Preparation method of high-purity LCP material

A high-purity, high-temperature technology, applied in the direction of liquid crystal materials, chemical instruments and methods, etc., can solve the problems of affecting the comprehensive performance of TLCP materials, affecting the properties of TLCP, and low purity, so as to meet the needs of mass production and manufacturing, and good application Foreground, the effect of simple overall process

Pending Publication Date: 2022-01-14
宁夏清研高分子新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the prior art, the synthesis of TLCP materials of HBA/HNA liquid crystal copolyesters is carried out in two steps, first HBA and HNA are acetylated to prepare 4-acetoxybenzoic acid (ABA) and 2-acetoxy-6-naphthalene Formic acid (ANA), and then raised to a certain temperature in an inert gas atmosphere such as nitrogen to prepare TLCP materials, but the reaction of HBA/HNA TLCP materials is very complicated during the polymerization process, and HBA will desorb at 150 ° C. The acid reaction produces phenol, and the process of HBA/HNA copolymerization is not a simple acidolysis process. In the later stage of the reaction, the removal of ketene leads to the generation of phenol end groups, and the deacidification leads to the generation of phenyl ester groups. The reaction mechanism has also changed from acidolysis to phenololysis. The purity of the product after

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Examples

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Example Embodiment

[0027] The preparation method of the high-purity LCP material of the present application comprises the following steps:

[0028] S1: Acetylation of HBA and HNA

[0029] Add HBA / HNA, acetic anhydride and catalyst A into the reaction vessel, raise the temperature to 140°C, pass through protective nitrogen gas and start stirring, the stirring speed is 200-300rpm, under this condition, HBA / HNA reacts with acetic anhydride to form ester compound, and condensed acetic anhydride to reflux for acetylation reaction, then stop the reaction, transfer the reactant to a container with deionized water, wait for the white crystals to precipitate, and finally wash and dry the white crystals for later use, the white crystals here for ABA / ANA;

[0030] S2: Preparation of high-purity LCP materials

[0031] Add the ABA, ANA and catalyst B prepared in S1 into the reaction vessel, transfer the reaction vessel to the salt bath and pass nitrogen to remove the air in the system, raise the temperatur...

Example Embodiment

[0043] Example 1:

[0044] S1: Acetylation of HBA and HNA

[0045]P-hydroxybenzoic acid (HBA) and acetic anhydride with a molar ratio of 1:2 were added to the three-necked flask, and the catalyst zinc acetate of 0.05% mass fraction was added simultaneously; Turn on stirring at a stirring speed of 300rpm / min, keep warm at this temperature for 2h to carry out the acetylation reaction, transfer it to a beaker with deionized water after the reaction, wait for the crystals to precipitate, and finally wash and dry the precipitated crystals (ABA) for later use .

[0046] Add 2-hydroxy-6-naphthoic acid (HNA) and acetic anhydride with a molar ratio of 1:2 into the three-necked flask, and at the same time add 0.05% mass fraction of the catalyst 1-methylimidazole; raise the temperature to react in the three-necked flask The temperature of the system reaches 140°C and the stirring is started at the same time. The stirring speed is 300rpm / min. The acetylation reaction is carried out at t...

Example Embodiment

[0049] Example 2:

[0050] S1: Acetylation of HBA and HNA

[0051] P-hydroxybenzoic acid (HBA) and acetic anhydride with a molar ratio of 1:3 were added into the there-necked flask, and the catalyst zinc acetate of 0.08% mass fraction was added simultaneously; Turn on the stirring, the stirring speed is 300rpm / min, keep warm at this temperature for 3h to carry out the acetylation reaction, transfer it to a beaker with deionized water after the reaction, wait for the crystals to precipitate, and finally wash and dry the precipitated crystals (ABA) for later use .

[0052] Add 2-hydroxy-6-naphthoic acid (HNA) and acetic anhydride with a molar ratio of 1:3 into the three-necked flask, and at the same time add 0.08% mass fraction of the catalyst 1-methylimidazole; raise the temperature to react in the three-necked flask The temperature of the system reaches 140°C and the stirring is started at the same time. The stirring speed is 300rpm / min. The acetylation reaction is carried o...

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Abstract

The invention relates to the technical field of liquid crystal polymers, in particular to a preparation method of a high-purity LCP material. The LCP material is prepared through a two-step method. Firstly, a specific catalyst is added to enable HBA/HNA and acetic anhydride to be subjected to a collaborative optimization reaction, so that complete acetylation of HBA/HNA is guaranteed to the maximum extent. Then, the ABA, ANA and catalyst after acetylation and the reaction conditions are controlled, and the purity of TLCP is improved by synergistically optimizing process parameters, so that the prepared LCP material is excellent in comprehensive performance and can better meet application requirements. In addition, the preparation method disclosed by the invention is simple in overall process and easy to operate, meets the requirements of large-batch production and manufacturing, and has a good application prospect.

Description

technical field [0001] The invention relates to the technical field of liquid crystal polymers, in particular to a preparation method of a high-purity LCP material. Background technique [0002] LCP (Liquid Crystal Polymer, liquid crystal polymer) is a kind of polymer between solid and liquid. It is a new type of polymer material, which has both the anisotropy of crystal and the fluidity of liquid. According to the physical conditions of the liquid crystal phase, LCP materials can be divided into thermotropic liquid crystal polymers (TLCP) and lyotropic liquid crystal polymers (LLCP). Liquid crystal polyesters are based on p-hydroxybenzoic acid (HBA) and 2-hydroxy- Synthesized from 6-naphthoic acid (HNA) as the main monomer, it is a typical thermotropic liquid crystal polymer (TLCP), with its unique high strength, high modulus, high heat-resistant temperature and unique rheological properties and The excellent electrical properties have attracted widespread attention from t...

Claims

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Application Information

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IPC IPC(8): C08G63/06C08G63/83C08G63/85C08G63/86C08G63/87C09K19/38
CPCC08G63/065C08G63/823C08G63/83C08G63/87C08G63/85C08G63/866C09K19/3809C08G2250/00
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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