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Method for preparing Si/C composite material by employing oil shale residue as raw material

A technology of oil shale waste residue and composite materials, which is applied in the direction of electrical components, electrochemical generators, battery electrodes, etc., can solve the problems of high cost, difficult control of Si/C composite material preparation process, unfavorable industrial production, etc., and achieve cost reduction Low cost, avoid product agglomeration and sintering, and long diffusion distance

Active Publication Date: 2018-08-24
WUHAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In view of the above defects or improvement needs of the prior art, the present invention provides a method for preparing Si / C composite materials using oil shale residue as a raw material, the purpose of which is to use oil shale residue as a raw material to , mixed with molten salt and magnesium powder to undergo magnesia thermal reaction, and get Si / C composite material after pickling, which can be used as lithium-ion battery negative electrode material, thus solving the difficulty in controlling the preparation process of Si / C composite materials in the prior art , high cost, unfavorable technical problems such as industrial production

Method used

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  • Method for preparing Si/C composite material by employing oil shale residue as raw material
  • Method for preparing Si/C composite material by employing oil shale residue as raw material
  • Method for preparing Si/C composite material by employing oil shale residue as raw material

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Effect test

Embodiment 1

[0054] (1) 100g of oil shale minerals are first simply washed repeatedly with deionized water and then dried; the washed oil shale is crushed and ground into powder, and further processed to micron by mechanical ball milling. The specific size range is 10-20μm.

[0055] (2) Put 10 g of ball-milled oil shale into a tube furnace and heat it to 550°C for 2 hours at a rate of 5°C / min under a protective atmosphere of argon to activate the oil shale residue. Take out after cooling to room temperature;

[0056] (3) Put the activated oil shale powder into a 1L round-bottomed flask with a condensation reflux device, add sulfuric acid with a mass fraction of 33%, cook with stirring and heating to 90°C for 3 hours, and wait for the flask to Cool to 70°C, pour out the liquid and filter it with suction, wash it neutral and put it in a vacuum dryer to dry.

[0057] (4) Put 5g of the dried sample into a tube furnace, heat it to 1200°C for 2 hours at a rate of 5°C / min under a protective atm...

Embodiment 2

[0062](1) 100g of oil shale minerals are first simply washed repeatedly with deionized water and then dried; the washed oil shale is crushed and ground into powder, and further processed to micron by mechanical ball milling. The specific size range is 10-20μm.

[0063] (2) Put 10g of ball-milled oil shale into a tube furnace and heat it to 600°C at a heating rate of 5°C / min under an argon protective atmosphere to keep it warm for 3 hours to activate the oil shale residue and wait for the product to cool with the furnace Take out after reaching room temperature;

[0064] (3) Put the activated oil shale powder into a 1L round bottom flask with a condensing reflux device, and add hydrochloric acid with a concentration of 3mol / L, boil it with stirring and heating to 90°C for 3 hours, and wait for the flask to Cool to 70°C, pour out the liquid and filter it with suction, wash it neutral and put it in a vacuum dryer to dry.

[0065] (4) Put 5g of the dried sample into a tube furna...

Embodiment 3

[0070] (1) 100g of oil shale minerals are first simply washed repeatedly with deionized water and then dried; the washed oil shale is crushed and ground into powder, and further processed to micron by mechanical ball milling. The specific size range is 10-20μm.

[0071] (2) Put 10 g of ball-milled oil shale into a tube furnace and heat it to 650°C for 4 hours at a rate of 5°C / min under a protective atmosphere of argon to activate the oil shale residue. Take out after cooling to room temperature;

[0072] (3) Put the activated oil shale powder into a 1L round-bottomed flask with a condensation reflux device, add sulfuric acid with a mass fraction of 33%, cook with stirring and heating to 90°C for 3 hours, and wait for the flask to Cool to 70°C, pour out the liquid and filter it with suction, wash it neutral and put it in a vacuum dryer to dry.

[0073] (4) Put 5g of the dried sample into a tube furnace, heat it to 1000°C for 2 hours at a rate of 5°C / min under an argon protect...

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Abstract

The invention belongs to the technical field of inorganic material preparation and particularly relates to a method for preparing a Si / C composite material by employing an oil shale residue as a raw material. The method comprises the following steps of (1) carrying out pretreatment on the micron-sized oil shale residue, wherein the pretreatment comprises impurity-removal treatment and carbonization treatment, and obtaining pretreated oil shale residue; (2) mixing the pretreated oil shale residue with magnesium powder and molten salt evenly, putting the mixture into a closed vacuum environmentand carrying out heating for magnesium heat reduction reaction to obtain a mixed reaction product; and (3) pickling the mixed reaction product obtained in the step (2) to obtain the Si / C composite material. The preparation method is simple and feasible, the purity of the product is high and large-scale production can be implemented.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic materials, and more specifically relates to a method for preparing Si / C composite materials by using oil shale waste residue as a raw material. Background technique [0002] Silicon is the second most abundant element (approximately 26.4%) in the earth's crust. As a common semiconductor material, it has become an indispensable and important technical basis for modern high-tech society. Elemental silicon has extensive and important applications in energy, semiconductor, organic silicon, and metallurgical industries. At present, the anode materials of mature commercial lithium-ion batteries are mainly graphite carbon materials, but the theoretical lithium storage capacity of carbon materials is only 372mAh / g, which cannot meet people's demand for high energy density materials. Very high theoretical capacity (about 4200mAh / g), ten times the capacity of commercial graphene, has great...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/38H01M4/62H01M10/0525
CPCH01M4/362H01M4/386H01M4/62H01M4/625H01M10/0525Y02E60/10
Inventor 霍开富郭思广高标安威力付继江张旭明
Owner WUHAN UNIV OF SCI & TECH
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