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Polymerizing-pyrolytic method for preparing mesocarbon microbead in asphaltic base

A mesophase carbon microsphere and pitch-based technology, which is applied in the field of carbon materials, can solve the problems of low yield, uneven shape and size, and low preparation cost of mesophase carbon microspheres, and achieve easy operation, wide application, and particle size The effect of uniform diameter distribution

Inactive Publication Date: 2010-03-10
FUZHOU UNIVERSITY
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Problems solved by technology

[0003] The purpose of the present invention is to provide a kind of polymerization pyrolysis method to prepare pitch-based mesophase carbon microspheres, to solve the problems of low yield, high cost, uneven shape and size, environmental pollution and other problems of mesophase carbon microspheres in the prior art. The inventive method has high preparation yield, controllable particle size, uniform size, good sphericity and low preparation cost

Method used

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  • Polymerizing-pyrolytic method for preparing mesocarbon microbead in asphaltic base
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  • Polymerizing-pyrolytic method for preparing mesocarbon microbead in asphaltic base

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Embodiment 1

[0039] Coal tar pitch is used as raw material, formaldehyde is used as cross-linking agent, oxalic acid is used as catalyst, and the mass ratio of the three is 100:4:2. Add it into a three-necked flask. Before 100°C, the temperature is raised freely, and after 100°C, the speed is 5°C / min. The temperature is raised, and N is introduced from the beginning of the temperature rise 2 , N 2 The flow rate was 50mL / min, and the reaction was carried out at 130°C for 2h, and the obtained polymerized modified bitumen was 2 Treated at 420°C for 2 hours under protection, then dissolved by pyridine (the mass ratio of pyridine to pyrolysis product is 60:1) and extracted until colorless, and dried in vacuum to obtain mesophase carbon microspheres with a particle size of about 8 μm. The yield is 30.74%. Good sphericity and narrow particle size distribution.

Embodiment 2

[0041] Coal tar pitch is used as raw material, benzaldehyde is used as cross-linking agent, and p-toluenesulfonic acid is used as catalyst, and the mass ratio of the three is 100:12:2. / min rate of heating, and from the beginning of heating N into 2 , N 2 The flow rate was 50mL / min, and the reaction was carried out at 130°C for 3h, and the obtained polymerized modified bitumen was 2 Treat at 460°C for 2 hours under protection, then extract to colorless with pyridine (the mass ratio of pyridine to pyrolysis product is 60:1), and dry in vacuum to obtain mesophase carbon microspheres with a particle size of about 12 μm. The rate is 40.62%. The sphericity is good, and the fusion between carbon microspheres rarely occurs.

Embodiment 3

[0043] Coal tar pitch is used as raw material, p-tolualdehyde is used as cross-linking agent, oxalic acid is used as catalyst, and the mass ratio of the three is 100:8:2. / min rate of heating, and from the beginning of heating N into 2 , N 2 The flow rate was 50mL / min, and the reaction was carried out at 140°C for 2h, and the obtained polymerized modified bitumen was 2 Treat at 450°C for 1 h under protection, then extract to colorless with pyridine (the mass ratio of pyridine to pyrolysis product is 60:1), and dry in vacuum to obtain mesophase carbon microspheres with a particle size of about 10 μm. The rate is 35.54%. Good sphericity, good surface finish, and little fusion between balls.

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Abstract

The invention provides a polymerizing-pyrolytic method for preparing a mesocarbon microbead of asphaltic base, which solves the problems that in the prior art, the mesocarbon microbead has low yield,high cost, uneven shape and size and environmental pollution and the like. The polymerizing-pyrolytic method is used for preparing the mesocarbon microbead of asphaltic base, and the raw materials used for preparation comprise a basic material, a cross-linking agent and a catalyst, and the mesocarbon microbead of asphaltic base is prepared by processes of preparation of the raw materials, polymerization reaction, pyrolytic reaction, and separation and drying of pyrolysis products. The preparation method has high yield, controllable particle size, even size, good sphericity and low preparationcost.

Description

technical field [0001] The invention belongs to the field of carbon materials, and mainly relates to the preparation of pitch-based mesophase carbon microspheres by a polymerization pyrolysis method. Background technique [0002] Since the discovery of mesophase carbon microspheres by Brooks and Taylor in the 1960s, people have done a lot of research on their formation mechanism, structure, performance and application. As a high-quality precursor of advanced carbon materials, mesophase carbon microspheres have attracted great attention. Mesophase carbon microspheres have the characteristics of narrow particle size distribution, high density, high strength, good thermal stability, stable chemical properties, good electrical conductivity, excellent self-sintering property, and high carbon residue rate, and are considered to be the best choice for preparing high-performance carbon materials. High-quality precursors. At present, it has been used to prepare high-density and hig...

Claims

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Application Information

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IPC IPC(8): C01B31/02
Inventor 林起浪柯余良张高校
Owner FUZHOU UNIVERSITY
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