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Modification method of aramid fiber in supercritical CO2 by surface grafting polymerization

A kind of aramid fiber and surface grafting technology, applied in the field of modification of aramid fiber, can solve the problems of poor reaction, low inoculation rate, complicated operation, etc. controllable effect

Inactive Publication Date: 2013-11-13
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the two solution modification methods can modify the surface of aramid fibers, they have disadvantages such as complicated operation, toxic solvent, pollution, and poor control of the reaction, so they have not been applied on a large scale.
There are few studies on the modification of aramid fibers by solid-phase grafting, and there are disadvantages such as high reaction temperature, uncontrollable reaction, complicated operation, and low inoculation rate. Generally, it is not used to modify aramid fibers.

Method used

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  • Modification method of aramid fiber in supercritical CO2 by surface grafting polymerization
  • Modification method of aramid fiber in supercritical CO2 by surface grafting polymerization
  • Modification method of aramid fiber in supercritical CO2 by surface grafting polymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Cleaning of aramid fiber surface:

[0031] Put the acetone solution in the three-necked flask, and put the aramid fiber in the Soxhlet extractor. Heat the acetone to 70°C, wash the surface of the aramid fiber after the acetone is condensed and refluxed, and take out the vacuum-dried fiber after 24 hours of cleaning time.

[0032] (2) Aramid fiber surface graft polymerized styrene

[0033] A certain amount (BPO / St=0.3-1wt%) of initiator (take BPO as an example) and monomer St are added to the bottom of the autoclave, and aramid fibers whose surface has been cleaned (without contact with monomer and initiator) are added. Close the autoclave and fill the autoclave with CO 2 and discharge CO 2 three times to expel the air. Fill the kettle with CO 2 , and heat the system so that the pressure reaches 13-30MPa, the temperature is 45-50°C, and the system is in supercritical CO 2 state. After swelling the aramid fiber for 4-8 hours, directly heat the system to 70-100°...

Embodiment 2

[0039] (1) Cleaning of aramid fiber surface:

[0040] Put the acetone solution in the three-necked flask, and put the aramid fiber in the Soxhlet extractor. Heat the acetone to 70°C, wash the surface of the aramid fiber after the acetone is condensed and refluxed, and take out the vacuum-dried fiber after 24 hours of cleaning time.

[0041] (2) Aramid fiber surface graft polymerization methyl methacrylate

[0042] A certain amount (BPO / MMA=0.4-3wt%) of initiator and monomer MMA are added to the bottom of the autoclave, and aramid fiber (without contact with monomer and initiator) whose surface has been cleaned is added. Close the autoclave and fill the autoclave with CO 2 and discharge CO 2 three times to expel the air. Fill the kettle with CO 2 , and heat the system so that the pressure reaches 8-30MPa, the temperature is 45-50°C, and the system is in supercritical CO 2 state. After swelling the aramid fiber for 4-8 hours, directly heat the system to 80-100°C to initia...

Embodiment 3

[0048] (1) Cleaning of aramid fiber surface:

[0049] Put the acetone solution in the three-necked flask, and put the aramid fiber in the Soxhlet extractor. Heat the acetone to 70°C, wash the surface of the aramid fiber after the acetone is condensed and refluxed, and take out the vacuum-dried fiber after 24 hours of cleaning time.

[0050] (2) Graft polymerization of maleic anhydride on the surface of aramid fibers

[0051] A certain amount (BPO / MAH=0.4-3wt%) initiator and monomer MAH are added to the bottom of the autoclave, and aramid fibers whose surface has been cleaned (without contact with monomer and initiator) are added. Close the autoclave and fill the autoclave with CO 2 and discharge CO 2 three times to expel the air. Fill the kettle with CO 2 , and heat the system so that the pressure reaches 13-30MPa, the temperature is 45-50°C, and the system is in supercritical CO 2 state. After swelling the aramid fiber for 4-8 hours, directly heat the system to 125°C t...

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Abstract

The invention relates to a modification method of aramid fiber in supercritical CO2 by surface grafting polymerization. The method comprises the steps of: (1) cleaning aramid fiber surface with acetone and vacuum-drying fiber; (2) adding monomers and an initiator to a reaction vessel, then adding the aramid fiber, closing the reaction vessel, removing air, introducing CO2 into the reaction vessel at the temperature lower than the decomposition temperature of the initiator so that the system is in a supercritical CO2 state, swelling and heating for polymerizing the monomers to obtain surface-polymerization-modified aramid fiber, wherein the aramid fiber does not contact the monomers and the initiator; and (3) cleaning the surface-polymerization-modified aramid fiber with acetone until constant weight, and finally vacuum-drying the fiber. According to the invention, the method is simple in operation, economical, environmentally friendly and controllable in grafting ratio; and the obtained modified aramid fiber has rough surface due to the existence of the polymer, so that the adhesion and compatibility between the fiber and a composite material substrate are improved and the application of the fiber as a composite material reinforcing agent is facilitated.

Description

technical field [0001] The invention belongs to the field of modification of aramid fiber, in particular to a kind of aramid fiber modified in supercritical CO 2 Surface graft polymerization modification method in . Background technique [0002] Aramid fiber can be roughly divided into poly-m-phenylene isophthalamide fiber (referred to as meta-aramid fiber), poly-para-phenylene terephthalamide fiber (referred to as para-aramid fiber) and heterocyclic aromatic polyamide fiber. Amide fiber (referred to as aramid fiber III) and other varieties. Because aramid fibers have the characteristics of ultra-high modulus, high strength, high temperature resistance, and light weight, they are widely used in aerospace, military clothing, and material reinforcement. Since aramid fiber is formed by rigid molecular chains, it has a unique "skin-core" structure. The rod-like molecules in the core are arranged in parallel through hydrogen bonds, and the rigid molecular chains with high cryst...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D06M14/16C08L51/08
CPCY02P20/54
Inventor 余木火周建军滕翠青马禹韩克清孔海娟张蕊焦玉聪赵玲刘涛严斌尤伟刘振全
Owner DONGHUA UNIV
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