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Method for preparing high-quality mesophase pitch by ternary co-carbonization

A technology of mesophase pitch and co-carbonization, which is applied in the processing of tar pitch/petroleum pitch/natural pitch, chemically processing tar pitch/petroleum pitch/natural pitch, petroleum industry, etc. Energy consumption, expensive additives and other problems, to achieve the effect of less impurity ash content, increased reactivity, and improved optical appearance

Pending Publication Date: 2019-07-12
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the catalytic hydrogenation process complicates the production process, greatly increases the production cost, and the catalyst is difficult to remove, resulting in high ash content in the product, which adversely affects the performance of subsequent carbon materials
Another example is the patent CN103923681A, which uses coal liquefaction refined asphalt as raw material, uses coking heavy oil, self-washing oil, anthracene oil and other coal tar deep-processed products as additives, and prepares mesophase pitch by co-carbonization method, although the viscosity of the system is reduced and the system is improved. fluidity, but at the same time it also prolongs the polymerization reaction time and increases energy consumption, and the addition of various oils will also introduce some impurities, which will increase the ash content of the product and cause adverse effects on subsequent processing
The patent CN103923682A uses coal liquefaction refined asphalt as raw material, high molecular polymer as additive, and co-carbonization method to prepare mesophase pitch. Although the fluidity of the system has been improved and streamlined mesophase pitch has been obtained, the molecular structure of these additives It is very different from the polycyclic aromatic hydrocarbons in asphalt. After a series of treatments such as molding, carbonization and graphitization, defects such as pores may appear
Patent CN108485694A uses refined coal tar pitch as raw material and mesophase pitch as additive to prepare high-quality mesophase pitch through co-carbonization method. Although the reaction process is accelerated and a wide-area streamlined mesophase pitch product is obtained, the price of the additive is expensive and the production higher cost

Method used

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  • Method for preparing high-quality mesophase pitch by ternary co-carbonization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Put 400g of refined coal tar pitch raw material and 0.04g of graphene into a mixer for thorough mixing, then put the mixed powder and 10.59mL of tetrahydronaphthalene into a high-temperature and high-pressure reactor, blow nitrogen into it to purge and replace the air three times, and then seal the chamber. Describe the reactor, blow nitrogen into the reactor until the initial pressure is 0.2MPa, raise the temperature to 420°C at a rate of 2°C / min, start stirring when the temperature is greater than 120°C, the stirring rate is 350rmp, when the temperature rises to 420°C Keep warm for 10 hours. During the reaction, keep a closed constant pressure of 1.0MPa, and keep stirring at a constant speed. After the heat preservation is over, release the pressure, purging nitrogen for 30 minutes to remove light components, stop stirring, and cool to room temperature to obtain a wide-area streamlined mesophase pitch product with a softening point of 260°C, a mesophase content of up ...

Embodiment 2

[0031] Increase the quality of adding graphene from 0.04g to 0.12g, other conditions are the same as in Example 1, the softening point of the wide-area streamlined mesophase pitch product obtained is 256°C, the mesophase content is as high as 97%, and the quinoline insoluble content is 33wt %.

Embodiment 3

[0033] The quality of adding graphene is increased from 0.04g to 0.20g, and other conditions are the same as in Example 1. The softening point of the wide-area streamlined mesophase pitch product obtained is 252°C, the mesophase content is as high as 98%, and the quinoline insoluble content is 34wt %.

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Abstract

The invention discloses a method for preparing high-quality mesophase pitch by ternary co-carbonization, and belongs to the technical field of deep processing of coal tar pitch. The method is characterized in that the high-quality mesophase pitch is prepared from a small amount of graphene and a hydrogen supply reagent as additives and refined coal pitch as a raw material. The method comprises thesteps as follows: firstly, refined coal tar pitch powder and a small amount of graphene are put into a mixer to be evenly mixed, and then the mixed powder and the hydrogen supply reagent are put intoa high temperature and high pressure reactor to be subjected to direct thermal polymerization, and the high-quality mesophase pitch product is obtained. Formation of mesophase pitch in the reactor isobviously accelerated by addition of a small amount of graphene and the hydrogen supply reagent, so that the reaction temperature required for formation of the mesophase pitch from the refined coal pitch is reduced, and time is shortened. The mesophase content of the obtained product is as high as 80% or higher, the optical structure of the product is wide-area streamlined, and the product has low softening point and good spinnability, and can be used for preparing high-end carbon materials such as high-performance carbon fiber and high-heat conducting foam carbon.

Description

technical field [0001] The present invention relates to a preparation method of high-performance mesophase pitch, specifically a method for preparing high-quality coal-based mesophase pitch by using a small amount of graphene and a hydrogen-donating agent as additives and using refined coal tar pitch as a raw material through co-carbonization The method belongs to the technical field of coal tar pitch deep processing. Background technique [0002] Refined coal tar pitch is the product obtained by purification of medium temperature coal tar pitch. It not only has a very low ash content but also maintains a high degree of aromaticity, and is easy to polycondensate to form mesophase pitch. Compared with traditional coal tar pitch and petroleum pitch, the intermediate phase prepared by refined coal tar pitch is purer. Compared with artificially synthesized pure pitch, the source of raw materials is wide and the cost is low. It is a kind of preparation of mesophase pitch and then...

Claims

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Application Information

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IPC IPC(8): C10C3/02
CPCC10C3/023
Inventor 马兆昆张型伟宋怀河
Owner BEIJING UNIV OF CHEM TECH
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