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A kind of preparation method based on asphaltene highly active trace transition metal catalyst

A technology of transition metals and asphaltene, which is applied in the field of preparation of trace transition metal catalysts to achieve the effects of less metal loading, high catalytic efficiency, and environmentally friendly operation

Active Publication Date: 2021-04-20
CHINA UNIV OF MINING & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a preparation method based on asphaltenes highly active trace transition metal catalysts to solve the problem of using asphaltenes as catalysts in coal liquefaction residues and broaden the application of asphaltenes

Method used

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  • A kind of preparation method based on asphaltene highly active trace transition metal catalyst
  • A kind of preparation method based on asphaltene highly active trace transition metal catalyst
  • A kind of preparation method based on asphaltene highly active trace transition metal catalyst

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preparation example Construction

[0023] The preparation method of trace transition metal catalyst comprises the steps:

[0024] a. Using Soxhlet extraction method to extract asphaltenes, mixing the coal liquefaction residue with an asphaltene extraction solvent, and extracting the asphaltenes in the coal liquefaction residue at 50-90°C;

[0025] b. Place the clean corundum tube in a tube furnace, and raise the temperature of the high temperature part of the corundum tube to the reaction temperature under an atmosphere of argon, nitrogen or ammonia;

[0026] c. Put the corundum boat with asphaltene into the tube furnace, stop heating after 1-2h, and cool the reaction furnace to room temperature under the atmosphere of argon, nitrogen or ammonia;

[0027] d. Put another corundum boat with a transition metal sample into the tube furnace. Under the set conditions: 900-1500 ° C, normal pressure and argon, nitrogen or ammonia atmosphere or vacuum state, vacuum The degree of vacuum is 0-0.1; after heating for 1-6 h...

Embodiment 1

[0033] Embodiment 1: Put the corundum tube into a tube furnace, and under the protection of an argon inert gas with a flow rate of 0.05L / min, the temperature of the high temperature part of the corundum tube is raised to 900°C;

[0034] Put the corundum boat with asphaltene into the reaction furnace, stop heating after 1h, and cool the reaction furnace to room temperature under an ammonia atmosphere;

[0035] Put the corundum boat with the transition metal iron chromium into the tube furnace, heat it under the protection of argon under normal pressure for 1h, take out the sample in the corundum boat after cooling to room temperature, and the energy spectrum EDS analysis shows that the obtained asphaltenyl active transition The contents of the metal catalysts iron and chromium were 1.15 and 0.29 wt.%, respectively.

Embodiment 2

[0036] Embodiment 2: put the corundum tube into a tube furnace, and under the protection of nitrogen at a flow rate of 0.4L / min, the temperature of the high temperature part of the corundum tube is raised to 1300°C;

[0037] Put the corundum boat with asphaltene into the reaction furnace, stop heating after 1h, and cool the reaction furnace to room temperature under the protection of nitrogen gas;

[0038] Put the corundum boat with transition metal iron into the tube furnace, heat it under vacuum for 1 hour, take out the sample in the corundum boat after cooling to room temperature, and analyze the content of asphaltene-based active transition metal catalyst iron by energy spectrum EDS analysis. 0.80wt.%.

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Abstract

The invention discloses a preparation method of a trace transition metal catalyst with high activity based on asphaltene, which belongs to the preparation method of a trace transition metal catalyst. The method comprises the following steps: mixing the coal liquefaction residue with a selected solvent, extracting the asphaltenes in the coal liquefaction residue by Soxhlet extraction; placing a clean corundum tube in a tube furnace, and removing the high temperature part of the corundum tube The temperature is raised to the reaction temperature; put the corundum boat with asphaltene into the tube furnace, stop heating after a period of time, and cool the reaction furnace to room temperature under a protective atmosphere; put the corundum boat with transition metal chemicals Put it into a tube furnace, under the set conditions, heat it for a period of time and then cool it to room temperature, take out the sample in the corundum boat, and obtain the asphaltene highly active trace transition metal catalyst. Advantages: In the preparation, there is no conventional flammable and explosive gaseous and liquid metal reducing agents, which is environmentally friendly and easy to operate; the metal loading is small, and the catalyst preparation cost is low; there are many active crystal faces, and the catalytic activity is high.

Description

technical field [0001] The invention relates to a preparation method of a trace transition metal catalyst, in particular to a preparation method of a trace transition metal catalyst with high activity based on asphaltene. Background technique [0002] A catalyst is a substance that changes the reaction rate but does not change the total standard Gibbs free energy of the reaction, and its mass and chemical properties do not change before and after the reaction. In a general chemical reaction, the role of the catalyst is to reduce the activation energy required for the reaction to occur, essentially turning a relatively difficult reaction into an easy chemical reaction. Compared with noble metal catalysts such as platinum and ruthenium, in the field of catalysis, transition metal catalysts often receive great attention because of their lower cost, higher reserves and better catalytic activity. Among them, a small or trace amount of transition metal catalysts usually has more ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J21/18B01J32/00B01J37/08B01J23/755B01J23/745B01J23/86C10C3/08
CPCB01J21/18B01J23/745B01J23/755B01J23/862B01J37/084C10C3/08
Inventor 王全德刘滋武刘玲康国俊贾嘉韩菲轩锦锦黄晓寒王文鹏魏天宇马腾欢单毅
Owner CHINA UNIV OF MINING & TECH
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