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Preparation method of catalyzed synthesis of mesophase pitch

A mesophase asphalt and asphalt technology, which is applied in the field of catalytic synthesis of mesophase asphalt, can solve the problems of difficult catalyst recovery, harsh reaction conditions, and strong corrosion of equipment, and achieve process safety and environmental protection. Cost reduction, simple recycling, and potential safety hazards Reduced effect

Active Publication Date: 2017-03-15
湖南东映碳材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention mainly aims at problems such as harsh reaction conditions, strong corrosion to equipment, high cost, and difficulty in catalyst recovery existing in the existing method for catalytically synthesizing mesophase pitch, and provides a mesophase pitch with simple process, mild reaction conditions and high product purity. Preparation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A preparation method for catalytically synthesizing mesophase pitch, comprising the following steps:

[0026] (1) Put ethylene tar pitch and refined naphthalene with a softening point of 30°C, 0% toluene insoluble matter, and 0.005% ash content in a mass ratio of 3:2 into a low-pressure low-temperature reactor, and the filling volume ratio is 40%.

[0027] (2) Fill the catalyst boron trifluoride into the low-pressure low-temperature reactor according to the mass ratio of 2:5 to the reaction material, heat at 200°C, control the pressure at 1.5MPa, and react for 10 hours.

[0028] (3) After the reacted material is cooled, take it out and remove the liquid phase components. Pyridine was added to the solid phase component at twice the molar number of boron trifluoride, heated to 100°C, and the solid generated by the reaction was filtered out.

[0029] (4) Pass the filtered material into a negative pressure reactor, control the temperature at 300°C, stir at 600rpm, argon fl...

Embodiment 2

[0032] A preparation method for catalytically synthesizing mesophase pitch, comprising the following steps:

[0033] (1) Put coal tar pitch and durene with a softening point of 90°C, 0.01% toluene insoluble matter, and 0.01% ash content into a low-pressure low-temperature reactor at a mass ratio of 1:1, and the filling volume ratio is 50%.

[0034] (2) Fill the catalyst boron trifluoride into the low-pressure low-temperature reactor at a mass ratio of 1:4 to the reaction material, heat at 190°C, control the pressure at 1.2MPa, and react for 5 hours.

[0035] (3) After the reacted material is cooled, take it out and remove the liquid phase components. Pyridine was added to the solid phase component according to 3 times the mole number of boron trifluoride, heated to 150°C, and the solid generated by the reaction was filtered out.

[0036] (4) Pass the filtered material into a negative pressure reactor, control the temperature at 330°C, stir at 1000rpm, argon flow at 1.2L / kg.mi...

Embodiment 3

[0039] A preparation method for catalytically synthesizing mesophase pitch, comprising the following steps:

[0040](1) Put liquid catalytic cracking oil slurry with 0% toluene insoluble matter and 0.01% ash content and methylnaphthalene in a mass ratio of 4:1 into a low-pressure low-temperature reactor, and the filling volume ratio is 50%.

[0041] (2) Fill the catalyst boron trifluoride into a low-pressure low-temperature reactor at a mass ratio of 1:5 to the reaction material, heat at 200°C, and control the pressure at 2MPa, and react for 15 hours.

[0042] (3) After the reacted material is cooled, take it out and remove the liquid phase components. Pyridine is added to the solid phase component according to 1.5 times the mole number of boron trifluoride, heated to 100°C, and the solid generated by the reaction is filtered out.

[0043] (4) Pass the filtered material into a negative pressure reactor, control the temperature at 340°C, stir at 500rpm, argon flow at 0.4L / kg.m...

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Abstract

The invention relates to a preparation method of catalyzed synthesis of mesophase pitch. The method comprises the steps that catalytic polymerization of purified pitch, a pure aromatic compound and boron trifluoride or boron trifluoride diethyl etherate, the catalyst boron trifluoride etherate or boron trifluoride are added into a low-temperature reaction kettle according to the reaction mass ratio being 1:100-1:200, the heating temperature is 100-260 DEG C, the pressure is controlled to 0.5-2 Mpa to perform a reaction, pyridine is added into a cooled solid phase component, the temperature is increased to 100-150 DEG C, solids generated in the reaction are filtered out, and boron trifluoride is removed to obtain high-purity polymerized pitch; then, further thermal polymerization and micromolecule removal are performed to obtain the mesophase pitch. The reaction controllability is good, the catalyst is good in safety, the pitch can be recycled, and a polytetrafluoroethylene liner and a graphite liner are adopted to obtain the high-quality synthesis mesophase pitch. The problem that a catalyst existing in an existing method of catalytic synthesis of mesophase pitch is large in toxin and hard to remove is solved.

Description

technical field [0001] The invention belongs to the technical field of synthetic asphalt preparation methods, and in particular relates to a preparation method for catalytically synthesizing mesophase asphalt. Background technique [0002] Mesophase pitch is an indispensable raw material for the preparation of high-performance carbon materials, whether it is high-performance carbon fiber, needle coke, high-end negative electrode materials, high-density C / C composites, isostatic graphite, etc., are all restricted by the performance of raw materials. The raw materials of high-performance carbon materials generally require mesophase pitch to have the characteristics of high carbon yield and good fluidity, and then require less heteroatoms other than C and H, low ash content, high aromaticity, low condensation degree, H / C It has the characteristics of high ratio, neat molecular planarity, and narrow molecular weight distribution. [0003] Asphalt prepared by ordinary thermal po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10C3/02
CPCC10C3/026
Inventor 李轩科伍孝郭建光沈威威张福全刘金水
Owner 湖南东映碳材料科技股份有限公司
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