Liquid crystal polyester and its preparation method and use

A technology of liquid crystal polyester and polycondensation reaction, which is applied in the direction of liquid crystal materials, chemical instruments and methods, etc., can solve the problems of synthetic liquid crystal polyester, etc., and achieve excellent melt processing performance, good fluidity, excellent melt processing performance and mechanical properties performance effect

Active Publication Date: 2013-04-03
KINGFA SCI & TECH CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] There is no report on the synthesis of liquid crystal polyester using bisphenol fluorene and its derivatives as monomers

Method used

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  • Liquid crystal polyester and its preparation method and use
  • Liquid crystal polyester and its preparation method and use
  • Liquid crystal polyester and its preparation method and use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) Synthesis of prepolymer

[0045] with N 2 In the gas inlet, condenser and the reactor with a stirrer with a stirring power display, the raw material monomer, catalyst and acylating agent are added in sequence after nitrogen replacement three times,

[0046] Raw material monomer: p-hydroxybenzoic acid (HBA) 690.6g (5mol);

[0047] Biphenol (BP) 372.5g (2mol);

[0048] 9,9-bis(4-hydroxyphenyl)fluorene (BHPF) 175.2g (0.5mol);

[0049] Terephthalic acid (TA) 207.7g (1.25mol);

[0050] Isophthalic acid (IA) 207.7g (1.25mol);

[0051]Acylating agent: acetic anhydride 1235.3g (12.1mol);

[0052] Catalyst: 0.413 g of magnesium acetate.

[0053] After loading the raw materials, the temperature of the reaction system was raised to 145° C. for reflux reaction for 3 hours; then the temperature was raised to 305° C. within 150 minutes, and the reaction was kept at this temperature for 30 minutes. Then raise the temperature to 325°C and react for 30 minutes, then replace t...

Embodiment 2

[0057] (1) Synthesis of prepolymer

[0058] Add 828.8g (6mol) of HBA, 186.3g (1mol) of BP, 350.4g (1mol) of BHPF, 166.1g (1mol) of TA, 166.1g (1mol) of IA, 1235.3g (12.1mol) of acetic anhydride and 0.425g of magnesium acetate Into the reactor, raise the temperature of the reaction system to 145°C for reflux reaction for 4 hours; then raise the temperature to 305°C within 150 minutes, and keep the reaction at this temperature for 30 minutes. Then raise the temperature to 360°C and react for 3 hours, then replace the condenser with a vacuum device, and slowly increase the vacuum degree to polymerize to a predetermined level of torque. Then replace with nitrogen. Take out the prepolymer and pulverize it with a universal pulverizer to obtain a granular prepolymer.

[0059] (2) Solid phase polymerization

[0060] The prepolymer was vacuum-dried at 120°C for 2 hours, then added to a device capable of drawing a high vacuum, heated to 300°C, and reacted for 4.5 hours under the cond...

Embodiment 3

[0062] (1) Synthesis of prepolymer

[0063] HBA 828.8g (6mol), BP 279.5g (1.5mol), BHPF 175.2g (0.5mol), TA 249.2g (1.5mol), IA 83.1g (0.5mol), acetic anhydride 1235.3g (12.1mol) and acetic acid Add 0.404 g of magnesium into the reactor, raise the temperature of the reaction system to 140° C. for reflux reaction for 6 hours; then raise the temperature to 305° C. within 150 minutes, and keep the reaction at this temperature for 30 minutes. Then raise the temperature to 355°C and react for 2.5 hours, then replace the condenser with a vacuum device, and slowly increase the vacuum degree to polymerize to a predetermined level of torque. Then replace with nitrogen. Take out the prepolymer and pulverize it with a universal pulverizer to obtain a granular prepolymer.

[0064] (2) Solid phase polymerization

[0065] The prepolymer was vacuum-dried at 120°C for 2 hours, then added to a device capable of drawing a high vacuum, heated to 300°C, and reacted at 80Pa for 3 hours to obtai...

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Abstract

The invention belongs to the field of material engineering and discloses a liquid crystal polyester and its preparation method and use. The liquid crystal polyester is obtained by a condensation polymerization reaction of p-hydroxybenzoic acid, biphenol, diphenol with a fluorene skeleton and aromatic dicarboxylic acid. A unit with a fluorene skeleton side group is introduced into a chain structure of the liquid crystal polyester so that the liquid crystal polyester has a melting temperature of 310 to 360 DEG C, good fluidity and excellent melting processing performances.

Description

technical field [0001] The invention belongs to the field of material engineering, and in particular relates to a liquid crystal polyester and its preparation method and application. Background technique [0002] In 1959, Caldwell et al. used the acetate of p-hydroxybenzoic acid to obtain a polymer with liquid crystal properties through melt polymerization, but its melting temperature was very high, even exceeding its decomposition temperature. Therefore, p-hydroxybenzoic acid is usually copolymerized with aromatic diols and aromatic diacids to lower the melting temperature to a certain extent for processing. Commonly used comonomers include monomers with different lengths, parallel offset monomers, Substituent-containing monomers, flexible monomers, etc. [0003] Carborundum Company (US3637595 and US3975487) and Sumitomo of Japan both adopt p-hydroxybenzoic acid (HBA), hydroquinone (HQ), terephthalic acid (TA) / isophthalic acid (IPA) and biphenol (BP) copolymerization Prep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/60C08G63/80C09K19/38
Inventor 肖中鹏曹民罗湘安曾祥斌蔡彤旻姜苏俊姚程宁凯军
Owner KINGFA SCI & TECH CO LTD
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