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Method for producing liquid crystal polyester

A technology of liquid crystal polyester and prepolymer, applied in the direction of liquid crystal materials, chemical instruments and methods, etc., can solve problems such as unsatisfactory preparation methods, and achieve the effect of improving productivity

Inactive Publication Date: 2013-01-02
SUMITOMO CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, none of the above production methods is satisfactory from the viewpoint of improving productivity by shortening the production time (polymerization time) of liquid crystal polyester

Method used

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  • Method for producing liquid crystal polyester
  • Method for producing liquid crystal polyester

Examples

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preparation example Construction

[0016] Typical examples of liquid crystal polyesters prepared by the preparation method of the present invention include:

[0017] (I) Liquid crystal polyesters obtained by polycondensation of aromatic hydroxycarboxylic acids, aromatic dicarboxylic acids and / or aromatic diols;

[0018] (II) Liquid crystal polyester obtained by polycondensation of various aromatic dicarboxylic acids;

[0019] (III) A liquid crystalline polyester obtained by polymerizing a polyester such as polyethylene terephthalate with an aromatic hydroxycarboxylic acid.

[0020] Here, part or all of the aromatic hydroxycarboxylic acid, the aromatic dicarboxylic acid, and the aromatic diol may each independently become a polymerizable derivative thereof.

[0021] Examples of polymerizable derivatives of compounds having a carboxyl group such as aromatic hydroxycarboxylic acids and aromatic dicarboxylic acids include derivatives (esters) in which a carboxyl group is converted into an alkoxycarbonyl group or a...

Embodiment 1

[0104] In a polymerization tank having a volume of 200 L and an inner diameter of 600 mm equipped with a stirrer, a nitrogen introduction device, a thermometer, and a reflux condenser, 33.1 kg (0.322 kmol) of acetic anhydride was charged under a nitrogen atmosphere. Then add 27.9 kg (0.148 kmol) of 2-hydroxy-6-naphthoic acid, 7.4 kg (0.067 kmol) of hydroquinone, 2.2 kg (0.013 kmol) of terephthalic acid, 10.2 kg (0.047 kmol) of 2 , 6-naphthalene dicarboxylic acid and 4.8 g of 1-methylimidazole as acetylation catalyst. Then the temperature was raised to 140°C under nitrogen flow, and the reaction mixture was refluxed at a temperature of 137°C-140°C for 1 hour.

[0105] Pressurize the inside of the polymerization tank to 1kg / cm with nitrogen 2 , while transferring the reaction mixture to a 100 L polymerization vessel, then the temperature of the polymerization vessel was raised to 350° C. over 4 hours while distilling off acetic acid and unreacted acetic anhydride, and the react...

Embodiment 2

[0111] The interval between the belts of the double-belt cooler of Example 1 was adjusted to obtain a sheet having an almost uniform thickness of 2.0 mm as a whole, and the sheet was pulverized in the same manner as in Example 1 to obtain a bulk density of 0.41 g / cc of powder crushed products.

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Abstract

Disclosed is a method for producing a liquid crystal polyester, which includes the following steps of: (1) melt-polycondensing a compound as a monomer in a polymerization tank to produce a prepolymer; (2) discharging the prepolymer from the polymerization tank in a molten state, and solidifying the prepolymer through cooling to produce a sheet in which a portion having a thickness of 1.6 to 2 mm accounts for 80% by mass or more (of 100% by mass of the entire sheet); (3) crushing the sheet; and (4) subjecting the crushed product to solid-phase polymerization through heating.

Description

technical field [0001] The invention relates to a method for preparing liquid crystal polyester. Background technique [0002] JP-A-2001-72750 (corresponding application US2003-0088053A) describes a method for preparing liquid crystal polyester with high molecular weight with satisfactory productivity. The method for preparing liquid crystal polyester includes the following steps: (1) polycondensing monomers in a reaction vessel for a short time; (2) discharging the produced polymer in a molten state where the produced polymer can be easily discharged from the reaction vessel, and solidifying the polymer; and (3) making The cured polymer undergoes solid state polymerization to increase molecular weight. [0003] It has been studied that the efficiency of heat transfer can be improved by pulverizing the polymer solidified in step (2), thereby helping to control the degree of polymerization and shorten the polymerization time in step (3). For example, in order to facilitate ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/80C08G63/60C09K19/38
CPCC08G63/605C08G63/80C09K19/3809C08G63/78C08L67/02C09K19/46
Inventor 细田朋也细田英司松原政信
Owner SUMITOMO CHEM CO LTD