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Preparation method for composite carbon fiber based on graphene/ polyacrylonitrile

A technology of composite carbon fiber and polyacrylonitrile, applied in the direction of fiber chemical characteristics, single-component synthetic polymer rayon, wet spinning method, etc., to achieve good strength and toughness, easy operation, and wide source of raw materials

Active Publication Date: 2012-07-18
杭州德烯科技集团有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the latest research, macroscopic graphene fibers were prepared by chemically oxidizing graphene (Nature communication, 2011, 2:571), however, by improving the interaction between graphene sheets, a large number of graphene fibers with higher performance can be prepared Replacing traditional carbon fiber remains a challenge

Method used

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  • Preparation method for composite carbon fiber based on graphene/ polyacrylonitrile
  • Preparation method for composite carbon fiber based on graphene/ polyacrylonitrile

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preparation example Construction

[0024] The steps of the preparation method of graphene / polyacrylonitrile composite carbon fiber are as follows:

[0025] 1) 1 part by weight of graphene or graphene oxide, 10-1000 parts by weight of solvent, 10-1000 parts by weight of acrylonitrile monomer, add 0.01-10 parts by weight of initiator under nitrogen protection, and heat to 50-95 °C, react for 1-60 hours, precipitate, centrifuge, wash, and dry to obtain polyacrylonitrile-grafted graphene;

[0026] 2) Add 1 part by weight of polyacrylonitrile-grafted graphene to 5-150 parts by weight of an organic solvent, and process ultrasonically at 5-50 KHz at 30-80 °C for 0.1-10 hours to obtain polyacrylonitrile-grafted graphene spinning lyosol;

[0027] 3) Pass the polyacrylonitrile-grafted graphene spinning solution sol through a spinning capillary with a diameter of 5-500 μm at an extrusion speed of 1-100 mL / h, and stay in the coagulation solution at 10-80°C for 1-100s Solidified into filaments, collected by a winder, and ...

Embodiment 1

[0037] 1) Add 20 mg of graphene oxide, 20 mL of N, N-dimethylformamide (DMF), 15 g of acrylonitrile monomer, add 0.01 g of initiator by weight under nitrogen protection, and heat to 60 °C , reacted for 48 hours, through precipitation, centrifugation, washing, drying, to obtain graphene grafted with polyacrylonitrile;

[0038] 2) Add 50 mg of polyacrylonitrile-grafted graphene to 10 mL of N, N-dimethylacetamide, and process it at 30 °C with 25KHz ultrasonic for 5 hours to obtain polyacrylonitrile-grafted graphene spinning solution Sol;

[0039] 3) The polyacrylonitrile-grafted graphene spinning solution sol was passed through a spinning capillary with a diameter of 30 μm at an extrusion speed of 10 mL / h, and mixed with water and dimethyl sulfoxide (DMSO) at 20 °C Stay in the medium for 50 s to solidify into filaments, collect them with a winder, and obtain graphene oxide fibers after drying.

[0040] 4) The graphene fiber was reduced in hydroiodic acid for 10 h, washed and dr...

Embodiment 2

[0043] 1) Add 20 mg of graphene oxide, 20 mL of N, N-dimethylformamide (DMF), 10 g of acrylonitrile monomer, add 0.01 g of initiator by weight under nitrogen protection, and heat to 50 °C , reacted for 48 hours, through precipitation, centrifugation, washing, drying, to obtain graphene grafted with polyacrylonitrile;

[0044] 2) Add 50 mg of polyacrylonitrile-grafted graphene to 3 mL of butanol, and conduct ultrasonic treatment at 30 °C for 5 hours at 30KHz to obtain polyacrylonitrile-grafted graphene spinning solution sol;

[0045] 3) The polyacrylonitrile-grafted graphene spinning solution sol was passed through a spinning capillary with a diameter of 30 μm at an extrusion rate of 10 mL / h, and was solidified in a mixture of water and tetrahydrofuran at 20 °C for 50 s. The filaments were collected using a winder and dried to obtain graphene oxide fibers.

[0046] 4) Place the graphene fiber in an inert gas protection, raise the temperature to 500°C at 20°C / min, keep the temp...

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Abstract

The invention discloses a preparation method for composite carbon fiber based on graphene / polyacrylonitrile. The preparation method comprises the following steps: adding 0.01-10 parts by weight of initiating agent under nitrogen protection into 1 part by weight of graphene or oxidized graphene, 10-1000 parts by weight of solvent and 10-1000 parts by weight of acrylonitrile monomer; heating to 50-95DEG C; reacting for 1-60 hours; precipitating, carrying out centrifugation, washing and drying to obtain the polyacrylonitrile grafted graphene; dispersing the polyacrylonitrile grafted graphene into polar organic solvent to obtain spinning solution sol; continuously extruding the spinning solution from a spinning head capillary at a constant speed to enter solidification solution; collecting the solidified primary fiber; and drying to obtain the graphene fiber primary silk; and carrying out chemical or thermal treatment to obtain the graphene / polyacrylonitrile composite carbon fiber. The preparation method is simple and convenient, has simple technology, is convenient and quick for post-processing, and can be produced on a large scale. The obtained graphene / polyacrylonitrile composite carbon fiber embodies excellent intensity, toughness, modulus thermal stability and electrical conductivity and can be applied in various industrial fields to replace the traditional carbon fiber.

Description

technical field [0001] The invention relates to a method for preparing carbon fibers, in particular to a method for preparing composite carbon fibers based on graphene / polyacrylonitrile. Background technique [0002] Carbon fiber is a microcrystalline graphite material prepared by carbonizing and graphitizing organic fibers. The microstructure of carbon fiber is similar to artificial graphite, which is a turbostratic graphite structure. It has high axial strength and modulus, no creep, good fatigue resistance, specific heat and electrical conductivity between non-metal and metal, and small thermal expansion coefficient. It has good chemical resistance, low fiber density, and good X-ray permeability. It is a material with excellent mechanical properties and is an indispensable material for the development of cutting-edge technologies such as aerospace. However, the preparation process of traditional carbon fiber is cumbersome and complicated, and the properties of the precur...

Claims

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Application Information

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IPC IPC(8): D01F9/21D01F6/38D01D5/06C08F292/00
Inventor 高超刘峥
Owner 杭州德烯科技集团有限公司
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