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Preparation method of high-performance organic fibers on basis of 4,4'-diaminodiphenyl ether

A technology of diaminodiphenyl ether and organic fiber, which is applied in fiber processing, fiber chemical characteristics, wet spinning, etc., can solve the problems of poor interfacial adhesion between fiber and resin matrix, low interfacial shear strength, and difficulty in resin infiltration. , to achieve the effect of improving heat resistance, heat resistance and oxidation resistance, and reducing the internal stress of resin

Active Publication Date: 2013-08-14
浙江甬川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

[0003] The purpose of the present invention is to solve the problem that the traditional PBO fiber generally has a smooth fiber surface and low activity, which is not easy to infiltrate with the resin, resulting in poor interface bonding between the fiber and the resin matrix, and low interface shear strength. Preparation method of high-performance organic fiber based on 4,4'-diaminodiphenyl ether

Method used

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Comparison scheme
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specific Embodiment approach 1

[0017] Embodiment 1: A method for preparing high-performance organic fibers based on 4,4'-diaminodiphenyl ether in this embodiment is carried out according to the following steps:

[0018] 1. Mix 4,6-diaminoresorcinol hydrochloride, 4,4'-diaminodiphenyl ether, 2,5-dihydroxyterephthalic acid, polyphosphoric acid and the first part of phosphorus pentoxide , under the condition that the system pressure is less than 20mmHg, the temperature is raised to 20°C for 5 hours, the temperature is raised to 40°C for 120 hours, the temperature is raised to 20°C for 19 hours, the temperature is raised to 60°C for 24 hours, and then the second part of phosphorus pentoxide is added. After reacting at a temperature of 100°C for 24 hours, polymethylphenylsiloxane was added, followed by reacting at a temperature of 140°C for 24 hours and at a temperature of 195°C for 24 hours to obtain a crude polymer; 2. After filtering and degassing, extrude with a twin-screw extruder to obtain a spinning solut...

specific Embodiment approach 2

[0029] Specific embodiment 2: The difference between this embodiment and specific embodiment 1 is: 4,6-diaminoresorcinol hydrochloride, 4,4'-diaminodiphenyl ether, 2, The purity of 5-dihydroxyterephthalic acid is greater than 99.5%, and the monomer impurities are less than 0.2%. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0030] Embodiment 3: The difference between this embodiment and Embodiment 1 or 2 is that the mass ratio of polymethylphenylsiloxane to polyphosphoric acid described in Step 1 is 0.05-0.10:1. Others are the same as in the first or second embodiment.

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Abstract

The invention relates to a preparation method of high-performance organic fibers, particularly a preparation method of high-performance organic fibers on the basis of 4,4'-diaminodiphenyl ether. The invention aims to solve the common problems of poor interfacial binding property and low interfacial shear strength between fibers and resin substrate due to smooth surface, low activity and low soakage tendency with resin in the traditional PBO (poly(p-phenylene-2,6-benzobisoxazole)) fibers. The method comprises the following steps: adding 4,6-diamino-resorcinol hydrochloride, 4,4'-diaminodiphenyl ether, 2,5-dihydroxyterephthalic acid, polyphosphoric acid and phosphorus pentoxide into a polymerization kettle, dissolving by heating, adding phosphorus pentoxide, heating, adding polymethylphenylsiloxane, heating, filtering, degassing, extruding, preparing protofibrils, washing with water, washing with alcohol, washing with alkali, drying, and heating in a nitrogen protective atmosphere to obtain the high-performance organic fibers. The tensile strength of the high-performance organic fibers reaches 2.5-5.5 GPa. The invention is applicable to the field of preparation of organic fibers.

Description

technical field [0001] The invention belongs to the technical field of high-performance organic fiber preparation, and in particular relates to a new preparation method of a novel high-performance organic fiber. Background technique [0002] The traditional PBO preparation method mainly contains the following two kinds: 1. Use 4,6-diaminoresorcinol hydrochloride and terephthaloyl chloride or terephthalic acid to remove HCl first under the condition of polyphosphoric acid, Then the temperature rises to cause a polymerization reaction, and the obtained polymer is filtered and degassed to obtain a spinning solution. The spinning solution is extruded through a screw extruder through a spinneret, and is subjected to air bath, pickling, alkali washing, coiling, A PBO fiber with a diameter of about 15 microns is obtained, and a high modulus PBO fiber is obtained after heat treatment. 2. Prepare a complex salt with 4,6-diaminoresorcinol hydrochloride and equimolar terephthalic acid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/74D01F11/08C08G73/22D01D1/10D01D5/06
Inventor 王阳张宇田亚新
Owner 浙江甬川聚嘉新材料科技有限公司
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