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Thermotropic liquid crystal polyester with stable monomer composition ratio and its preparation method and application

A liquid crystal polyester and thermotropic technology, which is applied in the field of liquid crystal polyester, can solve the problems of large performance differences, unstable structure of liquid crystal polyester products, and the inability of monomers or oligomers to return to the reaction system, etc. The loss of body and the effect of stabilizing the ratio of monomer composition

Inactive Publication Date: 2019-05-07
SUN YAT SEN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the above preparation process, with the extraction of acetic acid and other by-products, some monomers or oligomers are taken out and cannot return to the reaction system
Due to the loss of monomers, the product structure (monomer composition ratio) of the final liquid crystal polyester is unstable, and the performance varies greatly

Method used

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  • Thermotropic liquid crystal polyester with stable monomer composition ratio and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Add the following monomer raw materials, acylating agent, and catalyst to a reaction vessel equipped with a stirrer, a monomer feeding port, a reflux condenser, a thermometer, a nitrogen gas inlet, and a torque sensor.

[0050] 4-Hydroxybenzoic acid (HBA) 10.08kg (73mmol),

[0051] 6-Hydroxy-2-naphthoic acid (HNA) 5.08kg (27mmol),

[0052] Catalyst: Magnesium acetate 150 mg,

[0053]After the feeding was completed, the atmosphere in the reaction vessel was completely replaced with nitrogen, and the temperature of the reaction system was raised to 120°C under the protection of nitrogen, and the acetylation reaction was carried out at this temperature for 3 hours under reflux. After the acetylation reaction is over, increase the nitrogen pressure, keep the pressure of the reaction system at 1.5MPa and raise the temperature to 270°C, and release the pressure to normal pressure after continuing the reaction for 1 hour, and discharge the acetic acid and unreacted acetic anh...

Embodiment 2

[0057] Add the following monomer raw materials, acylating agent, and catalyst to a reaction vessel equipped with a stirrer, a monomer feeding port, a reflux condenser, a thermometer, a nitrogen gas inlet, and a torque sensor.

[0058] 4-Hydroxybenzoic acid (HBA) 10.08kg (73mmol),

[0059] 6-Hydroxy-2-naphthoic acid (HNA) 5.08kg (27mmol),

[0060] Catalyst: Magnesium acetate 150 mg,

[0061] After the feeding was completed, the atmosphere in the reaction vessel was completely replaced with nitrogen, and the temperature of the reaction system was raised to 120°C under the protection of nitrogen, and the acetylation reaction was carried out at this temperature for 3 hours under reflux. After the acetylation reaction is over, increase the nitrogen pressure, keep the pressure of the reaction system at 1.5 MPa and raise the temperature to 280°C, and release the pressure to normal pressure after continuing the reaction for 1 hour, and discharge the acetic acid and unreacted acetic a...

Embodiment 3

[0065] Add the following monomer raw materials, acylating agent, and catalyst to a reaction vessel equipped with a stirrer, a monomer feeding port, a reflux condenser, a thermometer, a nitrogen gas inlet, and a torque sensor.

[0066] 4-Hydroxybenzoic acid (HBA) 10.08kg (73mmol),

[0067] 6-Hydroxy-2-naphthoic acid (HNA) 5.08kg (27mmol),

[0068] Catalyst: Magnesium acetate 150 mg,

[0069] After the feeding was completed, the atmosphere in the reaction vessel was completely replaced with nitrogen, and the temperature of the reaction system was raised to 120°C under the protection of nitrogen, and the acetylation reaction was carried out at this temperature for 3 hours under reflux. After the acetylation reaction is over, increase the nitrogen pressure, keep the pressure of the reaction system at 1.5MPa and raise the temperature to 290°C, and release the pressure to normal pressure after continuing the reaction for 1 hour, and discharge the acetic acid and unreacted acetic an...

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Abstract

The invention provides thermotropic liquid crystal polyester with a stable monomer composition ratio, and a preparation method and application thereof. The preparation method is characterized in that a monomer is subjected to melt phase polycondensation under a pressure maintaining condition to obtain a prepolymer, and the prepolymer is subjected to solid phase polymerization to obtain the liquid crystal polyester. According to the preparation method, the losses of the monomer in a polymerization process are lowered, and the thermotropic liquid crystal polyester with the stable monomer composition ratio is obtained. The element content of the thermotropic liquid crystal polyester basically keeps consistent with a theoretical content through elemental assay determination, and the monomer composition ratio is basically kept constant.

Description

technical field [0001] The invention relates to the technical field of liquid crystal polyesters, in particular to a liquid crystal polyester with a stable monomer composition ratio and its preparation method and application. Background technique [0002] As a high-performance special engineering plastic, thermotropic liquid crystal polymer (TLCP) has excellent mechanical properties, good fluidity, heat resistance, chemical corrosion resistance, flame retardancy and electrical insulation properties, and is currently used in electronic and electrical components and other fields are widely used. [0003] The method for preparing liquid crystal polyester usually includes the following steps: (1) acetylating the reaction monomer under the action of an acetylating reagent in a reaction vessel. (2) Raise the temperature to polycondense the monomer, discharge the produced polymer from the reaction vessel in a molten state, and solidify it; (3) conduct solid-state polymerization of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/06C08G63/78C09K19/38
CPCC08G63/065C08G63/78C09K19/38
Inventor 孙华伟池振国宋彩飞曹民姜苏俊曾祥斌蔡彤旻
Owner SUN YAT SEN UNIV
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