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Method for manufacturing ultrahigh-modulus graphite fiber continuous filament from coal tar

A graphite fiber and coal tar technology, applied in fiber chemical characteristics, textiles and papermaking, etc., can solve the problems that ultra-high modulus graphite fibers cannot be produced independently, and high-performance fibers are controlled by others

Inactive Publication Date: 2016-07-06
SHANDONG RUICHENG AEROSPACE CARBON MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing ultra-high modulus graphite fiber continuous filaments with coal tar, to solve the problem that domestic ultra-high modulus graphite fibers cannot be independently produced, and high-performance fibers are controlled by others

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Example 1: Add tetrahydrofuran and carbon disulfide mixed solvent 1 in equal proportions to coal tar, extract at 90°C, remove the mixture of mixed solvent 1 and coal tar pitch in the lower layer, filter, and recover mixed solvent 1 by distillation to obtain coal tar pitch; Add a mixed solvent 2 mixed with ethanol and acetone in equal proportions, extract at 90°C, take the mixture of the upper mixed solvent 2 and refined coal tar pitch, filter it, and recover the mixed solvent 2 by distillation to obtain refined coal tar pitch; place the refined coal tar pitch at high temperature and high pressure Polymerization in a reactor, temperature 400°C, pressure 1.5MPa, reaction time 10 hours, then lower the temperature to 380°C, reduce pressure to 20mbar, reaction time 10 hours, the softening point is 260°C, mesophase content 98%, good spinnability mesophase pitch; the mesophase pitch is melt-spun at 360°C, the pressure is 0.3MPa, and the drawing speed is 300m / min to obtain conti...

Embodiment 2

[0011] Example 2: Add tetrahydrofuran and carbon disulfide mixed solvent 1 mixed in equal proportions to coal tar, extract at 90°C, remove the mixture of mixed solvent 1 and coal tar pitch in the lower layer and filter, distill and recover mixed solvent 1 to obtain coal tar pitch; Add a mixed solvent 2 mixed with ethanol and acetone in equal proportions, extract at 90°C, take the mixture of the upper mixed solvent 2 and refined coal tar pitch, filter it, and recover the mixed solvent 2 by distillation to obtain refined coal tar pitch; place the refined coal tar pitch at high temperature and high pressure Polymerization in a reactor, temperature 410°C, pressure 2.0MPa, reaction time 15 hours, then lower the temperature to 380°C, depressurize to 30mbar, reaction time 15 hours, softening point 270°C, mesophase content 100%, good spinnability mesophase pitch; the mesophase pitch is melt-spun at 363°C, the pressure is 0.1MPa, and the drawing speed is 400m / min to obtain continuous le...

Embodiment 3

[0012] Example 3: Add tetrahydrofuran and carbon disulfide mixed solvent 1 mixed in equal proportions to coal tar, extract at 90°C, remove the mixture of mixed solvent 1 and coal tar pitch in the lower layer and filter, distill and recover mixed solvent 1 to obtain coal tar pitch; Add a mixed solvent 2 mixed with ethanol and acetone in equal proportions, extract at 90°C, take the mixture of the upper mixed solvent 2 and refined coal tar pitch, filter it, and recover the mixed solvent 2 by distillation to obtain refined coal tar pitch; place the refined coal tar pitch at high temperature and high pressure Polymerize in a reactor, temperature 420°C, pressure 2.5MPa, reaction time 20 hours, then cool down to 370°C, reduce pressure to 20mbar, reaction time 15 hours, softening point 280°C, mesophase content 100%, good spinnability mesophase pitch; melt-spin the mesophase pitch at 365°C, pressure 0.06MPa, and drawing speed 500m / min to obtain mesophase pitch fiber precursors with a di...

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PUM

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Abstract

The invention provides a method for manufacturing ultrahigh-modulus graphite fiber continuous filament from coal tar, belonging to a manufacture method of a graphite fiber. The method comprises the following steps of: extracting coal tar step by step with an organic solvent to obtain a pure pitch component; polymerizing the pure pitch component at a high temperature and high pressure to obtain a mesophase pitch with a moderate softening point, mesophase content not less than 98% and excellent spinnability; and performing fusion and continuous spinning on the mesophase pitch, and performing continuous oxidation, carbonization and graphitizing treatment to obtain the ultrahigh-modulus graphite fiber continuous filament with modulus not less than 600GPa. According to the method, the raw materials are readily available, the cost is low, the process is simple, the energy consumption is low, and the industrialization is facilitated.

Description

technical field [0001] The invention relates to a method for preparing ultra-high modulus graphite fiber continuous filaments from coal tar, and belongs to the technical field of high-performance new materials. Background technique [0002] In addition to light weight and high strength, mesophase pitch-based carbon fiber also has the characteristics of ultra-high modulus, high thermal conductivity, high electrical conductivity, and low thermal expansion coefficient. It is suitable for space environments with large temperature differences between day and night. Using it as a reinforcement can prepare thermal expansion Various structural and functional composite materials with coefficients of zero have become indispensable reinforcements for solving outer space structure and functional composite materials. Only Japan and the United States can produce mesophase pitch-based carbon fibers in the world, and have formed a certain production scale and serialized products, while my c...

Claims

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Application Information

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IPC IPC(8): D01F9/15
CPCD01F9/15
Inventor 王硕迟伟东张学军刘怀成王象东刘辉
Owner SHANDONG RUICHENG AEROSPACE CARBON MATERIAL CO LTD
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