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A kind of coal tar pitch chemical modification method for carbon fiber preparation

A technology of chemical modification and coal tar pitch, applied in the direction of chemically processing tar pitch/petroleum pitch/natural pitch, etc., can solve the problems of energy consumption and production cost, and achieve the effect of good modification effect and simple process

Inactive Publication Date: 2011-11-30
徐国财
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, high-temperature treatment brings energy consumption and an increase in production costs.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh coal tar pitch with a softening point temperature of 50°C and place it in an oven at 110°C to constant weight to remove moisture. Add the solvent quinoline into the extraction vessel containing the coal tar pitch at a volume-to-mass ratio of 5:1 (volume of solvent: mass of coal tar pitch), and stir at room temperature for 5 hours. After the stirring is finished, the liquid in the extraction container is suction filtered, and the filtrate is extracted. The filtrate was poured into a reaction vessel, heated to 100° C. under the conditions of continuous nitrogen flow and constant stirring, and reacted for a period of time for 10 hours. Then the solvent quinoline is distilled off by heating, until no quinoline solvent is distilled off, the reaction ends. Modified coal tar pitch was obtained. The viscosity at 70°C tested by a rheometer is 80Pa.s.

Embodiment 2

[0023] Coal tar pitch with a softening point of 50°C was weighed and placed in an oven at 120°C to constant weight to remove moisture. Add the solvent quinoline into the extraction vessel containing the coal tar pitch at a volume-to-mass ratio of 3:1 (solvent volume: mass of coal tar pitch), and stir at room temperature for 15 hours. After the stirring is completed, the liquid in the extraction vessel is suction-filtered to obtain a filtrate. Pour the filtrate into a reaction vessel, and add boron trifluoride ether as a catalyst with 1% coal tar pitch mass when heated to 100°C under constant nitrogen flow and stirring. The reaction was carried out at 100° C. for 5 hours. Then the solvent quinoline is distilled off by heating, until no quinoline solvent is distilled off, the reaction ends. Modified coal tar pitch was obtained. Its viscosity is 600Pa·s at 70°C by rheometer test.

Embodiment 3

[0025]Coal tar pitch with a softening point of 50°C was weighed and placed in an oven at 120°C to constant weight to remove moisture. Add the solvent quinoline into the extraction vessel containing the coal tar pitch at a volume-to-mass ratio of 5:1 (solvent volume: mass of coal tar pitch), and stir at room temperature for 10 hours. After the stirring is finished, the liquid in the extraction container is suction filtered, and the filtrate is extracted. Pour the filtrate into a reaction vessel, and add boron trifluoride ether as a catalyst with 5% coal tar pitch mass when heated to 100°C under constant nitrogen flow and stirring. The reaction was carried out at 110° C. for 8 hours. Then the solvent quinoline is distilled off by heating, until no quinoline solvent is distilled off, the reaction ends. Modified coal tar pitch was obtained. The viscosity at 190°C tested by rheometer is 1500Pa.s.

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Abstract

The invention relates to a chemical modification method of coal tar pitch used for carbon fiber preparation. The operation steps of the method are as follows: dry the coal tar pitch at a temperature of 110-120°C to constant weight; mix the solvent quinoline and coal tar pitch at a volume-to-mass ratio of 3-15:1, and stir for 5-15 hours; solution; filter the mixed solution to obtain the filtrate; pour the filtrate into a reaction vessel, heat it under continuous nitrogen flow and stirring, and when it is heated to 80-120°C, add a catalyst to the filtrate according to 1-16% of the mass of coal tar pitch. The catalyst is The mixture of boron trifluoride diethyl ether and nitroaromatics is reacted at 100-180°C for 5-10 hours, and the solvent quinoline is distilled out by heating, until no quinoline solvent is distilled out, and the viscosity at 190°C is 1000-3400Pa·s Chemically modified coal tar pitch. The present invention can successfully realize the chemical modification of coal tar pitch only by using a chemical reaction catalyst, the process is simple, the modification effect is good, the modified coal tar pitch is easy to spin and carbonize, and the purpose of preparing high-quality coal pitch as a carbon fiber precursor is successfully achieved.

Description

technical field [0001] The invention belongs to the technical field of high-strength carbon fiber preparation, and in particular relates to a method for chemically modifying carbon fiber precursor coal tar pitch. Background technique [0002] The raw material for preparing carbon fiber is a substance with high carbon content. The commercial prospects are polyacrylonitrile and asphalt. Asphalt is the residue after processing carbon petrochemicals, and can be divided into petroleum asphalt and coal-based asphalt according to the source. Coal tar pitch is a large by-product in the coal coking industry. Only by deep processing of coal tar pitch can the petrochemical resources of carbon be fully utilized. Coal polygeneration technology is a new technology that maximizes the use of coal resources, but this technology also has a large amount of waste in the processing process that cannot be solved-coal tar pitch. Only when the outlet of polygeneration residues is solved, can coa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10C3/02
Inventor 徐国财王雪礼李欣李少冰张晓梅朱宗君唐军
Owner 徐国财
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