A kind of method for grafting hexamethylenetetramine on carbon fiber surface in supercritical methanol

A technology of hexamethylenetetramine and supercritical methanol is applied in the directions of carbon fiber, fiber processing, textile and paper making, etc., which can solve the problems of uneven distribution of groups, low bonding strength of carbon fiber and resin, etc., to improve the reaction efficiency, Increase the surface area and increase the effect of mechanical meshing

Inactive Publication Date: 2016-08-24
HARBIN INST OF TECH
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  • Summary
  • Abstract
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  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to solve the problems that the existing carbon fiber surface modification method has few groups grafted to the carbon fiber, the group is unevenly distributed on the carbon fiber, and the bonding strength between the modified carbon fiber and the resin is low. A method of grafting hexamethylenetetramine on the surface of carbon fiber in supercritical methanol

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  • A kind of method for grafting hexamethylenetetramine on carbon fiber surface in supercritical methanol
  • A kind of method for grafting hexamethylenetetramine on carbon fiber surface in supercritical methanol
  • A kind of method for grafting hexamethylenetetramine on carbon fiber surface in supercritical methanol

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specific Embodiment approach 1

[0054] Specific embodiment one: This embodiment is a method for grafting hexamethylenetetramine on the surface of carbon fibers in supercritical methanol, specifically as follows:

[0055] 1. Cleaning:

[0056] ① Put the carbon fiber into a Soxhlet extractor filled with acetone, and use acetone to clean and remove impurities on the surface of the carbon fiber at a temperature of 75°C to 85°C. The cleaning time is 2h to 8h, and the cleaned carbon fiber is taken out. Obtain the carbon fiber after cleaning with acetone;

[0057] ②. Place the carbon fiber cleaned with acetone obtained in step ① into a supercritical device, and soak it in a supercritical acetone-water system with a temperature of 350°C to 370°C and a pressure of 8MPa to 14MPa for 20min to 30min to obtain ring removal Carbon fiber after oxygen coating;

[0058] The volume ratio of acetone and water in the supercritical acetone-water system described in step 2. is 5:1;

[0059] ③. Place the carbon fibers obtained ...

specific Embodiment approach 2

[0094] Specific embodiment 2: The difference between this embodiment and specific embodiment 1 is that in step 2 ①, the dry and cleaned carbon fiber obtained in step 1 ③ is impregnated into potassium persulfate / silver nitrate mixed aqueous solution, heated to 70°C, and The temperature is kept at 70°C for 1.5 hours to obtain oxidized carbon fibers; the concentration of potassium persulfate in the potassium persulfate / silver nitrate mixed aqueous solution is 0.1mol / L to 0.15mol / L; the persulfuric acid The concentration of silver nitrate in the potassium / silver nitrate mixed aqueous solution is 0.003mol / L-0.005mol / L. Other steps are the same as in the first embodiment.

specific Embodiment approach 3

[0095] Specific embodiment three: the difference between this embodiment and specific embodiment one or two is: in step three (1), put the thionyl chloride / N,N-dimethylformamide mixture into the dry reaction bottle, Put the dry oxidized carbon fibers obtained in step 2 ⑥ into a reaction flask, heat to 80°C, and react at a constant temperature of 80°C for 45h to 50h to obtain acyl chloride carbon fibers containing impurities. Other steps are the same as those in Embodiment 1 or 2.

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Abstract

The invention discloses a method of grafting hexamine on a carbon fiber surface in supercritical methanol and relates to a carbon fiber surface modification method. The method aims at solving the problems that few groups are grafted onto a carbon fiber and distributed on the carbon fiber nonuniformly, and the bonding strength of the modified carbon fiber with resin is low for the existing carbon fiber surface modification method. The method of grafting hexamine on the carbon fiber surface in supercritical methanol comprises the steps: I, cleaning, II, oxidizing, III, acylating chlorination, IV, alcoholysis, and V, grafting of hexamine in supercritical methanol to form the carbon fiber with hexamine grafted on the surface. Interfacial shear strength of the carbon fiber with hexamine grafted on the surface is improved to 106.1MPa from 64.9MPa of a precursor fiber by 63.5%.The method of grafting hexamine on the carbon fiber surface in supercritical methanol can be obtained.

Description

technical field [0001] The invention relates to a method for modifying the surface of carbon fibers. Background technique [0002] Carbon fiber and carbon fiber composite materials are widely used in aerospace, national defense, machinery manufacturing and other fields. In carbon fiber composites, the interface between carbon fibers and the matrix plays a crucial role, and a good interface bond can effectively transfer loads, thereby improving the mechanical properties of the material. However, the surface of untreated carbon fiber is inert and the interface with the resin matrix is ​​weak, which affects the full play of the excellent performance of carbon fiber composite materials. Therefore, it is necessary to carry out surface treatment on carbon fiber to improve the interfacial bonding quality of its composite material, thereby improving the interfacial mechanical properties of the material. [0003] Commonly used carbon fiber surface modification methods mainly includ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D06M13/358D06M13/144D06M13/268D06M11/50D06M11/65D06M13/127D06M101/40
Inventor 孟令辉马丽春黄玉东武光顺王宇威赵敏谢非
Owner HARBIN INST OF TECH
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