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Preparation method of microstructure-controllable coal pitch-based carbon material

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

Active Publication Date: 2021-03-09
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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  • Preparation method of microstructure-controllable coal pitch-based carbon material
  • Preparation method of microstructure-controllable coal pitch-based carbon material
  • Preparation method of microstructure-controllable coal pitch-based carbon material

Examples

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Effect test

Embodiment 1

[0026] Embodiment 1 (comparative example 1)

[0027] First, take 100g of medium-temperature coal tar pitch, add it into the reaction kettle and raise the temperature to 180°C, stir and react for 0.5h under the protection of nitrogen, and cool to room temperature after completion; The temperature was raised to 1100 °C for 3 hours, and the untreated coal tar pitch-based carbon material was obtained. The 002 layer spacing of the untreated coal tar pitch-based carbon material was 0.355 nm in XRD.

Embodiment 2

[0028] Embodiment 2 (comparative example 2)

[0029] First, take 0.3g of imidazoline naphthenic acid and 100g of medium-temperature coal tar pitch, add them to the reactor and heat up to 180°C, stir and react for 0.5h under the protection of nitrogen, and cool to room temperature after the end; put the above-mentioned pretreated coal tar pitch into the carbonization furnace, Under an argon atmosphere, the temperature was raised to 1100°C at 0.5°C / min, and carbonized at high temperature for 3h to obtain naphthenic acid pretreated coal tar pitch-based carbon materials. figure 1 It is the SEM figure after carbonization of coal tar pitch in embodiment 1, figure 2 This is the SEM image of coal tar pitch carbonized by naphthenic acid imidazoline pretreatment. The morphology of the carbon material does not change significantly before and after treatment, and no layered structure appears; is 0.353nm.

Embodiment 3

[0031] Step 1: First, take 0.3g of imidazoline naphthenate and 100g of medium-temperature coal tar pitch, add them into the reaction kettle and raise the temperature to 180°C, stir and react for 0.5h under the protection of nitrogen, and cool to room temperature for later use.

[0032]Step 2: Take 50g of naphthenic acid imidazoline pretreated coal tar pitch and 20g of styrene, add them to the reaction kettle, raise the temperature to 140°C under the protection of nitrogen, and after constant temperature reaction for 6 hours, heat up to 200°C and distill under reduced pressure until no monomer remains , The monomer conversion rate of the in-situ polymerization reaction 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 a high temperature for 2 hours to obtain a polystyrene-modified coal tar pitch-based carbon material. image 3 It...

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Abstract

The invention discloses a preparation method of a microstructure-controllable coal pitch-based carbon material, and belongs to the field of polymer chemical industry, coal chemical industry and carbonmaterial preparation processes. The method comprises the following steps of: shielding or removing interference of carbonyl, aldehyde group and the like in coal pitch on free radical polymerization reaction by using a reducing agent; co-dissolving the coal pitch and a monomer, forming a bulk solution polymerization system by taking the coal pitch as a solute, and performing thermal initiation bulk polymerization to prepare polymer modified coal pitch; carrying out reduced pressure distillation to remove monomer residuals and light components to obtain high-softening-point polymer modified coal pitch; and performing program carbonization on the high-softening-point polymer modified coal pitch to obtain coal pitch-based carbon materials with different morphological structures. With the method of the invention adopted, the problem that a pure polymer is difficult to disperse in a single chain segment of a coal pitch system is solved; a coal pitch-based precursor is improved; the problemthat just a single carbonization regulation and control method exists is solved; the requirement of refinement of high-molecular modified coal pitch is met; the preparation of a carbon material structure is controllable; and a new method and a new thought are provided for preparation of a high-performance carbon functional material.

Description

technical field [0001] The invention relates to the technical fields of polymer chemical industry, coal chemical industry and carbon material, and relates to a preparation method of coal tar 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 quality of coal tar. Coal tar pitch is one of the precursors for the synthesis of various functional carbon materials due to its high residual carbon, abundant sources, and low cost. Due to the complex components of coal tar pitch, during the carbonization process, when the pitch molecules are pyrolyzed and polycondensed at high temperature, not only a planar structure is formed between molecules, but also a crosslinking reaction occurs between layers, which will eventually make The structure of the carbonized material is interwoven in a network shape, and there is a disordered and disordered structure...

Claims

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Application Information

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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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