Method of producing liquid crystal polyester

A technology of liquid crystal polyester and a manufacturing method, which is applied to liquid crystal materials, chemical instruments and methods, etc., can solve the problems of difficult continuous production and difficult discharge, and achieve the effect of inhibiting sintering and stable continuous preparation.

Inactive Publication Date: 2013-07-31
SUMITOMO CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, on the other hand, if the molecular weight is increased to a desired molecular weight, since the obtained polymer has a high viscosity, it is difficult to discharge it from the reaction vessel, and there is a problem that continuous production is difficult.

Method used

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  • Method of producing liquid crystal polyester
  • Method of producing liquid crystal polyester
  • Method of producing liquid crystal polyester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1）

[0100] (1) Melt polymerization

[0101] As the polymerization tank, a three-way connecting pipe (ト-type connecting pipe) equipped with a ジムロロート cooling pipe, a nitrogen introduction pipe and a thermocouple for measuring the internal temperature, an anchor-type stirring blade, and a A 3-liter four-necked separable flask with a thermocouple on the outside of the flask. 1176.8g (8.52 moles) of 4-hydroxybenzoic acid, 654.9g (3.48 moles) of 6-hydroxy-2-naphthoic acid and 1347.6g (13.2 moles) of acetic anhydride were put into the polymerization tank. The external temperature of the flask was raised to 150° C. by a resistance heater, and the acetylation reaction was carried out under reflux for about 3 hours while stirring at 200 rpm. After the acetylation reaction was completed, the temperature was raised to 280° C. at a rate of 0.6° C. / min. During this period, the by-produced acetic acid in the polycondensation reaction was continuously distilled off. After reaching 280° C., stir...

Embodiment 2）

[0106] Prepolymer powder 2 was obtained in the same manner as in Example 1 except that the retention time at 280° C. during melt polymerization was 40 minutes. When the flow start temperature of the prepolymer powder 2 was measured, it was 228°C.

[0107] The obtained prepolymer powder 2 was subjected to solid-state polymerization in the same manner as in Example 1 to obtain a liquid crystal polyester 2 having a flow initiation temperature of 269°C.

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Abstract

A method is provided of producing a liquid crystal polyester, including: preparing a liquid crystal polyester prepolymer containing a repeating unit represented by general formula (1) and a repeating unit represented by general formula (2) by melt polymerization, cooling and solidifying the prepolymer to obtain a solidified prepolymer, pulverizing the solidified prepolymer to obtain a prepolymer powder, and heating the prepolymer powder to conduct solid-phase polymerization. A liquid crystal polyester is thereby prepared having a polymerization degree higher than the prepolymer. Preparing a liquid crystal polyester is performed with a rate of temperature rise within a temperature range of from a temperature 10 DEG C. lower than a final end-point temperature of the solid-phase polymerization to the final end-point temperature of from 0.01 DEG C. / min to 0.03 DEG C. / min.

Description

technical field [0001] The present invention relates to a method for producing liquid crystal polyester. [0002] This application claims the priority based on Japanese Patent Application No. 2012-018941 for which it applied to Japan on January 31, 2012, and uses the content here. Background technique [0003] Liquid crystal polyester resins exhibiting liquid crystallinity when melted are excellent in heat resistance and processability, and thus are used in various application fields. [0004] Liquid crystal polyesters are obtained by polycondensing the corresponding monomers, that is, aromatic hydroxycarboxylic acids or ester compounds. When the molecular weight of the obtained liquid crystal polyester is increased, the mechanical strength can be improved, and it can be used suitably for various applications. On the other hand, however, if the molecular weight is increased to a desired molecular weight, since the obtained polymer has a high viscosity, it is difficult to d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/06C08G63/80C09K19/38
CPCC09K19/38C09K19/3809C08G63/78C08G63/06C09K19/46
Inventor 大友新治古高英浩
Owner SUMITOMO CHEM CO LTD
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