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Solid phase tackifying method of liquid crystal polymer

A technology of liquid crystal polymers and solid phase viscosity increase, which is applied in the direction of liquid crystal materials, chemical instruments and methods, etc., can solve the problems affecting the rheological properties of TLCP, the color of TLCP turns yellow, and limit the application of TLCP, so as to achieve good heat and mass transfer Good effect, increase molecular weight, good color performance

Active Publication Date: 2019-05-03
KINGFA SCI & TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These small molecular products make the color of TLCP yellow, and at the same time, it is easy to cause branching of linear molecular chains, which affects the rheological properties of TLCP and limits the application of TLCP in many fields.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] A kind of embodiment of the solid-phase thickening method of liquid crystal polymer of the present invention comprises the following steps:

[0051] (1) Preparation of TLCP prepolymer

[0052] In a reaction kettle equipped with a stirrer, a thermometer, a nitrogen inlet pipe and a reflux condensing device, add 979.83kg of monomer p-hydroxybenzoic acid, 440.32kg of 4,4'-biphenyldiphenol, 294.63kg of terephthalic acid, Isophthalic acid 98.21kg, and adding acetic anhydride 1271.19kg is that acylating agent and 1-methylimidazole 2.07kg are catalyzer; Then nitrogen is fed into the reactor to replace; Heating from room temperature to 150°C, reflux at this temperature for 2 hours; then continue to heat up, and heat the mixture from 150°C to 320°C for 3 hours, during which unreacted acetic anhydride and by-product acetic acid are evaporated; final polycondensation stage , decompress the reaction system, and judge the key point of the end of the reaction by observing the increa...

Embodiment 2

[0057] A kind of embodiment of the solid-phase thickening method of liquid crystal polymer of the present invention comprises the following steps:

[0058] (1) Preparation of TLCP prepolymer

[0059] In a reaction kettle equipped with a stirrer, a thermometer, a nitrogen inlet pipe and a reflux condensing device, add 627.78 kg of monomer 6-hydroxy-2-naphthoic acid, 428.55 kg of hydroquinone, 323.29 kg of terephthalic acid, 2,6 -naphthalene dicarboxylic acid 420.71kg, and adding 569.32kg of acetic anhydride is that acylating agent and 1.8kg of 1-methylimidazole are catalyzer; Then nitrogen is passed into the reactor to replace; Heating from room temperature to 140°C, reflux at this temperature for 1 hour; then continue to heat up, and heat the mixture from 140°C to 300°C over 2 hours, during which unreacted acetic anhydride and by-product acetic acid are evaporated; final polycondensation stage , decompress the reaction system, and judge the key point of the end of the reactio...

Embodiment 3

[0064] A kind of embodiment of the solid-phase thickening method of liquid crystal polymer of the present invention comprises the following steps:

[0065] (1) Preparation of TLCP prepolymer

[0066] In a reaction kettle equipped with a stirrer, a thermometer, a nitrogen inlet pipe and a reflux condensing device, add 1605.14 kg of monomer p-hydroxybenzoic acid, 120.22 kg of 2,6-naphthalenediol, 53.63 kg of terephthalic acid, and isophthalic acid Diformic acid 53.63kg, and adding acetic anhydride 7933.22kg is an acylating agent and 1-methylimidazole 54.44kg is a catalyst; Then nitrogen is passed into the reactor for replacement; Start stirring, and the reaction mixture is heated by room temperature in a nitrogen stream to 160°C, reflux at this temperature for 3 hours; then continue to heat up, and heat the mixture from 160°C to 350°C over 4 hours, during which unreacted acetic anhydride and by-product acetic acid are distilled off; final polycondensation stage, for The reactio...

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Abstract

The invention relates to a solid phase tackifying method of a liquid crystal polymer, and belongs to the technical field of special engineering plastics. The solid phase tackifying method of the liquid crystal polymer comprises the following steps: (1) carrying out acetylation reaction on a hydroxyl-containing aromatic monomer and acetic anhydride in a first reactor; (2) transferring the acetylated reactant into a second reactor, and carrying out melt polycondensation on the acetylated reactant and an aromatic diacid monomer so as to obtain a prepolymer; (3) crushing and granulating to obtainprepolymer powder; and (4) vacuumizing a solid-phase tackifying reactor, filling a protective gas, and carrying out solid-phase tackifying on the prepolymer powder. According to the solid phase tackifying method disclosed by the invention, side reactions in the tackifying process of the thermotropic liquid crystal polymer can be inhibited, and the generation of small molecule by-products and branched chains is reduced, so that the molecular weight of the product is effectively improved, and the darkening of the color of the product due to the by-products is avoided; the original chromaticity value of the liquid crystal polymer can be maintained while tackifying, yellowing is not easy, and the color performance is good.

Description

technical field [0001] The invention relates to a solid-phase thickening method for liquid crystal polymers, belonging to the technical field of special engineering plastics. Background technique [0002] Thermotropic liquid crystal polymer (TLCP) has a high melting point and high melt viscosity. Its synthesis often adopts a two-step method: first, a low-molecular-weight prepolymer is synthesized by melt polymerization, and then passed through drums and other equipment, at a temperature lower than its melting point. The temperature of solid phase viscosity increase to obtain high molecular weight products. The disadvantage of using drums for viscosification is that the heat transfer is not uniform, resulting in large differences in viscosification effects between pellets, and uneven performance of the same batch of products; at the same time, the drum production cycle is long and consumes a lot of energy, which increases The production cost of the product. [0003] During ...

Claims

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Application Information

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IPC IPC(8): C08G63/60C08G63/78C08J3/00C09K19/38C08G67/00
Inventor 谢沛乐肖中鹏邢羽雄罗德彬许伯荣唐钜成曹民姜苏俊
Owner KINGFA SCI & TECH CO LTD