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Intermediate phase asphalt and preparation method thereof

A mesophase pitch and extraction technology, which is applied in the direction of processing tar pitch/petroleum pitch/natural pitch by chemical method, and processing tar pitch/petroleum pitch/natural pitch by selective extraction, etc., can solve the problem of insufficient and effective asphalt substances The utilization of resources, waste of resources and other problems, to achieve the effect of improving resource utilization, convenient and safe operation, and simple process flow

Inactive Publication Date: 2013-07-10
CHNA ENERGY INVESTMENT CORP LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The invention provides a mesophase pitch and its preparation method to solve the problem that the pitch substances in the coal liquefaction residue cannot be fully and effectively utilized, resulting in waste of resources

Method used

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  • Intermediate phase asphalt and preparation method thereof

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preparation example Construction

[0020] In a typical implementation of the present invention, the preparation method of mesophase pitch includes the following steps: A. mixing and stirring the coal liquefaction residue with an extraction solvent, extracting, and centrifuging to obtain an extract; B. subjecting the extract to normal pressure or Distillation under reduced pressure to obtain refined extracts; C. Polymerize the refined extracts at 400-450° C. under an inert gas atmosphere and 0.1-3.0 MPa at constant pressure and temperature to obtain mesophase pitch. Through extraction, centrifugation and distillation to recover the extraction solvent, the content of quinoline insolubles in the obtained refined extract is effectively reduced, and the refined extract is mainly composed of polycyclic condensed aromatic hydrocarbons, with high aromaticity and high carbon content , easy to polymerize or cross-link, so it can be used as a high-quality raw material for the preparation of mesophase pitch; furthermore, un...

Embodiment 1

[0030] Add 800g of coal liquefaction residue and 3000g of coal liquefaction oil from the <110°C fraction obtained from the direct coal liquefaction process into a 5L stirring tank, and stir and mix thoroughly for 60 minutes; then perform centrifugation at a speed of 4000r / min; the extract is poured out, and the solvent is recovered by atmospheric distillation to obtain the refined extract. According to GB / T2293-2008 "Test Method for Quinoline Insolubles in Coking Pitch Products", the concentration of quinoline insolubles in the refined extract is measured. The content is 0.01%. The softening state is measured at room temperature by an automatic asphalt softening point tester.

[0031] Take 100 grams of the extracted and refined product obtained under the above conditions and pour it into an autoclave. After sealing it, purge it with nitrogen to make the pressure of nitrogen reach 0.1MPa, and gradually raise the temperature to 430°C at a heating rate of 4°C / min. The constant p...

Embodiment 2

[0034] Add 400g of coal liquefaction residue and 2000g of coal liquefaction oil obtained from the 110°C to 160°C fraction obtained from the direct coal liquefaction process into a 5L stirring tank, stir and mix thoroughly for 30 minutes; then perform centrifugation, and the speed of the centrifuge is 6000r / min; Pour out the extract, and carry out solvent recovery by atmospheric distillation to obtain the refined extract, which is insoluble in quinoline in the refined extract determined according to GB / T2293-2008 "Test Method for Quinoline Insolubles in Coking Pitch Products" The content of asphalt is 0.35%, and the softening point is 80°C measured by an automatic asphalt softening point tester.

[0035] Crush the refined extract obtained under the above conditions to a particle size ≤ 5mm, take 100 grams and pour it into an autoclave, seal it and purge it with nitrogen to make the pressure of nitrogen reach 1.0MPa, quickly heat up to 80°C, and then set the temperature at 2°C T...

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Abstract

The invention provides intermediate phase asphalt and a preparation method thereof. The preparation method comprises the following steps that A, mixing coal liquefaction residuals with an extraction solvent, stirring, extracting, and carrying out centrifugal separation to form an extraction liquid; B, carrying out atmospheric or reduced pressure distillation on the extraction liquid to form an extraction refined substance; and C, carrying out a polymerization reaction on the extraction refined substance at constant 400-450 DEG C and at constant 0.1-3.0MPa in an inert gas atmosphere for 5-16 hours to form the intermediate phase asphalt. According to the preparation method, under the condition that no catalyst is added, the intermediate phase asphalt in a good streamline structure is prepared, and serves as a carbon precursor for further preparing various carbon materials; the flow of a whole technical process is relatively simple; operation is convenient and safe; utilization potential of asphalt substances in the coal liquefaction residuals is fully exerted; the application field of the coal liquefaction residuals is expanded; and the resource utilization ratio is increased.

Description

technical field [0001] The invention relates to the field of deep coal processing, in particular to a mesophase pitch and a preparation method thereof. Background technique [0002] As a clean energy technology, coal liquefaction has developed a variety of direct coal liquefaction processes. However, no matter what kind of coal direct liquefaction process is adopted, the conversion rate of coal cannot reach 100%. In the end, there will always be a small amount of unreacted coal, inorganic minerals entrained in coal, and solid substances such as catalysts added to coal slurry. Coal liquefaction plant, usually these solid substances, liquefied heavy oil and bituminous substances are discharged in the solid-liquid separation unit, and this part of the discharge is called coal liquefaction residue. Coal liquefaction residue is a high-carbon, high-ash and high-sulfur substance. It looks like solid pitch at room temperature, with a softening point of about 180°C and a solid conte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10C3/02C10C3/08
Inventor 常鸿雁李克健章序文韩坤李永伦程时富
Owner CHNA ENERGY INVESTMENT CORP LTD
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