Method and system for continuously preparing liquid crystal polymer with adjustable molecular structure

A liquid crystal polymer and molecular structure technology, applied in chemical instruments and methods, chemical/physical processes, chemical/physical/physicochemical processes, etc., can solve problems such as difficulty in continuous production, small specific surface area, and high monomer concentration , to achieve the effects of inhibiting the formation of small molecule by-products and branched chains, enhancing the mass transfer and heat transfer effects, and reducing the acetylation reaction time

Active Publication Date: 2021-01-15
惠生(中国)投资有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high viscosity of the reaction system in the post-melt polycondensation stage, internal parts such as internal coils are usually not used in traditional tank-type polymerization reactors. The heat transfer process mainly depends on the heat transfer of the tank wall, but the specific surface area of ​​the tank-type polymerization reactor is small. The temperature rise rate is slow; at the same time, due to the stirring mode of the polymerization tank reactor, the material is mixed unevenly, especially when the viscosity of the polymerization system rises in the late stage of the reaction, the difficulty of material mixing is further increased, and it is easy to cause the concentration of local monomers to be too high, which will intensify the aroma.

Method used

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  • Method and system for continuously preparing liquid crystal polymer with adjustable molecular structure
  • Method and system for continuously preparing liquid crystal polymer with adjustable molecular structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0138] With p-hydroxybenzoic acid (A) and 2-hydroxy-6-naphthoic acid (B 1 ) as raw material, the continuous preparation of the structural unit is AB 1 AB 1 type liquid crystal polymers.

[0139] Such as figure 1 138.13g of p-hydroxybenzoic acid, 0.11g of potassium acetate and 204g of acetic anhydride are added to the first raw material dissolving device 8, and after the materials are dissolved, they are introduced into the first multi-stage micro-reaction device 1 through an advection pump for acetylation reaction. The stage micro-reaction device 1 includes a plurality of microreactors connected in series. The reaction time of materials in each stage of microchannels is gradually shortened, the heating temperature is gradually increased, and the propulsion rate of the advection pump is controlled at 100-120ml / min. The residence time in the micro-reaction device 1 is controlled to be 10-20s, and the reaction temperature is controlled to be 130-140°C; The heating temperature...

Embodiment 2

[0145] With p-hydroxybenzoic acid (A) and 2-hydroxy-6-naphthoic acid (B 1 ) as raw material, the continuous preparation of the structural unit is AAAB 1 AAAB 1 type liquid crystal polymers.

[0146] Such as figure 1 138.13g of p-hydroxybenzoic acid, 0.11g of potassium acetate and 204g of acetic anhydride are added to the first raw material dissolving device 8, and after the materials are dissolved, they are introduced into the first multi-stage micro-reaction device 1 through an advection pump for acetylation reaction. The stage micro-reaction device 1 includes a plurality of microreactors connected in series. The reaction time of materials in each stage of microchannels is gradually shortened, the heating temperature is gradually increased, and the propulsion rate of the advection pump is controlled at 100-120ml / min. The residence time in the micro-reaction device 1 is controlled to be 10-20s, and the reaction temperature is controlled to be 130-140°C; The heating tempera...

Embodiment 3

[0151] With p-hydroxybenzoic acid (A), hydroquinone (B 2 ) and terephthalic acid (C) as raw materials, the continuous preparation of the structural unit is AAB 2 C-type liquid crystal polymer.

[0152] Such as figure 2 138.13g of p-hydroxybenzoic acid, 0.11g of potassium acetate and 204g of acetic anhydride are added to the first raw material dissolving device 8, and after the materials are dissolved, they are introduced into the first multi-stage micro-reaction device 1 through an advection pump for acetylation reaction. The stage micro-reaction device 1 includes a plurality of micro-reactors connected in series. The reaction time of materials in each stage of micro-channel is gradually shortened, and the heating temperature is gradually increased. The residence time in the first-stage micro-reaction device 1 is controlled to be 10-20s, and the reaction temperature is controlled to be 130-140°C; The heating temperature of the screw extrusion device 3 is controlled at 200-...

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Abstract

The invention relates to the technical field of polymer material preparation, in particular to a method and system for continuously preparing a liquid crystal polymer with a controllable molecular structure. The method at least comprises the following steps: 1) carrying out multistage tandem acetylation reaction and/or pre-polymerization reaction on a first acetylation reaction material to providea first acetylation monomer and/or a prepolymer with a polymerization degree of Xn; 2) carrying out multistage tandem acetylation reaction and/or pre-polymerization reaction on the second acetylationreaction material to provide a second acetylation monomer and/or a prepolymer with a polymerization degree of X'n; and 3) carrying out polymerization reaction on the first acetylated monomer and/or the prepolymer with the polymerization degree of Xn in the step 1) and the second acetylated monomer and/or the prepolymer with the polymerization degree of X'n in the step 2), removing small moleculesand acetic acid in vacuum, and performing extruding and pelletizing to provide the liquid crystal polymer. According to the invention, the molecular structure can be regulated and controlled; and meanwhile, the generation of small molecular by-products and branched chains is inhibited, and the product performance is improved.

Description

technical field [0001] The invention relates to the technical field of polymer material preparation, in particular to a method and system for continuously preparing liquid crystal polymers with adjustable molecular structure. Background technique [0002] Thermotropic liquid crystal polymer (TLCP), as a high-performance special engineering plastic, has a series of excellent properties, such as high strength, outstanding heat resistance, chemical corrosion resistance, small linear expansion coefficient, low hygroscopicity Excellent electrical insulation, etc., are currently more and more widely used in the fields of aerospace, electronic appliances, and small precision thin-walled parts. [0003] Typical steps for preparing thermotropic liquid crystal polymers are usually as follows: [0004] (1) Reaction monomer, acetic anhydride and catalyzer are carried out acetylation reaction in reactor by a certain ratio; [0005] (2) Carry out temperature rise melt polycondensation r...

Claims

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Application Information

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IPC IPC(8): C08G63/06C08G63/78B01J19/00B29C48/00
CPCC08G63/065C08G63/78C08G63/785B01J19/0093B29C48/022
Inventor 高敬民吴煜金纪阳
Owner 惠生(中国)投资有限公司
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