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Preparation method of a novel thermotropic liquid crystal high-performance polyarylate film

A technology of thermotropic liquid crystal and polyarylate, applied in a new field, can solve the problems of long production cycle, unsuitable for large-scale continuous production, etc., achieve sufficient material contact, overcome unstable product quality, and shorten production cycle Effect

Active Publication Date: 2021-11-12
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

However, this method obviously has the problem that the production cycle is too long, and it is not suitable for industrialized large-scale continuous production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Put 69g of p-hydroxybenzoic acid and 254g of 2-(3-hydroxyphenyl)-6-carboxybenzimidazole, 310g of acetic anhydride and 3.5g of 4-ethylaminopyridine into a 2L Hastelloy polymerization kettle, between 120°C Keep for 5 hours; heat up to 310°C at a rate of 0.5°C / min, keep warm for 2 hours, fill the polymerization tank with 0.2MPa nitrogen, and release the prepolymer through a 10-hole discharge valve with a diameter of 3mm, crush it, and pass through a 20-mesh sieve , After drying at 130°C for 2h, the prepolymer was obtained. The intrinsic viscosity of the prepolymer is 1.1dl / g, and then the prepolymer is discharged through the Hastelloy polymerizer, crushed, and the nitrogen flow rate is 0.3m 3 Under the condition of 190℃, 48 hours of solid-state polycondensation in a rotary kiln under the condition of 190℃, a high-weight polymer powder was obtained. Its intrinsic viscosity is 6.1dl / g, and its weight average molecular weight is 43800. The high molecular weight polymer powd...

Embodiment 2

[0017] Put 138g of p-hydroxybenzoic acid and 254g of 2-(3-hydroxyphenyl)-6-carboxybenzimidazole, 410g of acetic anhydride and 4.5g of 4-ethylaminopyridine into a 2L Hastelloy polymerization kettle, between 120°C Keep for 5 hours; heat up to 310°C at a rate of 0.5°C / min, keep warm for 2 hours, fill the polymerization tank with 0.2MPa nitrogen, and release the prepolymer through a 10-hole discharge valve with a diameter of 3mm, crush it, and pass through a 20-mesh sieve , After drying at 130°C for 2h, the prepolymer was obtained. The intrinsic viscosity of the prepolymer is 2.1dl / g, and then the prepolymer is discharged through the Hastelloy polymerizer, crushed, and the nitrogen flow rate is 0.3m 3 Under the condition of 190℃, 48 hours of solid-state polycondensation in a rotary kiln under the condition of 190℃, a high-weight polymer powder was obtained. Its intrinsic viscosity is 6.5dl / g, and its weight average molecular weight is 48200. The high molecular weight polymer pow...

Embodiment 3

[0019]Put 276g of p-hydroxybenzoic acid and 254g of 2-(3-hydroxyphenyl)-6-carboxybenzimidazole, 612g of acetic anhydride and 6.9g of 4-ethylaminopyridine into a 2L Hastelloy polymerization kettle, and heat it at 120°C Keep the temperature for 5 hours; raise the temperature to 310 ℃ at a speed of 0.5 ℃ / min, and after 2 hours of heat preservation, fill the polymerization kettle with 0.2MPa nitrogen gas, and the prepolymer is discharged through a 10-hole discharge valve with a diameter of 3 mm, crushed, and passed through 20 mesh Sieve and dry at 130°C for 2 hours to obtain a prepolymer. The intrinsic viscosity of the prepolymer is 2.3dl / g, and then the prepolymer is discharged through the Hastelloy polymerizer, crushed, and the nitrogen flow rate is 0.3m 3 Under the condition of 190℃, 48 hours of solid-state polycondensation in a rotary kiln under the condition of 190℃, a high-weight polymer powder was obtained. Its intrinsic viscosity is 8.1dl / g, and its weight average molecul...

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Abstract

A method for preparing a novel thermotropic liquid crystal high-performance polyarylate film. Specifically, the prepolymer of thermotropic liquid crystal polyarylate is prepared by melt polycondensation in the Hastelloy polymerization kettle. The intrinsic viscosity of the prepolymer is 1.0-2.8dl / g, and then the prepolymer is polymerized by Hastelloy After being discharged from the kettle, after crushing and solid-state polycondensation, a high-molecular-weight thermotropic liquid crystal polyarylate is prepared, with an intrinsic viscosity of 6.0-9.5dl / g and a weight-average molecular weight of 4.5×10 4 ~8.0×10 4 . The obtained polymer is kneaded by a twin-screw extruder, exhausted, cooled by metering pumps and components, side blown, drawn, and wound to obtain a high-strength polyarylate film. The tensile strength of the obtained nascent film can reach 0.2 ‑0.3GPa, and the tensile strength of the finished film after heat treatment can reach 0.4‑0.5GPa. The method is simple to operate, and the reaction conditions are easy to control. The prepared thermotropic liquid crystal polyarylate has high molecular weight and can be continuously produced, which solves the problem of cumbersome preparation steps of thermotropic liquid crystal polyarylate in the past. The disadvantage of low film strength.

Description

technical field [0001] The invention relates to a method for preparing a novel thermotropic liquid crystal high-performance polyarylate film, specifically preparing a thermotropic liquid crystal polyarylate prepolymer through melt polycondensation in a Hastelloy polymerization kettle. The intrinsic viscosity is 1.0-2.8dl / g, and then the prepolymer is discharged through the Hastelloy polymerizer, crushed, and solid-state polycondensed to prepare a high-molecular-weight thermotropic liquid crystal polyarylate, and its intrinsic viscosity is 6.0-9.5 dl / g, the weight average molecular weight is 4.5×10 4 ~8.0×10 4 . The obtained polymer is kneaded by a twin-screw extruder, exhausted, cooled by metering pumps and components, side blown, drawn, and wound to obtain a high-strength polyarylate primary film. The tensile strength of the obtained primary film can reach 0.2-0.3GPa, and the tensile strength of the finished film after heat treatment can reach 0.4-0.5GPa. The method is si...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B29C48/08C08G63/685C08G63/87C08G63/80
CPCC08G63/6852C08G63/80C08G63/87
Inventor 王阳王卉
Owner 宁波聚嘉新材料科技有限公司
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