方法 (High-heat-resistance LCP material easy to mold and process and preparation method thereof ) 是由 张东宝 于冉 徐良 于 2021-09-08 设计创作，主要内容包括：本发明公开了一种易于成型加工的高耐热LCP材料及其制备方法,其制备方法包括以下步骤：将混合单体、反应性封端剂、无机填料和乙酸酐混合,保护气氛下搅拌,按照预设程序升温,保护气氛下冷却,粉碎研磨,得到易于成型加工的高耐热LCP材料；其中,所述的反应性封端剂包括N-(4-羧基苯基))-4-苯基乙炔基邻苯二甲酰亚胺和N-(4-乙酰氧基苯基)-4-苯基乙炔基邻苯二甲酰亚胺。本发明通过引入反应性封端剂,通过降低聚合物主链的分子量起降低熔点作用同时反应性封端剂也能使线型聚合物交联固化,提高交联密度,提高LCP的耐热性能。另外引入合适的碳纳米填料,进一步提升其耐热性能,从而最终达到保证LCP材料高耐热性能的同时又兼顾可加工性。(The invention discloses a high heat-resistant LCP material easy to form and process and a preparation method thereof, wherein the preparation method comprises the following steps: mixing the mixed monomer, the reactive end-capping reagent, the inorganic filler and the acetic anhydride, stirring under a protective atmosphere, heating according to a preset program, cooling under the protective atmosphere, crushing and grinding to obtain the high heat-resistant LCP material easy to mold and process; wherein the reactive end-capping reagent comprises N- (4-carboxyphenyl)) -4-phenylethynylphthalimide and N- (4-acetoxyphenyl) -4-phenylethynylphthalimide. The invention introduces the reactive end capping agent, reduces the molecular weight of the main chain of the polymer to play a role in reducing the melting point, and simultaneously, the reactive end capping agent can also enable the linear polymer to be crosslinked and cured, thereby improving the crosslinking density and the heat resistance of the LCP. In addition, proper carbon nano-filler is introduced to further improve the heat resistance of the LCP material, so that the high heat resistance of the LCP material is ensured and the processability is also considered.)

1. A preparation method of a high heat-resistant LCP material easy to form and process is characterized by comprising the following steps:

mixing the mixed monomer, the reactive end-capping reagent, the inorganic filler and the acetic anhydride, stirring under a protective atmosphere, heating according to a preset program, cooling under the protective atmosphere, crushing and grinding to obtain the high heat-resistant LCP material easy to mold and process;

wherein the reactive end-capping reagent comprises N- (4-carboxyphenyl)) -4-phenylethynylphthalimide and N- (4-acetoxyphenyl) -4-phenylethynylphthalimide.

2. The method for preparing easy-to-mold high heat-resistant LCP material as claimed in claim 1, wherein the mixed monomer is at least three of 4-hydroxybenzoic acid, terephthalic acid, 4' -dihydroxybiphenyl, hydroquinone, 6-hydroxy-2-naphthoic acid and 2, 6-naphthoic acid;

the inorganic filler is carbon nano-tube.

3. The method for preparing a high heat-resistant LCP material easy to mold and process as claimed in claim 1, wherein the predetermined procedure comprises: heating to 130-.

4. The method for preparing high heat resistant LCP material easy to mold and process as claimed in claim 1, wherein the molar ratio of the mixed monomer and the reactive end-capping agent is 1: 0.1-0.2;

the inorganic filler accounts for 0.5-5% of the mixed monomer by mass.

5. The method for preparing high heat-resistant LCP material easy to mold and process as claimed in claim 1, wherein the method for preparing N- (4-carboxyphenyl)) -4-phenylethynylphthalimide comprises:

heating and dissolving 4-phenylethynyl phthalic anhydride in acetic acid, adding 4-aminobenzoic acid, heating and preserving heat, cooling to separate out crystals, washing and drying to obtain N- (4-carboxyphenyl)) -4-phenylethynyl phthalimide.

6. The method for preparing high heat-resistant LCP material easy to mold and process according to claim 1, wherein the method for preparing N- (4-acetoxyphenyl) -4-phenylethynylphthalimide comprises:

heating and dissolving 4-phenylethynyl phthalic anhydride in acetic acid, adding 4-aminophenol, heating and preserving heat, cooling to separate out crystals, washing and drying to obtain the N- (4-acetoxyphenyl) -4-phenylethynyl phthalimide.

7. The method for preparing high heat resistant LCP material easy to mold and process according to claim 5 or 6, wherein the molar ratio of 4-phenylethynyl phthalic anhydride and acetic acid is 1: 30-40;

the heating and heat preservation temperature is 130-150 ℃, and the time is 4-6 h;

the cooling temperature is 50-60 ℃;

the drying temperature is 150 ℃ and 170 ℃, and the drying time is 24-36 h.

8. The method for preparing high heat resistant LCP material easy to mold and process as claimed in claim 5, wherein the molar ratio of 4-phenylethynyl phthalic anhydride and 4-aminobenzoic acid is 1: 1.

9. The method for preparing high heat resistant LCP material easy to mold and process as claimed in claim 6, wherein the molar ratio of 4-phenylethynyl phthalic anhydride and 4-aminophenol is 1: 1.

10. A high heat resistant LCP material which is easily shaped and processed, prepared by the method of any one of claims 1 to 9; the melting point of the high-heat-resistance LCP material easy to mold and process is 240-330 ℃, and the thermal decomposition temperature is 435-490 ℃.

Technical Field

The invention relates to the technical field of liquid crystal polymers, in particular to a high-heat-resistance LCP material easy to mold and process and a preparation method thereof.

Background

High-performance polymers are distinguished by high heat resistance and generally exhibit a high glass transition temperature (Tg > 200 ℃) or an outstanding initial thermal decomposition temperature (Td > 350 ℃) or outstanding mechanical properties. Current high performance polymers are generally based on the use of aromatic (heterocyclic) monomers.

Backbone wholly aromatic liquid crystalline polymers (MALCPs) are one of the unique high performance wholly aromatic polymers that are capable of forming highly ordered structures in solution (lyotropic liquid crystals) or in the molten state (thermotropic liquid crystals) and of exhibiting a high degree of orientation in the polymer chains by processing MALCPs in the liquid crystal phase.

Wholly aromatic thermotropic liquid crystal polyesters, which are the most widely studied class of thermotropic liquid crystals in MALCPs, are composed mainly of aromatic moieties linked by ester functional groups. Thermotropic Liquid Crystalline Polyesters (TLCPs) having a fully aromatic backbone are relatively excellent in heat resistance, mechanical properties and chemical resistance.

However, most LCP materials have melting points that are too high above the thermal decomposition temperature. They decompose before melting, making the LCP material difficult to shape.

Disclosure of Invention

In view of the above-mentioned disadvantages of the prior art, the present invention aims to provide a high heat-resistant LCP material which is easily molded and processed, and a method for preparing the same, and to obtain a low-melting-point, high heat-resistant LCP material.

In order to achieve the purpose, the invention is realized by the following technical scheme:

a preparation method of a high heat-resistant LCP material easy to form and process comprises the following steps:

mixing the mixed monomer, the reactive end-capping reagent, the inorganic filler and the acetic anhydride, stirring under a protective atmosphere, heating according to a preset program, cooling under the protective atmosphere, crushing and grinding to obtain the high heat-resistant LCP material easy to mold and process;

wherein the reactive end-capping reagent comprises N- (4-carboxyphenyl)) -4-phenylethynylphthalimide and N- (4-acetoxyphenyl) -4-phenylethynylphthalimide.

The preparation method of the high heat-resistant LCP material easy to mold and process comprises the following steps of mixing at least three monomers selected from 4-hydroxybenzoic acid, terephthalic acid, 4' -dihydroxybiphenyl, hydroquinone, 6-hydroxy-2-naphthoic acid and 2, 6-naphthalenedicarboxylic acid;

the inorganic filler is carbon nano-tube.

The preparation method of the high heat-resistant LCP material easy to mold and process comprises the following steps: heating to 130-.

The preparation method of the high heat-resistant LCP material easy to form and process is characterized in that the molar ratio of the mixed monomer to the reactive end-capping reagent is 1: 0.1-0.2;

the inorganic filler accounts for 0.5-5% of the mixed monomer by mass.

The preparation method of the high heat-resistant LCP material easy to mold and process comprises the following steps:

heating and dissolving 4-phenylethynyl phthalic anhydride in acetic acid, adding 4-aminobenzoic acid, heating and preserving heat, cooling to separate out crystals, washing and drying to obtain N- (4-carboxyphenyl)) -4-phenylethynyl phthalimide.

The preparation method of the high heat-resistant LCP material easy to mold and process comprises the following steps:

heating and dissolving 4-phenylethynyl phthalic anhydride in acetic acid, adding 4-aminophenol, heating and preserving heat, cooling to separate out crystals, washing and drying to obtain the N- (4-acetoxyphenyl) -4-phenylethynyl phthalimide.

The preparation method of the high heat-resistant LCP material easy to mold and process comprises the following steps of (1) preparing a high heat-resistant LCP material, wherein the molar ratio of 4-phenylethynyl phthalic anhydride to acetic acid is 1: 30-40;

the heating and heat preservation temperature is 130-150 ℃, and the time is 4-6 h;

the cooling temperature is 50-60 ℃;

the drying temperature is 150 ℃ and 170 ℃, and the drying time is 24-36 h.

The preparation method of the high heat-resistant LCP material easy to mold and process comprises the step of preparing the high heat-resistant LCP material, wherein the molar ratio of the 4-phenylethynyl phthalic anhydride to the 4-aminobenzoic acid is 1: 1.

The preparation method of the high-heat-resistance LCP material easy to mold and process comprises the step of preparing the high-heat-resistance LCP material, wherein the molar ratio of the 4-phenylethynyl phthalic anhydride to the 4-aminophenol is 1: 1.

Meanwhile, the invention also provides a high heat-resistant LCP material which is easy to form and process and is prepared by the method; the melting point of the high-heat-resistance LCP material easy to mold and process is 240-330 ℃, and the thermal decomposition temperature is 435-490 ℃.

Has the advantages that: the invention discloses a high heat-resistant LCP material easy to form and process and a preparation method thereof. And then by introducing the reactive end capping agent, the melting point is reduced by reducing the molecular weight of the main chain of the polymer, and meanwhile, the linear polymer can be crosslinked and cured by the reactive end capping agent, so that the crosslinking density is improved, and the heat resistance of the LCP is improved. In addition, proper carbon nano-filler is introduced in the synthesis process, and the heat resistance of the LCP material is further improved by controlling the reasonable addition amount of the carbon nano-filler, so that the high heat resistance of the LCP material is ensured and the processability is also considered at the same time.

Detailed Description

The present invention provides a high heat-resistant LCP material which is easy to be formed and processed and a preparation method thereof, and the present invention is further described in detail below in order to make the purpose, technical scheme and effect of the present invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

Specifically, the invention provides a preparation method of a high heat-resistant LCP material which is easy to form and process, comprising the following steps:

(1) mixing 4-phenylethynyl phthalic anhydride (PEPA) and acetic acid according to a ratio of 1:30-40, adding the mixture into a three-neck flask with a condensing device, heating the mixture to 120 ℃ in an oil bath, slowly adding 4-aminobenzoic acid (ABA) under stirring, heating the mixture to 130-150 ℃, keeping the temperature for 4-6h, naturally cooling the mixture to 50-60 ℃ until crystals are completely precipitated, washing the mixture with acetic acid and ethanol, and drying the mixture for 24-36h at 150-170 ℃ to obtain N- (4-carboxyphenyl)) -4-phenylethynyl phthalimide (PE-COOH).

Wherein the molar ratio of PEPA to ABA is 1: 1.

(2) Mixing 4-phenylethynyl phthalic anhydride (PEPA) and acetic acid according to a ratio of 1:30-40, adding the mixture into a three-neck flask with a condensing device, heating the mixture to 120 ℃ in an oil bath, slowly adding 4-Aminophenol (AP) while stirring, heating the mixture to 130-150 ℃, keeping the temperature for 4-6h, naturally cooling the mixture to 50-60 ℃ until crystals are completely separated out, washing the crystals with acetic acid and ethanol, and drying the crystals for 24-36h at 150-170 ℃ to obtain N- (4-acetoxyphenyl) -4-phenylethynyl phthalimide (PE-OAc).

Wherein the molar ratio of PEPA to AP is 1: 1.

(3) Mixing the mixed monomer, PE-COOH, PE-OAc, the carbon nano tube and acetic anhydride, stirring under a protective atmosphere, heating to 130-;

wherein the mixed monomer is at least three of 4-hydroxybenzoic acid, terephthalic acid, 4' -dihydroxybiphenyl, hydroquinone, 6-hydroxy-2-naphthoic acid and 2, 6-naphthalenedicarboxylic acid;

the molar ratio of the mixed monomer to PE-COOH to PE-OAc is 1: 0.05-0.1: 0.05-0.1.

The mass of the carbon nano tube accounts for 0.5-5% of the mass of the mixed monomer.

Meanwhile, the invention also provides a high heat-resistant LCP material which is easy to form and process and is prepared by the method; the melting point of the high-heat-resistance LCP material easy to mold and process is 240-330 ℃, and the thermal decomposition temperature is 435-490 ℃.

The high heat resistant LCP material of the present invention which is easy to be formed and processed and the preparation method thereof are further explained by the following specific examples:

example 1

One embodiment of the present invention provides a method for preparing a high heat resistant LCP material which is easy to be formed, wherein the method comprises the following steps:

(1) mixing 0.15mol of PEPA and 5mol of acetic acid, adding the mixture into a three-neck flask with a condensing device, heating the mixture in an oil bath at 120 ℃ until PEPA is completely dissolved, slowly adding 0.15mol of ABA while stirring, heating the mixture to 135 ℃, keeping the temperature for 4h, naturally cooling the mixture at 50 ℃ until crystals are completely separated out, washing the crystals with acetic acid and ethanol, and drying the crystals for 24h at 160 ℃ to obtain PE-COOH.

(2) Mixing 0.15mol of PEPA and 5mol of acetic acid, adding the mixture into a three-neck flask with a condensing device, heating the mixture in an oil bath at 120 ℃ until the PEPA is completely dissolved, slowly adding 0.15mol of AP while stirring, heating the mixture to 135 ℃, keeping the temperature for 4h, naturally cooling the mixture at 50 ℃ until crystals are completely separated out, washing the crystals with acetic acid and ethanol, and drying the crystals for 24h at 160 ℃ to obtain the PE-OAc.

(3) Mixing 0.5mol of 4-hydroxybenzoic acid, 0.2mol of terephthalic acid, 0.2mol of hydroquinone, 0.1mol of 6-hydroxy-2-naphthoic acid, 0.1mol of PE-COOH, 0.1mol of PE-OAc and 1.5mol of acetic anhydride, adding 0.5% of carbon nano tube, heating to 150 ℃ under the condition of nitrogen stirring, preserving heat for 1.5h, heating to 250 ℃ for 3h, heating to 300 ℃ for 2h, cooling under a protective atmosphere, crushing and grinding to obtain the high heat-resistant LCP material easy to mold and process;

another embodiment of the present invention also provides a high heat resistant LCP material, which is easily molded, prepared by the method of embodiment 1; the easily molded and processed high heat resistant LCP material of example 1 had a melting point of 252 ℃ and a thermal decomposition temperature of 443 ℃.

Example 2

One embodiment of the present invention provides a method for preparing a high heat resistant LCP material which is easy to be formed, wherein the method comprises the following steps:

(1) mixing 0.1mol of PEPA and 4mol of acetic acid, adding the mixture into a three-neck flask with a condensing device, heating the mixture in an oil bath at 110 ℃ until PEPA is completely dissolved, slowly adding 0.1mol of ABA while stirring, heating the mixture to 130 ℃, keeping the temperature for 6h, naturally cooling the mixture at 60 ℃ until crystals are completely separated out, washing the crystals with acetic acid and ethanol, and drying the crystals for 48h at 150 ℃ to obtain PE-COOH.

(2) Mixing 0.1mol of PEPA and 4mol of acetic acid, adding the mixture into a three-neck flask with a condensing device, heating the mixture to the temperature of 110 ℃ in an oil bath until the PEPA is completely dissolved, slowly adding 0.1mol of AP while stirring, heating the mixture to the temperature of 130 ℃, keeping the temperature for 6 hours, naturally cooling the mixture at the temperature of 60 ℃ until crystals are completely separated out, washing the crystals with acetic acid and ethanol, and drying the crystals for 48 hours at the temperature of 150 ℃ to obtain the PE-OAc.

(3) Mixing 0.5mol of 4-hydroxybenzoic acid, 0.2mol of terephthalic acid, 0.1mol of hydroquinone, 0.2mol of 6-hydroxy-2-naphthoic acid, 0.1mol of PE-COOH, 0.1mol of PE-OAc and 1.5mol of acetic anhydride, adding 5% of carbon nano tubes, heating to 130 ℃ under the condition of nitrogen stirring, preserving heat for 2 hours, heating to 220 ℃ and preserving heat for 4 hours, heating to 290 ℃ and preserving heat for 3 hours, cooling under a protective atmosphere, crushing and grinding to obtain the high heat-resistant LCP material easy to mold and process;

another embodiment of the present invention also provides a high heat resistant LCP material, which is easy to be formed and processed, prepared by the method of embodiment 2; the easily moldable high heat resistant LCP material of example 2 had a melting point of 245 ℃ and a thermal decomposition temperature of 455 ℃.

Example 3

One embodiment of the present invention provides a method for preparing a high heat resistant LCP material which is easy to be formed, wherein the method comprises the following steps:

(1) mixing 0.1mol of PEPA and 4mol of acetic acid, adding the mixture into a three-neck flask with a condensing device, heating the mixture in an oil bath at 120 ℃ until PEPA is completely dissolved, slowly adding 0.1mol of ABA while stirring, heating the mixture to 150 ℃, keeping the temperature for 4h, naturally cooling the mixture at 50 ℃ until crystals are completely separated out, washing the crystals with acetic acid and ethanol, and drying the crystals for 24h at 160 ℃ to obtain PE-COOH.

(2) Mixing 0.1mol of PEPA and 4mol of acetic acid, adding the mixture into a three-neck flask with a condensing device, heating the mixture in an oil bath at 120 ℃ until the PEPA is completely dissolved, slowly adding 0.1mol of AP while stirring, heating the mixture to 150 ℃, keeping the temperature for 4h, naturally cooling the mixture at 50 ℃ until crystals are completely separated out, washing the crystals with acetic acid and ethanol, and drying the crystals for 24h at 160 ℃ to obtain the PE-OAc.

(3) Mixing 0.5mol of 4-hydroxybenzoic acid, 0.2mol of terephthalic acid, 0.2mol of hydroquinone, 0.1mol of 2, 6-naphthalenedicarboxylic acid, 0.05mol of PE-COOH, 0.05mol of PE-OAc and 1.5mol of acetic anhydride, adding 1% of carbon nano tubes, heating to 180 ℃ under the condition of nitrogen stirring, keeping the temperature for 1h, heating to 270 ℃ and keeping the temperature for 2h, heating to 290 ℃ and keeping the temperature for 1h, cooling under the protective atmosphere, crushing and grinding to obtain the high heat-resistant LCP material easy to mold and process;

another embodiment of the present invention also provides a high heat resistant LCP material, which is easy to mold and process, prepared by the method of embodiment 3; the easily molded high heat resistant LCP material of example 3 had a melting point of 256 ℃ and a thermal decomposition temperature of 438 ℃.

Example 4

One embodiment of the present invention provides a method for preparing a high heat resistant LCP material which is easy to be formed, wherein the method comprises the following steps:

(1) mixing 0.1mol of PEPA and 3mol of acetic acid, adding the mixture into a three-neck flask with a condensing device, heating the mixture in an oil bath at 120 ℃ until PEPA is completely dissolved, slowly adding 0.1mol of ABA while stirring, heating the mixture to 135 ℃, keeping the temperature for 4h, naturally cooling the mixture at 50 ℃ until crystals are completely separated out, washing the crystals with acetic acid and ethanol, and drying the crystals for 24h at 160 ℃ to obtain PE-COOH.

(2) Mixing 0.1mol of PEPA and 3mol of acetic acid, adding the mixture into a three-neck flask with a condensing device, heating the mixture in an oil bath at 120 ℃ until the PEPA is completely dissolved, slowly adding 0.1mol of AP while stirring, heating the mixture to 135 ℃, keeping the temperature for 4h, naturally cooling the mixture at 50 ℃ until crystals are completely separated out, washing the crystals with acetic acid and ethanol, and drying the crystals for 24h at 160 ℃ to obtain the PE-OAc.

(3) Mixing 0.5mol of 4-hydroxybenzoic acid, 0.2mol of terephthalic acid, 0.2mol of hydroquinone, 0.1mol of 6-hydroxy-2-naphthoic acid, 0.05mol of PE-COOH, 0.05mol of PE-OAc and 1.5mol of acetic anhydride, adding 1% of carbon nano tube, heating to 150 ℃ under the condition of nitrogen stirring, preserving heat for 1.5h, heating to 250 ℃ for 3h, heating to 300 ℃ for 2h, cooling under a protective atmosphere, crushing and grinding to obtain the high-heat-resistant LCP material easy to mold and process;

another embodiment of the present invention also provides a high heat resistant LCP material, which is easy to be formed and processed, prepared by the method of embodiment 4; the easily molded high heat resistant LCP material of example 4 had a melting point of 265 ℃ and a thermal decomposition temperature of 488 ℃.

Example 5

One embodiment of the present invention provides a method for preparing a high heat resistant LCP material which is easy to be formed, wherein the method comprises the following steps:

(1) mixing 0.1mol of PEPA and 4mol of acetic acid, adding the mixture into a three-neck flask with a condensing device, heating the mixture in an oil bath at 120 ℃ until PEPA is completely dissolved, slowly adding 0.1mol of ABA while stirring, heating the mixture to 135 ℃, keeping the temperature for 4 hours, naturally cooling the mixture at 50 ℃ until crystals are completely separated out, washing the crystals with acetic acid and ethanol, and drying the crystals for 24 hours at 160 ℃ to obtain PE-COOH.

(2) Mixing 0.1mol of PEPA and 4mol of acetic acid, adding the mixture into a three-neck flask with a condensing device, heating the mixture in an oil bath at 120 ℃ until the PEPA is completely dissolved, slowly adding 0.1mol of AP while stirring, heating the mixture to 135 ℃, keeping the temperature for 4 hours, naturally cooling the mixture at 50 ℃ until crystals are completely separated out, washing the crystals with acetic acid and ethanol, and drying the crystals for 24 hours at 160 ℃ to obtain the PE-OAc.

(3) Mixing 0.5mol of 4-hydroxybenzoic acid, 0.2mol of terephthalic acid, 0.2mol of 4, 4' -dihydroxybiphenyl, 0.1mol of 6-hydroxy-2-naphthoic acid, 0.05mol of PE-COOH, 0.05mol of PE-OAc and 1.5mol of acetic anhydride, adding 1% of carbon nano tube, heating to 150 ℃ under the condition of nitrogen stirring, keeping the temperature for 1.5h, heating to 250 ℃ for 3h, heating to 300 ℃ for 2h, cooling under a protective atmosphere, crushing and grinding to obtain the high heat-resistant LCP material easy to mold and process.

Another embodiment of the present invention also provides a high heat resistant LCP material, which is easy to be formed and processed, prepared by the method of embodiment 5; the easily shaped, high heat resistant LCP material of example 5 had a melting point of 325 ℃ and a thermal decomposition temperature of 470 ℃.

Comparative example 1

One comparative example of the present invention provides a method for preparing an LCP material, which comprises the steps of:

mixing 0.5mol of terephthalic acid, 0.2mol of hydroquinone and 1.5mol of acetic anhydride, heating to 150 ℃ under the condition of stirring with nitrogen, preserving heat for 1.5h, heating to 250 ℃ and preserving heat for 3h, heating to 300 ℃ and preserving heat for 2h, cooling under a protective atmosphere, crushing and grinding to obtain the high-heat-resistance LCP material easy to mold and process.

Another comparative example of the present invention also provides an LCP material prepared by the method of comparative example 1; the LCP material of comparative example 1 had a melting point of 580 c and a thermal decomposition temperature of 395 c.

Comparative example 2

One comparative example of the present invention provides a method for preparing an LCP material, which comprises the steps of:

mixing 0.5mol of 4-hydroxybenzoic acid, 0.2mol of terephthalic acid, 0.2mol of hydroquinone, 0.1mol of 6-hydroxy-2-naphthoic acid and 1.5mol of acetic anhydride, heating to 150 ℃ under the condition of stirring nitrogen, preserving heat for 1.5h, heating to 250 ℃ and preserving heat for 3h, heating to 300 ℃ and preserving heat for 2h, cooling in a protective atmosphere, crushing and grinding to obtain the high heat-resistant LCP material easy to mold and process.

Another comparative example of the present invention also provides an LCP material prepared by the method of comparative example 2; the easy LCP material of comparative example 2 had a melting point of 343 ℃ and a thermal decomposition temperature of 415 ℃.

It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.