A kind of preparation method of mesophase pitch

A technology based on mesophase pitch and time, which is applied in the field of preparation of new carbon materials, can solve problems such as the difficulty in realizing the industrialization of high-quality mesophase pitch preparation, the combination method, the results obtained during the operation process are not up to expectations, and the separation of low components is difficult. Excellent spinnability, high mesophase content, moderate softening point

Active Publication Date: 2021-11-05
湖南东映碳材料科技股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this type of method is still cumbersome, and the stability control is difficult, especially the separation of low components in mesophase pitch, which limits the application of co-carbonization, especially the development of high-performance carbon fiber.
[0010] Some scholars have also tried to combine several methods such as hydrogenation reduction, co-carbonization, and sedimentation separation to carry out research on the preparation of mesophase pitch, but the combination method, operation process, and results are not up to expectations, and it is difficult to achieve high-quality mesophase pitch preparation. industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0058] The invention provides a kind of preparation method of mesophase pitch, comprising the following steps:

[0059]Raw material A is subjected to primary polymerization in an inert atmosphere at a temperature of 380°C to 420°C to obtain raw material B; raw material B is subjected to secondary polymerization in an inert atmosphere at a temperature of 380°C to 420°C to obtain raw material C ; The raw material C is aged in an inert atmosphere at a temperature of 320-360° C. to obtain the mesophase pitch; the raw material A is composed of petroleum pitch, ethylene tar pitch or heavy aromatic components of catalytic cracking oil slurry One or more of them are obtained after heat treatment; said S2 includes that when the viscosity of the reaction system of the secondary polymerization reaction is greater than or equal to 0.1 Pa·s, the viscosity of the reaction system of the secondary polymerization reaction is adjusted to be less than 0.1 by adding a viscosity reducer Pa·s steps...

Embodiment 1

[0062] The catalytic cracking oil slurry is subjected to vacuum rectification in a vacuum tower, and the fraction with a boiling point between 238-420° C. is cut to prepare 50 kg of viscosity reducer. After testing, the TI content of the viscosity reducer is 0.005%, the QI content is 0, the C / H value is 9.2, the S content is 0.38%, the N content is 0.36%, the colloid content is 3.5%, and the asphaltene content is 0.2%.

[0063] Take 400kg of petroleum asphalt with a softening point of 100°C after the purification treatment as raw material A, put it into a 500L primary polymerization reactor, and carry out the primary polymerization reaction under nitrogen protection at 400°C for 8 hours to obtain a softening point of 212°C. Raw material B with an AC content of 28%, a TI content of 46%, and a QI content of 10%.

[0064] Take 150kg of raw material B, put it into a 200L secondary polymerization reactor, 3 / (h·kg) and 410°C for secondary polymerization. At the beginning of the s...

Embodiment 2

[0067] The catalytic cracking oil slurry was rectified under vacuum in a vacuum tower, and the fraction with a boiling point of 242-420°C was cut to prepare 50kg of viscosity reducer. After testing, the TI content of the viscosity reducer is 0.008%, the QI content is absent, the C / H value is 9.6, the S content is 0.41%, the N content is 0.42%, the colloid content is 4%, and the asphaltene content is 0.28%.

[0068] Take 400kg of purified petroleum asphalt with a softening point of 100°C as raw material A, put it into a 500L first-stage polymerization reactor, and conduct a first-stage polymerization reaction under nitrogen protection at 410°C for 8 hours to obtain a softening point of 228°C and an AC content of 33 %, TI content 51%, QI content 12% raw material B.

[0069] Take 150kg of raw material B, put it into a 200L secondary polymerization reactor, 3 / (h·kg) and 415°C for secondary polymerization. At the beginning of the secondary polymerization reaction, the viscosity ...

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Abstract

The invention discloses a preparation method of mesophase pitch, which comprises the following steps: S1 performing primary polymerization of raw material A in an inert atmosphere at a temperature of 380°C to 420°C to obtain raw material B; S2 making raw material B in an inert atmosphere, At a temperature of 380°C to 420°C, a secondary polymerization reaction is carried out to obtain raw material C; S3, the raw material C is subjected to an aging reaction in an inert atmosphere at a temperature of 320°C to 360°C to obtain the mesophase pitch; the raw material A Obtained by heat treatment of one or more of petroleum asphalt, ethylene tar pitch or heavy aromatic components of catalytic cracking oil slurry; the S2 includes when the viscosity of the reaction system of the secondary polymerization reaction is greater than or equal to 0.1Pa·s , the step of adjusting the viscosity of raw material B to less than 0.1 Pa·s by adding a viscosity reducer.

Description

technical field [0001] The invention relates to a preparation method of mesophase pitch, which belongs to the field of preparation of new carbon materials. Background technique [0002] The 21st century is called the "super carbon era". As the basic raw material of high-end carbon materials, high-quality mesophase pitch is the core competitiveness of occupying the commanding heights of advanced carbon materials. It is widely used in high thermal conductivity / high modulus pitch-based carbon fibers, high Preparation of thermally conductive foamed carbon, ultra-high specific surface area porous carbon, high-performance electrode and negative electrode materials, etc. [0003] Accelerating the industrialization of high-quality mesophase pitch and expanding the scope of application are not only the requirements of national innovation and development, local industrial structure adjustment, transformation and upgrading, but also the urgent needs of major areas of the national econo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C10C3/10
CPCC10C3/10
Inventor 叶崇陈坤余洋伍孝石奎黄东刘金水
Owner 湖南东映碳材料科技股份有限公司
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