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Thermotropic liquid crystal polyester material and preparation method thereof

A liquid crystal polyester, thermotropic technology, applied in the direction of liquid crystal materials, chemical instruments and methods, etc., can solve the problems of high packing degree, limited application, high melting point of materials, etc., and achieve the effect of lowering the melting point and reducing the degree of close packing

Active Publication Date: 2021-10-15
宁夏清研高分子新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The polyp-hydroxybenzoic acid thermotropic liquid crystal material prepared with p-hydroxybenzoic acid as a monomer has a very high melting point due to its high molecular chain rigidity and high packing degree, which in turn affects its composite processing with other polymer materials. Limit its application in the field of polymer material processing aids

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] One embodiment of the present invention provides a method for preparing a thermotropic liquid crystal polyester material, which includes the following steps:

[0037] (1) Preparation of acetylated monomer: Take 0.1mol of p-hydroxybenzoic acid, 0.15mol of acetic anhydride and 0.2g of concentrated sulfuric acid and add them into a three-necked flask under stirring conditions, stir at 160°C for 3h, then stir in an ice-water bath for 0.5h, Filter, wash and dry to obtain acetylated p-hydroxybenzoic acid.

[0038] Take 0.1mol of 4-hydroxy-3-methoxybenzoic acid, 0.15mol of acetic anhydride and 0.2g of concentrated sulfuric acid into a three-necked flask under stirring conditions, stir at 160°C for 3h, stir in an ice-water bath for 0.5h, filter and wash , and dried to obtain acetylated 4-hydroxy-3-methoxybenzoic acid.

[0039] (2) Preparation of thermotropic liquid crystal polyester material: 0.09mol acetylated p-hydroxybenzoic acid, 0.01mol acetylated 4-hydroxy-3-methoxybenzo...

Embodiment 2

[0042] One embodiment of the present invention provides a method for preparing a thermotropic liquid crystal polyester material, which includes the following steps:

[0043] (1) Preparation of acetylated monomer: Take 0.1mol of p-hydroxybenzoic acid, 0.1mol of acetic anhydride and 0.2g of concentrated sulfuric acid and add them to a three-necked flask under stirring conditions, stir at 150°C for 3h, stir in an ice-water bath for 2h, and filter , washed and dried to obtain acetylated p-hydroxybenzoic acid.

[0044] Take 0.1mol of 4-hydroxy-3-methoxybenzoic acid, 0.1mol of acetic anhydride and 0.2g of concentrated sulfuric acid and add them into a three-necked flask under stirring conditions, stir at 150°C for 3h, then stir in an ice-water bath for 2h, filter, wash, Dry to obtain acetylated 4-hydroxy-3-methoxybenzoic acid.

[0045] (2) Preparation of thermotropic liquid crystal polyester material: 0.05mol acetylated p-hydroxybenzoic acid, 0.05mol acetylated 4-hydroxy-3-methoxyb...

Embodiment 3

[0048] One embodiment of the present invention provides a method for preparing a thermotropic liquid crystal polyester material, which includes the following steps:

[0049] (1) Preparation of acetylated monomer: Take 0.1mol of p-hydroxybenzoic acid, 0.3mol of acetic anhydride and 0.2g of concentrated sulfuric acid and add them into a three-necked flask under stirring conditions, stir at 300°C for 1h, then stir in an ice-water bath for 0.5h, Filter, wash and dry to obtain acetylated p-hydroxybenzoic acid.

[0050] Take 0.1mol of 4-hydroxyphenylpyruvate, 0.3mol of acetic anhydride and 0.2g of concentrated sulfuric acid and add them into a three-neck flask under stirring conditions, stir at 300°C for 1h, then stir in an ice-water bath for 0.5h, filter, wash, and dry. Acetylated 4-hydroxyphenylpyruvate is obtained.

[0051] (2) Preparation of thermotropic liquid crystal polyester material: 0.07mol acetylated p-hydroxybenzoic acid, 0.03mol acetylated 4-hydroxyphenylpyruvate, 10ml...

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Abstract

The invention discloses a thermotropic liquid crystal polyester material and a preparation method thereof, and the preparation method comprises the following steps: (1) preparing acetylated monomers: respectively carrying out acetylation reaction on monomers to obtain acetylated monomers; and (2) preparing the thermotropic liquid crystal polyester material: polymerizing the acetylated monomer, acetic anhydride and zinc acetate at high temperature, and crushing to obtain the thermotropic liquid crystal polyester material, wherein the acetylated monomer comprises acetylated hydroxybenzoic acid and an acetylated first monomer. Through monomer acetylation, the reaction activity of the monomer can be improved, and self-polymerization of the monomer and oxidation of hydroxyl in the monomer are avoided; and the close packing degree of a regular polymer molecular chain is reduced by adjusting the variety and proportion of acetylated monomers, so that the melting point of the thermotropic liquid crystal copolyester is reduced, and the thermotropic liquid crystal copolyester is widely applied to the field of high polymer material processing aids.

Description

technical field [0001] The invention relates to the technical field of liquid crystal polymers, in particular to a thermotropic liquid crystal polyester material and a preparation method thereof. Background technique [0002] Liquid crystal polymer (LCP) is a kind of polymer material that loses the fluidity of the substance after being melted by heat or dissolved by a solvent, but can still maintain part of the orderly arrangement, forming a polymer material with both crystal and liquid properties. According to the different ways of presenting the liquid crystal state, liquid crystal polymers can be further divided into thermotropic liquid crystal polymers and lyotropic liquid crystal polymers. Among them, thermotropic liquid crystal refers to the liquid crystal state of the material within a certain temperature range as the temperature changes, while lyotropic liquid crystal refers to the liquid crystal state of the material within a certain concentration range. [0003] T...

Claims

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Application Information

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IPC IPC(8): C08G63/06C08G63/664C08G63/78C09K19/38
CPCC08G63/065C08G63/664C08G63/78C09K19/3809C08G2250/00
Inventor 张东宝于冉徐良
Owner 宁夏清研高分子新材料有限公司
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