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A kind of preparation method of isotropic high softening point coal tar pitch

A high softening point, isotropic technology, applied in chemical processing of tar pitch/petroleum pitch/natural pitch, and selective extraction of tar pitch/petroleum pitch/natural pitch, etc. The stability of properties is difficult to control, the pitch-based carbon fibers are broken or woolly, and the application effect is affected, so as to achieve the effects of low toluene soluble content, narrow molecular weight distribution, and short reaction time.

Active Publication Date: 2021-04-02
EAST CHINA UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

2) Although the higher the QI content, the higher the residual carbon rate of high softening point coal tar pitch will be, but its rheological properties in the liquefied state will become worse during use, which will affect its practical application effect
3) Affected by factors such as thermal field distribution, gas distribution and high viscosity of the oxidation reactor, the stability of the physical and chemical properties of high softening point coal tar pitch is difficult to control
4) Since there is no domestic centrifugal equipment capable of deashing at a temperature of 250-350°C, the ash content of high softening point coal tar pitch is higher than 500ppm, and the metal components in these ash will be released in downstream products (such as pitch-based carbon fiber) In the process of high temperature carbonization (800~1600℃), it plays the role of catalyst and causes some negative effects, such as the production of pitch-based carbon fiber is prone to broken wires or hairs, etc.

Method used

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  • A kind of preparation method of isotropic high softening point coal tar pitch
  • A kind of preparation method of isotropic high softening point coal tar pitch
  • A kind of preparation method of isotropic high softening point coal tar pitch

Examples

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Effect test

Embodiment 1

[0024] Using medium-temperature coal tar pitch with a softening point of 75°C, a QI content of 5.2%, and an ash content of 1358ppm as a raw material, the medium-temperature coal tar pitch is liquefied at 150°C by a disc centrifuge and then centrifuged at a speed of 8000 rpm , the QI and ash content of the medium temperature coal tar pitch were reduced to 0.2% and 56ppm respectively, and the modified medium temperature coal tar pitch with a softening point of 81°C was obtained.

Embodiment 2

[0026] With 500g [embodiment one] modified medium temperature coal tar pitch, 60g sulfuric acid and 100g iodine pentoxide (I 2 o 5 ) are simultaneously placed in a 5-liter high-pressure reactor, and after sealing, feed 99.999% high-purity nitrogen until the pressure in the kettle reaches 0.5MPa. The temperature in the kettle was raised to 180° C. at a heating rate of 3° C. / min, and the stirring was continued for 3 hours at a rotating speed of 145 r / min to obtain coal tar pitch with a high softening point. The prepared high softening point coal tar pitch was extracted with methanol at 50°C for 2 hours. After drying, the obtained isotropic high softening point coal tar pitch had a softening point of 267°C, a residual carbon rate of 76.4%, and a toluene soluble content of 6.6%. , the toluene insoluble-quinoline soluble content is 89.7%, the quinoline insoluble content is 3.7%, the ash content is 79ppm, and the molecular structure of the prepared high softening point coal tar pit...

Embodiment 3

[0028] With 500g [embodiment one] modified medium temperature coal tar pitch, 60g sulfuric acid and 200g iodine pentoxide (I 2 o 5 ) are simultaneously placed in a 5-liter high-pressure reactor, and after sealing, feed 99.999% high-purity nitrogen until the pressure in the kettle reaches 0.5MPa. The temperature in the kettle was raised to 180° C. at a heating rate of 3° C. / min, and the stirring was continued for 3 hours at a rotating speed of 145 r / min to obtain coal tar pitch with a high softening point. The prepared high softening point coal tar pitch was extracted with methanol at 50°C for 2 hours. After drying, the softening point of the obtained high softening point coal tar pitch was 282°C, the residual carbon rate was 77.5%, the ash content was 74ppm, and the molecular structure was isotropic. Same-sex structure ( figure 2 ) and a narrow molecular weight distribution. Among them, the toluene soluble content is 5.4%, the toluene insoluble-quinoline soluble content is...

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Abstract

The invention discloses a preparation method of isotropic coal pitch with a high softening point. The method comprises the following steps: 1) removing ash and quinoline insolubles in medium-temperature coal pitch by using a disc centrifuge to obtain modified medium-temperature coal pitch; 2) reacting the modified medium-temperature coal pitch at 120-180 DEG C based on an electrophilic iodinationassistance technology for 2-4 h with chemical reagents such as sulfuric acid as a catalyst to prepare coal pitch with the high softening point; and (3) removing light components in the prepared coal pitch with the high softening point by taking an organic solvent as an extractant and adopting an extraction technology so as to obtain the coal pitch with the isotropic structure and the high softening point. The softening point of the prepared high-softening-point coal pitch is 180-290 DEG C, the carbon residue rate is 60-78%, the content of toluene solubles is lower than 10%, the content of quinoline insolubles is lower than 5%, and the molecular structure is isotropic. The method promotes refinement of the coal chemical industry in China, and accelerates the development of carbon, electrolytic aluminum, automobiles and aerospace industries in China.

Description

Technical field: [0001] The invention relates to a preparation method of isotropic high softening point coal tar pitch, in particular to a high softening point coal tar pitch with high softening point, high residual carbon rate, low ash content, narrow molecular weight distribution and isotropic molecular structure method of preparation. Background technique: [0002] Medium-temperature coal tar pitch is obtained by distillation and separation of coal tar as a raw material. Its softening point is generally 70-120°C. It is mainly used as an impregnating agent for high-power graphite electrodes, a binder for electrolytic aluminum anodes, or graphite for lithium-ion batteries. The coating material of the negative electrode material. Since the domestic coal coking industry produces about 5 million tons of medium-temperature coal tar pitch every year, the market competition for medium-temperature coal tar pitch is very cruel. Therefore, the development of high-quality and high-s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C10C3/02C10C3/08
CPCC10C3/02C10C3/08
Inventor 詹亮王艳莉
Owner EAST CHINA UNIV OF SCI & TECH