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Method for preparing polythioether polymer grafted carbon fibers on basis of thiol-ene photopolymerization

A carbon fiber and polysulfide technology, applied in carbon fiber, fiber processing, textiles and papermaking, etc., can solve the problems of low modification efficiency, generation of harmful substances, complicated processing process, etc., to improve interface properties, improve wettability, The effect of simplifying post-processing steps

Active Publication Date: 2017-03-22
江西国计纳米科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are many surface modification methods for carbon fibers, including oxidation treatment, coating treatment and radiation treatment, etc., but the treatment process of these methods is complicated, the modification efficiency is not high, and some modification processes may even produce harmful substances

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] This example illustrates a method for preparing a polysulfide polymer-grafted carbon fiber based on mercapto-ene photopolymerization provided by the present invention.

[0017] Step 1: Add 1g of raw carbon fiber to 70mL of concentrated nitric acid with a concentration of 65% by mass, and react under reflux for 4 hours at 90°C. After the reaction, wash with distilled water until the pH value is neutral, and place in a vacuum at 80°C Dry in a drying oven for 24 hours to obtain acid-treated carbon fibers;

[0018] Step 2: Add 0.5 g of acid-treated carbon fiber and 0.05 mol of 3-mercapto-1-propanol into 40 mL of xylene, stir at room temperature for 40 minutes, then add 0.005 mol of 4-dimethylaminopyridine and 0.05 mol of bicyclic Hexylcarbodiimide, continue to react at room temperature for 6 hours, after the reaction is completed, suction filter and wash with xylene for 4 times, and then dry in a vacuum oven at 80°C for 24 hours to obtain thiolated carbon fibers;

[0019] ...

Embodiment 2

[0021] This example illustrates a method for preparing a polysulfide polymer-grafted carbon fiber based on mercapto-ene photopolymerization provided by the present invention.

[0022] Step 1: Add 1g of raw carbon fiber to 50mL of concentrated nitric acid with a concentration of 65% by mass, and react under reflux for 6 hours at 70°C. After the reaction, wash with distilled water until the pH value is neutral, and place in a vacuum at 80°C Dry in a drying oven for 24 hours to obtain acid-treated carbon fibers;

[0023] Step 2: Add 0.5 g of acid-treated carbon fiber and 0.01 mol of 4-mercapto-1-butanol to 20 mL of xylene, stir at room temperature for 30 minutes, then add 0.001 mol of 4-dimethylaminopyridine and 0.01 mol of bicyclic Hexylcarbodiimide, continue to react at room temperature for 4 hours, after the reaction is completed, suction filter and wash 4 times with xylene, and then dry in a vacuum oven at 80°C for 24 hours to obtain mercaptolated carbon fibers;

[0024] Ste...

Embodiment 3

[0026] Step 1: Add 1g of raw carbon fiber to 100mL of concentrated nitric acid with a concentration of 65% by mass, and reflux at 100°C for 2 hours. After the reaction, wash with distilled water until the pH value is neutral, and place in a vacuum at 80°C. Dry in a drying oven for 24 hours to obtain acid-treated carbon fibers;

[0027] Step 2: Add 0.5 g of acid-treated carbon fiber and 0.1 mole of mercaptoethanol to 50 mL of xylene, stir at room temperature for 50 minutes, then add 0.01 mole of 4-dimethylaminopyridine and 0.1 mole of dicyclohexylcarbodiimide, Continue to react at room temperature for 8 hours. After the reaction is completed, filter with suction and wash with xylene for 4 times, and then dry in a vacuum oven at 80°C for 24 hours to obtain mercaptolated carbon fibers;

[0028] Step 3: Add 0.5g of mercaptocarbon fiber, 0.2mol of 1,2-ethanedithiol and 0.2mol of 1,3-butadiene to 50mL of dimethylformamide, then add 100mg of 2-hydroxy -2-Methyl-1-phenyl-1-propanone,...

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Abstract

The invention discloses a method for preparing polythioether polymer grafted carbon fibers on the basis of thiol-ene photopolymerization. The method specifically includes the steps that firstly, carbon fibers are subjected to acidification to obtain acidified carbon fibers; secondly, the acidified carbon fibers further react with mercapto-alcohol to obtain sulfhydrylated carbon fibers; thirdly, the sulfhydrylated carbon fibers, dimercapto monomers and diene monomers initiate a thiol-ene photopolymerization reaction under irradiation of ultraviolet, and the polythioether polymer grafted carbon fibers are obtained. The method has the advantages that by means of the thiol-ene photopolymerization reaction, the consumption of solvents is reduced, after-treatment steps are simplified, large-scale production is benefited, and meanwhile the toxic and harmful acylating chlorination process existing in a traditional carbon fiber surface grafting and modifying process is avoided; polythioether polymer is grafted on the surfaces of the carbon fibers so that active functional groups on the surfaces of the carbon fibers are increased, wettability of the carbon fibers with resin is easily improved, and interface performance between the carbon fibers and a resin matrix is improved.

Description

technical field [0001] The invention relates to a preparation method of polysulfide polymer grafted carbon fiber based on mercapto-ene photopolymerization. Background technique [0002] As an important structural material in the aerospace field, carbon fiber reinforced resin matrix composites have attracted widespread attention in recent years due to their advantages such as high specific strength, high specific modulus, high temperature resistance, good designability and corrosion resistance. However, the untreated carbon fiber surface is inert and has less active functional groups, and its wettability with the resin matrix is ​​poor, resulting in poor interface bonding with the resin matrix and many defects at the interface, which limits the carbon fiber reinforced resin matrix composite. The overall performance of the material. Therefore, modifying the surface of carbon fiber to improve its bonding performance with the resin matrix is ​​one of the focuses in the current ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D06M15/687C08G75/045C08K9/10C08K7/06D06M101/40
CPCC08G75/045C08K7/06C08K9/10D06M15/687D06M2101/40
Inventor 熊磊兰道松梁红波黄圣梅
Owner 江西国计纳米科技有限公司
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