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A preparation method of coal tar pitch-based carbon material with controllable microscopic morphology

A technology of microscopic morphology and coal tar pitch, which is applied in the field of preparation of coal tar pitch-based carbon materials, can solve problems such as good structural orientation of carbon materials, low expansion rate, and difficulty in single-segment dispersion

Active Publication Date: 2022-05-20
DALIAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method of the coal tar pitch-based carbon material precursor can solve the problem of difficult dispersion of polymers in the coal tar pitch system, and increase the coal tar pitch as the means and method of the carbon-based material precursor, and the prepared carbon material has a structural orientation Good singleness, low expansion rate, excellent electrical conductivity

Method used

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  • A preparation method of coal tar pitch-based carbon material with controllable microscopic morphology
  • A preparation method of coal tar pitch-based carbon material with controllable microscopic morphology
  • A preparation method of coal tar pitch-based carbon material with controllable microscopic morphology

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Effect test

Embodiment 1

[0026] Example 1 (Comparative Example 1)

[0027] First, take 100g of medium-temperature coal tar pitch, add it to the reaction kettle and heat it up to 180°C, stir and react under nitrogen protection for 0.5h, and cool down to room temperature after the end; Min heating to 1100 ℃, high temperature carbonization for 3 hours, to obtain untreated coal tar-based carbon material, the 002 layer spacing of untreated coal tar-based carbon material XRD is 0.355nm.

Embodiment 2

[0028] Example 2 (Comparative Example 2)

[0029] First, take 0.3 g of naphthenic acid imidazoline and 100 g of medium-temperature coal tar pitch, add them to the reaction kettle and heat up to 180 ° C, stir and react under nitrogen protection for 0.5 h, and then cool to room temperature after completion; put the above-mentioned pretreated coal tar pitch into the carbonization furnace, Under argon atmosphere, the temperature was raised to 1100°C at 0.5°C / min, and carbonized at high temperature for 3 hours to obtain naphthenic acid pretreated coal tar-based carbon material. figure 1 It is the SEM image after carbonization of coal pitch in Example 1, figure 2 This is the SEM image after carbonization of coal tar pitch pretreated with naphthenic acid imidazoline. The morphology of carbon materials before and after treatment has no obvious change, and no layered structure appears. is 0.353nm.

Embodiment 3

[0031] Step 1: First, take 0.3 g of naphthenic acid imidazoline and 100 g of medium-temperature coal tar pitch, add them to the reaction kettle and heat up to 180 ° C, stir and react for 0.5 h under nitrogen protection, and cool to room temperature after completion.

[0032]Step 2: Take 50 g of naphthenic acid imidazoline pretreated coal tar pitch and 20 g of styrene, add them into the reaction kettle, heat up to 140°C under nitrogen protection, and after 6 hours of constant temperature reaction, heat up to 200°C and distill under reduced pressure until no monomer remains. , the monomer conversion rate of in-situ polymerization was 50.2%.

[0033] Step 3: Put the polymer modified coal tar pitch obtained above into a carbonization furnace, raise the temperature to 1100° C. at 0.5° C. / min in an argon atmosphere, and carbonize at high temperature for 2 hours to obtain a polystyrene-modified coal tar pitch-based carbon material. image 3 This is the SEM image of the carbonized pol...

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Abstract

A preparation method of a coal pitch-based carbon material with controllable microscopic appearance belongs to the fields of polymer chemical industry, coal chemical industry and carbon material preparation technology. First, use a reducing agent to shield or remove the interference of carbonyl and aldehyde groups in the coal tar pitch to the free radical polymerization reaction; co-dissolve the coal tar pitch with the monomer, and use the coal tar pitch as a solute to form a bulk solution polymerization system, and conduct thermally induced bulk polymerization to prepare the polymerization modified coal tar pitch; vacuum distillation to remove residual monomers and light components to obtain high softening point polymer modified coal tar pitch; program carbonization of high softening point polymer modified coal tar pitch to obtain different morphological structures coal tar-based carbon materials. The invention solves the problem that the single-segment dispersion of the pure polymer is difficult in the coal tar pitch system, and simultaneously improves the coal tar pitch-based precursor and the problems of a single carbonization control method, and realizes the requirement for the refinement of the polymer modified coal tar pitch. The controllable preparation of the material structure provides new methods and new ideas for the preparation of high-performance carbon functional materials.

Description

technical field [0001] The invention relates to the technical fields of polymer chemical industry, coal chemical industry and carbon materials, and relates to a preparation method of a coal pitch-based carbon material with controllable microscopic appearance. Background technique [0002] Coal tar pitch is a by-product of coal tar processing, accounting for 55% to 65% of the coal tar mass. Coal tar pitch has high residual carbon, abundant sources and low cost, and is one of the precursors for the synthesis of various functional carbon materials. Due to the complex composition of coal tar pitch, in the carbonization process, when the pitch molecules undergo pyrolysis and polycondensation at high temperature, not only a planar structure is formed between molecules, but also a cross-linking reaction occurs between layers, which will eventually cause The structure of carbonized material is interwoven in a network, and there are disordered layers and disordered structural states...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/05
CPCC01B32/05Y02E60/10
Inventor 申凯华李茂辉鲍方健聂健夫
Owner DALIAN UNIV OF TECH
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