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Preparation method of polyarylester based on 2-(3-hydroxyphenyl)-6-carboxypyridioimidazole

A technology of pyridoimidazole and hydroxyphenyl, which is applied in the field of preparation of polyarylate based on 2-(3-hydroxyphenyl)-6-carboxypyridoimidazole, can solve the problem of difficulty in the preparation of liquid crystal polyarylate. There is a large difference between the tensile strength and the theoretical value, etc., to achieve the effects of convenient continuous production, easy control of reaction conditions, and simple operation

Active Publication Date: 2019-03-29
宁波聚嘉新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a kind of based on 2-(3-hydroxyphenyl)-6-carboxypyridimidazole in order to solve the problems such as the difficulty of preparation of liquid crystal polyarylate, the large difference between the tensile strength and the theoretical value, etc. The preparation method of polyarylate

Method used

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specific Embodiment approach 1

[0011] Specific embodiment one: the preparation method of the thermotropic liquid crystal polyarylate of this embodiment is implemented according to the following steps:

[0012] 1. P-hydroxybenzoic acid, 2-(3-hydroxyphenyl)-6-carboxypyridimidazole, acetic anhydride, 4-aminopyridine and chlorinated chlorinated acid with a molar ratio of (0.4~3.0):1 Add tin into the Hastelloy polymerization kettle, keep it at 120-160°C for 3-6 hours, then raise the temperature to 320°C, keep it warm for 3 hours, fill the Hastelloy polymerization kettle with nitrogen, and discharge it through the Hastelloy polymerization kettle. After crushing and drying, a prepolymer is obtained;

[0013] 2. Place the prepolymer obtained in step 1 under nitrogen protection conditions, and carry out solid-state polycondensation reaction in a rotary kiln at 200-210 ° C to obtain high molecular weight polymer powder;

[0014] 3. Mix the high-molecular-weight polymer powder obtained in step 2 through a single-scre...

specific Embodiment approach 2

[0018] Embodiment 2: This embodiment differs from Embodiment 1 in that the purity of p-hydroxybenzoic acid and 2-(3-hydroxyphenyl)-6-carboxypyridimidazole in step 1 is greater than 99.5%. Other steps and parameters are the same as those in Embodiment 1.

specific Embodiment approach 3

[0019] Specific embodiment three: the difference between this embodiment and specific embodiment one or two is that the molar weight of acetic anhydride in step one is that of polymerized monomer p-hydroxybenzoic acid and 2-(3-hydroxyphenyl)-6-carboxypyrido 1.8 to 2.8 times the total number of moles of hydroxyl groups in imidazole. Other steps and parameters are the same as those in Embodiment 1 or Embodiment 2.

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Abstract

The invention discloses a preparation method of polyarylester based on 2-(3-hydroxyphenyl)-6-carboxypyridioimidazole, relates to the preparation method of polyarylester based on 2-(3-hydroxyphenyl)-6-carboxypyridioimidazole, and solves the problems of difficult preparation and unsatisfactory mechanical properties of liquid crystal polyarylester. The preparation method comprises the steps: 1, adding p-hydroxybenzoic acid with 2-(3-hydroxyphenyl)-6-carboxypyridioimidazole, acetic anhydride, 4-aminopyridine and an antioxidant into a polymerization kettle, and carrying out melt condensation polymerization to obtain a prepolymer of thermotropic liquid crystal polyarylester; 2, placing the prepolymer under a nitrogen gas protection condition, and carrying out solid-state condensation polymerization reaction in a rotary kiln, to obtain high-molecular-weight polymer powder; 3, mixing the high-molecular-weight polymer powder, then cooling, and drawing to obtain primary polyarylester; and 4, carrying out heat treatment of the primary polyarylester. The preparation method of the thermotropic liquid crystal polyarylester fibers is simple to operate, and the tensile strength of the ultimately obtained polyarylester fibers can reach 160-200 MPa.

Description

technical field [0001] The invention relates to a preparation method of polyarylate based on 2-(3-hydroxyphenyl)-6-carboxypyridoimidazole. Background technique [0002] TLCP has excellent properties and a wide range of applications that cannot be compared with conventional polymers, and has attracted the attention of many researchers. Since Jackson reported the first thermotropic liquid crystal polyester in the 1970s, people have launched a large-scale research on thermotropic liquid crystal polyarylate. The preparation methods of thermotropic liquid crystal polyarylates are roughly divided into two categories, one is the acid chloride method, that is, adding dibasic acid chlorides, dihydric phenols and corresponding catalysts into an organic solvent for reaction to prepare thermotropic liquid crystal polyarylates. The second type is the melt ester polycondensation method. The dibasic acid or dihydric phenol is first reacted with a small molecule monohydric alcohol or acid ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/685C09K19/38
CPCC08G63/6852C09K19/3809C09K19/3823
Inventor 郭继磊王丹李楠蒲海建
Owner 宁波聚嘉新材料科技有限公司
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