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Preparation method of novel thermotropic liquid crystal high-performance polyarylester film

A technology of thermotropic liquid crystal and polyarylate, applied in the field of preparation of new type of thermotropic liquid crystal high-performance polyarylate film, can solve the problems of long production cycle, unsuitable for large-scale continuous production, etc. The effect of unstable product quality and shortened production cycle

Active Publication Date: 2020-05-22
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

[0017] 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 polymer obtained above was kneaded...

Embodiment 2

[0019] 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 polymer obtained above was kneade...

Embodiment 3

[0021]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

The invention provides a preparation method of a novel thermotropic liquid crystal high-performance polyarylester film. The preparation method comprises the specific steps of preparing prepolymer of thermotropic liquid crystal polyarylester in a hastelloy alloy polymerizing reactor through melt polycondensation, wherein the intrinsic viscosity of the prepolymer is 1.0-2.8 dl / g; discharging the prepolymer from the hastelloy alloy polymerizing reactor, and preparing high-molecular-weight thermotropic liquid crystal polyarylester through crushing and solid phase polycondensation, wherein the intrinsic viscosity of the high-molecular-weight thermotropic liquid crystal polyarylester is 6.0-9.5 dl / g, and the weight-average molecular weight is 4.5*10<4>-8.0*10<4>; conducting mixing on the obtained polymer through a double-screw extruder, conducting air exhausting, enabling the polymer to pass through a metering pump and an assembly, conducting cross air blowing cooling, and then conducting drafting and winding to obtain a high-strength polyarylester film, wherein the tensile strength of the initial film can reach up to 0.2-0.3 GPa; and conducting heat treatment to obtain the finished filmof which the tensile strength can reach up to 0.4-0.5 GPa. The preparation method is simple in operation. Reaction conditions are easy to control. The molecular weight of the prepared thermotropic liquid crystal polyarylester is high, and continuous production can be realized. The problems that an original thermotropic liquid crystal polyarylester preparation method is complex in step, conditionsare not easy to control, the quality is unstable and the strength of the finished film is low are solved.

Description

technical field [0001] The invention relates to a preparation method of a novel thermotropic liquid crystal high-performance polyarylate film, specifically [0002] First prepare the prepolymer of thermotropic liquid crystal polyarylate by melt polycondensation in the Hastelloy polymerizer, the intrinsic viscosity of the prepolymer is 1.0-2.8dl / g, and then discharge the prepolymer through the Hastelloy polymerizer , after pulverization 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...

Claims

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Application Information

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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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