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A kind of short process preparation method of thermotropic liquid crystal polyarylate nanofibrils

A polyarylate and thermotropic technology, which is applied in the field of preparation of thermotropic liquid crystal polyarylate nano-fibrils, can solve the problem of high molecular weight thermotropic liquid crystal polyarylate spinning forming process and fiber spinning processing equipment High precision requirements, narrow processing window temperature and other issues, to achieve the effect of easy substrate contact, environmental protection and continuous production, and conducive to mold filling

Active Publication Date: 2016-06-08
WUHAN TEXTILE UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method has complex spinning process, long process and special requirements for equipment
Chinese Patent Publication No. CN102071493A, published on May 25, 2011, the title of the invention is "A Method for Preparation of Thermotropic Liquid Crystal Polyarylate Fiber", the application provides a low molecular weight thermotropic liquid crystal polyarylate fiber The high-viscosity thermotropic liquid crystal polyarylate spinning method aims to effectively improve the rheological behavior of the system, widen the processing temperature range, and effectively solve the processing window encountered in the spinning of thermotropic liquid crystal polyarylate slices Narrow temperature and high precision requirements for fiber spinning processing equipment
In this application, the main problem to be solved is that the spinning and forming process of high-molecular-weight thermotropic liquid crystal polyarylate is relatively difficult.
Chinese Patent Publication No. CN1189517A, published on August 5, 1998, the title of the invention is "a hybrid composite material containing glass fibers and thermotropic liquid crystal polymer microfibers", the application uses thermotropic liquid crystal polymer (TLCP ) microfiber and glass microfiber hybrid reinforced polycarbonate composite material, the purpose is to overcome the disadvantages of poor melt fluidity of glass fiber reinforced PC system, wear and tear on equipment, large number of broken glass fibers, and poor tensile properties of TLCP reinforced PC system
It can be seen that in the prior art, there is no relevant report about the short-process preparation method of thermotropic liquid crystal polyarylate nano-fibrils

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0032] ② Preparation of complex

[0033] The dried alkali-soluble polyester and thermotropic liquid crystal polyarylate are blended and extruded in a twin-screw extruder according to mass percentage respectively.

[0034] in,

[0035] 85-95 parts of alkali-soluble polyester

[0036] Thermotropic liquid crystal polyarylate 5-15 parts

[0037] The heating temperatures of the twin-screws are respectively: 220-250°C in the feed zone, 260-310°C in the melting zone, 250-300°C in the compression zone, and 260-310°C at the outlet.

[0038] Then, the compound prepared by the twin-screw extruder is vacuum-dried at 100-130° C. and kept at constant temperature for 24-48 hours.

[0039] ③ Melt spinning

[0040] The compound prepared by step ② is placed in a spinning machine for melt spinning to obtain alkali-soluble polyester fibers containing thermotropic liquid crystal polyarylate nanofibrils.

[0041]The screw heating temperatures for melt spinning are: feed zone 230-250°C, melting...

Embodiment 1

[0049] The fully aromatic random copolyester of p-hydroxybenzoic acid / 6-hydroxy-2-naphthoic acid with a melting point of 250°C and the alkali-soluble polyester with a melting point of 250°C are pre-crystallized and vacuum-dried, and the initial temperature of the vacuum drying temperature is 80°C , 1h to raise the temperature to 120°C, keep the temperature for 10h, then raise the temperature to 150°C, keep the temperature for 24h to make the water content reach 30ppm. The dried alkali-soluble polyester and the fully aromatic random copolyester of p-hydroxybenzoic acid / 6-hydroxy-2-naphthoic acid are mixed in a twin-screw extruder at a mass percentage of 85 / 15. The heating temperatures of the extruder are respectively: 220°C in the feed zone, 260°C in the melting zone, 250°C in the compression zone, and 260°C at the outlet. Then, the compound extruded by the twin-screw extruder was vacuum-dried, the vacuum drying temperature was 100° C., and the constant temperature time was 24 ...

Embodiment 2

[0051] The fully aromatic random copolyester of p-hydroxybenzoic acid / 6-hydroxy-2-naphthoic acid with a melting point of 280°C and the alkali-soluble polyester with a melting point of 280°C are pre-crystallized and vacuum-dried, and the initial temperature of the vacuum drying temperature is 90°C , 1h to raise the temperature to 130°C, keep the temperature for 11h, then raise the temperature to 160°C, keep the temperature for 32h to make the water content reach 20ppm. The dry alkali-soluble polyester and the fully aromatic random copolyester of p-hydroxybenzoic acid / 6-hydroxy-2-naphthoic acid are mixed in a twin-screw extruder at a mass percentage of 90 / 10. The heating temperatures of the extruder are respectively: 240°C in the feed zone, 285°C in the melting zone, 270°C in the compression zone, and 285°C at the outlet. Then, the compound extruded by the twin-screw extruder was vacuum-dried, the vacuum drying temperature was 120° C., and the constant temperature time was 32 ho...

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Abstract

The invention relates to a short-process preparation method of thermotropic liquid crystal polyarylester raw nano fibers, and in particular relates to a preparation method by which the thermotropic liquid crystal polyarylester raw nano fibers are obtained through melt blending alkali polyester and thermotropic liquid crystal polyarylester. The method comprises the following steps of: combining the thermotropic liquid crystal polyarylester with water-soluble polyester and spinning by utilizing the alkali polyester as a dissolving and separating component so that the thermotropic liquid crystal polyarylester is sufficiently oriented along a melt flow direction in a spinneret orifice with a high length-diameter ratio and raw nano fibers are formed; dissolving and removing the alkali polyester through a hot alkali liquor, separating and drying to obtain the thermotropic liquid crystal polyarylester raw nano fibers with excellent comprehensive performance. By utilizing the method, the thermotropic liquid crystal polyarylester raw nano fibers with excellent performances such as high length-diameter ratio, high strength, high modulus, high temperature resistance and radiation resistance can be produced; and moreover, the preparation method is simple and short in process, and time-consuming winding and back draft processing processes do not need, so that the method not only is environment-friendly but also can easily realize continuous production.

Description

technical field [0001] The present invention relates to a short-process preparation method of thermotropic liquid crystal polyarylate nanofibrils, in particular to a method for preparing thermotropic liquid crystal polyarylate nanofibrils by using alkali-soluble polyester as a dissolving component method. Background technique [0002] Thermotropic liquid crystal polyarylate (TLCP) fiber is a high-performance fiber with high strength and high modulus, excellent heat resistance, chemical corrosion resistance, extremely small linear expansion coefficient, and aging resistance. Nowadays, high-tech needs comprehensive properties such as high strength, high modulus, high temperature resistance, and radiation resistance. Especially in the national defense fields such as aerospace, armor protection, ship ropes and cables, and high-temperature filter materials, electronic insulation materials and other military-civilian dual-use fields, the application is very extensive. [0003] D...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F8/14D01D1/04D01D5/08
Inventor 王罗新施伟利王桦吴静周虎
Owner WUHAN TEXTILE UNIV