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Preparation method of high-modulus carbon fibers and precursor mesophase pitch thereof

A mesophase pitch and carbon fiber technology, which is applied in the field of preparation of high modulus carbon fiber and its precursor mesophase pitch, can solve the problems of high energy consumption and complicated pretreatment process, and achieve low energy consumption, good spinnability, high The effect of tensile strength

Active Publication Date: 2020-08-25
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the pretreatment process is more complex and consumes more energy

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0030] In one or more examples of this embodiment, a more specific technical solution is provided. The preparation method of the mesophase pitch and the high modulus carbon fiber includes the following specific steps:

[0031] Take a certain quality of heavy oil as a raw material, use flushing agent as a solvent to form a solution with a mass fraction of 5%, add this solution to a chromatographic column equipped with polystyrene packing, and carry out size exclusion chromatography separation. The gel column diameter of size exclusion chromatography is 50-100mm, the height is 800-1000mm, and the packing pore diameter The top of the column layer is pressurized to collect the effluent oil; the effluent oil is sequentially passed through the large-pore cation exchange resin made by introducing sulfonic acid groups and the large-pore anion exchange resin made by introducing quaternary ammonium groups. Resin is separated by ion exchange chromatography, the packed column of the ion ...

Embodiment 1

[0037] (1) Get 20g catalytic cracking oil slurry, adopt tetrahydrofuran to be made into the solution that mass fraction is 5% as solvent, join this solution in the chromatographic column that polystyrene is housed, gel column diameter 50-100mm, height 800- 1000mm, packing hole diameter The top of the column layer is pressurized to collect the effluent oil; the effluent oil is added to the cation exchange resin filler (with styrene-diethylene copolymer as the skeleton, introducing sulfonic acid group) and anion exchange resin filler (with styrene-diethylene copolymer) respectively. The ethylene copolymer is the skeleton, introduced into the chromatographic column of quaternary amino group), the diameter of the packed column is 10-20mm, and the height is 500-1000mm, and the effluent oil is collected. Add the effluent oil into the autoclave, replace the air with nitrogen for 3 times, then raise the pressure to 4MPa with nitrogen, raise the temperature to 430°C, and heat-treat fo...

Embodiment 2

[0039] (1) get 20g atmospheric residual oil, adopt hexanaphthene to be made into the solution that mass fraction is 5% as solvent, this solution joins in the chromatographic column that polystyrene filler is housed, gel column diameter 50-100mm, Height 800-1000mm, filler hole diameter The top of the column layer is pressurized to collect the effluent oil; the effluent oil is added to the cation exchange resin (with polystyrene as the skeleton, introducing sulfonic acid groups) and anion exchange resin packing (with polystyrene as the skeleton, introducing quaternary ammonium) respectively. In the chromatographic column of base), the gel column diameter is 10-20mm, the height is 500-1000mm, and the effluent oil is collected. Add the effluent oil into the high-pressure reaction kettle, replace the air with nitrogen for 3 times, then introduce nitrogen to raise the pressure to 5MPa, raise the temperature to 440°C, and heat-treat for 8 hours under constant stirring. During the re...

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Abstract

The invention provides a preparation method of high-modulus carbon fibers and precursor mesophase pitch thereof. According to the method, with heavy oil adopted as a raw material, components with molecular weight distribution of 400-1000 are separated out by volume exclusion chromatography; acidic components and alkaline components in the heavy oil are respectively removed through ion exchange chromatography and by means of large-aperture cation exchange resin and anion exchange resin in sequence, so that modified raw oil can be obtained; thermal polycondensation carbonization is performed onthe modified raw oil to obtain the high-quality mesophase pitch with good spinnability; the high-quality mesophase pitch has the advantages of high mesophase content, low softening point, low viscosity, meltability and good spinnability, and is a high-quality raw material for preparing high-modulus carbon fibers; and after melt spinning, pre-oxidation, carbonization and graphitization treatment are carried out, the high-modulus mesophase pitch-based carbon fibers can be obtained.

Description

technical field [0001] The invention belongs to the technical field of deep processing of petroleum and the field of preparation of advanced new carbon materials, and in particular relates to a preparation method of high modulus carbon fiber and its precursor mesophase pitch. Background technique [0002] Carbon fiber is a microcrystalline graphite material, which is formed by stacking organic fibers such as flake graphite microcrystals along the axial direction of the fiber, and is obtained by carbonization and graphitization. It is a new fiber material with high strength and high modulus with a carbon content of more than 95%. It has superior mechanical properties, its tensile strength can reach more than 3500MPa, its light weight, low density, strong corrosion resistance and wear resistance, high electrical and thermal conductivity, etc., is widely used in ultra-high thermal conductivity materials, aviation Aircraft manufacturing, new building reinforcement materials, au...

Claims

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Application Information

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IPC IPC(8): C10B55/00C10G55/04
CPCC10B55/00C10G55/04B01D15/34B01D15/362B01D15/363B01J20/261B01J20/28047B01J20/28054C10B57/045C10C3/002C10G25/02D01F9/155C10C3/08D01F9/15D10B2101/12
Inventor 刘东龚鑫李志浩李骏于庆生杨朝合付玉娥
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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