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Preparation method of low-ash mesophase pitch

A technology of mesophase pitch and low ash content, which is applied in the field of preparing mesophase pitch by thermal polymerization, can solve the problems of difficulty in purifying coal pitch, and achieve the effects of low raw material cost, low energy consumption and enhanced flexibility

Inactive Publication Date: 2017-02-01
HANGZHOU INST OF ADVANCED MATERIAL BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problem that coal tar pitch is difficult to purify, the present invention selects coal tar as a raw material, and starts to purify directly from coal tar

Method used

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  • Preparation method of low-ash mesophase pitch
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  • Preparation method of low-ash mesophase pitch

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Example 1: Gravity sedimentation of coal tar in a constant temperature water bath at 75°C for 4h, and then centrifuged at a speed of 5000r / min for 3min, after centrifugation, filtered through a filter with a pore size of 2 microns, and then kept at 80°C for 1h while stirring Demulsification treatment, then heating to 120°C to remove water and ammonium salts, the measured ash content of the purified coal tar is 0.0075%. Put 400ml of purified coal tar into a reactor with a capacity of 1L, blow nitrogen to remove the air, then continue to blow nitrogen to make the initial pressure inside the reactor reach 1Mpa, set the temperature at 4°C / min to 400°C, and at the same time, set the temperature at 400r / min. Stir at a speed of 1 min, the pressure changes with the change of temperature, and keep warm for 5 hours. After the heat preservation is over, release the pressure, blow nitrogen for 20 minutes to remove light components, stop stirring, and cool to obtain purified coal tar...

Embodiment 2

[0013] Example 2: The gravity settling time of coal tar was extended to 12 hours, and other conditions were the same as in Example 1. The yield of mesophase pitch obtained was 42%, the softening point was 230°C, the mesophase content was 98%, and the ash content was 50ppm.

Embodiment 3

[0014] Example 3: The gravity settling time of coal tar was extended to 24 hours, and the other conditions were the same as in Example 1. The softening point of the obtained mesophase pitch was 230° C., the mesophase content was 98%, and the ash content was 45 ppm.

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Abstract

The invention provides a preparation method of low-ash high-property mesophase pitch. The method comprises the steps that the raw material coal tar is purified, a fraction is put into a reaction kettle, temperature programming and heat preservation are conducted in sequence, and purified coal tar pitch is obtained. The purified coal tar pitch and a co-carbonization agent are mixed, the mixture is added into a high pressure reactor, under certain pressure condition, the temperature is increased to a certain temperature, then heat preservation is conducted, and the mesophase pitch is obtained. According to the method, a series of physical methods such as gravity settlement centrifugation and circulating filtration are adopted to purify the coal tar, the very good effect of removing ash impurities is achieved, quinoline insoluble matter formed by mesophase is especially hindered, the content of the mesophase pitch ash is lower than 50 ppm, the content of mesophase reaches up to 100%, and carbon fibers with excellent properties can be prepared continuously; meanwhile, by mixing the pitch with the co-carbonization agent, the rheological property of the mesophase pitch is improved. Compared with a coal tar pitch purification process, the coal tar purification technology is simple, the cost is low, and the high-purity purified coal tar pitch can be obtained through preparation, so that the low-ash high-property mesophase pitch is obtained.

Description

technical field [0001] The invention relates to the preparation of mesophase pitch by thermal polymerization, in particular to the purification of coal tar and the preparation of mesophase pitch by co-carbonization. Background technique [0002] Mesophase pitch is a typical carbonaceous mesophase raw material, which is the necessary stage to obtain graphitized carbon materials. Mesophase pitch has properties such as high carbonization yield and easy graphitization, and is widely used in the preparation of high value-added carbon materials such as pitch-based carbon fibers, graphite fibers, carbon / carbon composites, and needle coke for ultra-high-power electrodes. [0003] Coal tar pitch, petroleum pitch and pure aromatic compounds are the main raw materials for preparing mesophase pitch. Although pure aromatic compounds have low heteroatom content, single composition structure, convenient molecular structure design, regular molecular structure, narrow molecular weight distr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10C1/00C10C1/02C10C1/20C10C3/02
CPCC10C1/00C10C1/02C10C1/20C10C3/02
Inventor 马兆昆黄琪曹瑞雄宋怀河
Owner HANGZHOU INST OF ADVANCED MATERIAL BEIJING UNIV OF CHEM TECH
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