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Hollow carbon microspheres and preparation method thereof

A technology of carbon microspheres and hollow, applied in the field of hollow carbon microspheres and its preparation, can solve problems such as great influence on quality, narrow downstream application paths and scope, and non-compliance, and achieve simple and easy-to-operate preparation methods and easy-to-use process parameters The effect of controlling and reducing production difficulty

Active Publication Date: 2020-01-17
CHINA UNIV OF PETROLEUM (BEIJING) +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, limited by the reaction method, there are few reports on the application of heavy oil in the field of high value-added carbon materials
The main reason is that the reaction of heavy oil is complex and difficult to control. Although there are many related reports on deep processing applications, there are generally defects in downstream product standards that are unstable or poor in quality and low in yield.
Although a small number of manufacturers have realized the preparation of needle coke and mesophase products (pitch or carbon microspheres) from heavy oil as raw materials, this should be the main way to prepare carbonized products from heavy oil through thermal condensation and coking reactions. , but the characteristics of heavy oil and the results of previous separation and treatment have a great impact on the quality of carbonized products such as needle coke. With the current industrial production process, each batch of needle coke products will have 30% or more inferior coke that does not meet the standard , in order to produce high-quality carbonized products with high output, it requires high production process control and equipment investment
On the other hand, even if the production of high-quality carbonized products can be achieved, compared with heavy oil raw materials with huge output, its downstream application path and scope are still relatively narrow

Method used

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  • Hollow carbon microspheres and preparation method thereof
  • Hollow carbon microspheres and preparation method thereof
  • Hollow carbon microspheres and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] The preparation method of the hollow carbon microspheres of the present embodiment is as follows:

[0070] 1) Add coal tar into the tank reactor, then add 5°C mixed xylene (petroleum mixed xylene (GB / T 3407-2010)) into the tank reactor, stir evenly and lock the tank reactor ;

[0071] Use nitrogen to purge the tank reactor, then increase the pressure to 5MPa, and use a heating furnace to heat at a heating rate of about 1.5°C / min. After the temperature rises to 390°C, keep the temperature and pressure for about 5 hours;

[0072] Wherein, the agent oil mass ratio of mixed xylene and coal tar is about 3:1;

[0073] 2) After the temperature and pressure of the tank reactor are lowered to room temperature and normal pressure, the mixed solution in the tank reactor is taken out and filtered, and the filter cake is collected as a crude product;

[0074] 3) Put the filter cake in step 2) into a flask equipped with a condenser tube and a stirrer, then add mixed xylenes into th...

Embodiment 2

[0083]The preparation method of the hollow carbon microspheres of the present embodiment is as follows:

[0084] 1) Add coal tar into the tank reactor, then add toluene into the tank reactor, stir evenly and lock the tank reactor;

[0085] Use nitrogen to purge the tank reactor, then increase the pressure to 6MPa, and use a heating furnace to heat at a heating rate of about 1.5°C / min. After the temperature rises to 350°C, keep the temperature and pressure for about 5 hours;

[0086] Wherein, the agent oil mass ratio of toluene and coal tar is 4:1;

[0087] 2) After the temperature and pressure of the tank reactor are lowered to room temperature and normal pressure, the mixed solution in the tank reactor is taken out and filtered, and the filter cake is collected as a crude product;

[0088] 3) put the filter cake in step 2) into a flask equipped with a condenser tube and a stirrer, then add toluene in the flask, heat the flask until the solvent refluxes, and stop heating afte...

Embodiment 3

[0096] The preparation method of the hollow carbon microspheres of the present embodiment is as follows:

[0097] 1) Add coal tar into the tank reactor, then add toluene into the tank reactor, stir evenly and lock the tank reactor;

[0098] Use nitrogen to purge the tank reactor, then increase the pressure to 5MPa, and use a heating furnace to heat at a heating rate of about 1.5°C / min. After the temperature rises to 400°C, keep the temperature and pressure for about 3 hours;

[0099] Wherein, the agent oil mass ratio of toluene and coal tar is 3:1;

[0100] 2) After the temperature and pressure of the tank reactor are lowered to room temperature and normal pressure, the mixed solution in the tank reactor is taken out and filtered, and the filter cake is collected as a crude product;

[0101] 3) Put the filter cake in step 2) into a flask equipped with a condenser tube and a stirrer, then add toluene to the flask, heat the flask until the solvent refluxes, and stop heating aft...

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Abstract

The invention provides hollow carbon microspheres and a preparation method thereof. The preparation method comprises the steps that a reaction system containing heavy oil, serving as a raw material, and an organic solvent is subjected to a thermal polycondensation reaction after reaching a supercritical or near-critical state of the organic solvent; after the thermal polycondensation reaction is completed, the organic solvent is separated, a coarse product is collected, and a separating solvent is added for purifying treatment; and drying treatment is performed on the coarse product subjectedto the purifying treatment to obtain the hollow carbon microspheres. According to the preparation method, the heavy oil is used as the raw material, no template or catalyst needs to added, and the hollow carbon microspheres are prepared in one step; an meanwhile, hollow carbon microspheres with different dimensions can be prepared by changing the raw material and adjusting parameters of the preparation technology, and large-scale application is easy to realize.

Description

technical field [0001] The invention relates to a hollow carbon microsphere and a preparation method thereof, belonging to the fields of high value-added processing of heavy oil and carbon materials. Background technique [0002] Hollow carbon microsphere is a kind of spherical carbon material with great potential. It has the characteristics of low toxicity, large specific surface area, low density, thermodynamic and chemical stability, etc. Whether it is used as a high-performance catalyst carrier or in biology, adsorption, energy storage, It has good application prospects in the fields of optoelectronics, heat insulation, sound insulation and electrode materials. [0003] As a carbonization product, although there are a wide range of raw materials for the preparation of hollow carbon microspheres, most of them are pure substances, such as glucose, phenol, benzene, ethylene, formaldehyde or polymers, etc. as carbon sources. The preparation method is mainly based on the tem...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/05
CPCC01B32/05Y02P20/54
Inventor 赵锁奇张德凯许志明张霖宙冯叶于颖孙学文徐春明
Owner CHINA UNIV OF PETROLEUM (BEIJING)