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Preparation method of high-specific-surface-area ribbon-shaped graphite

A high specific surface area, band-shaped technology, applied in chemical instruments and methods, inorganic chemistry, non-metallic elements, etc., can solve problems such as the influence of electrode energy density and power density, reduce application effect, and damage to graphite crystallites. Inexpensive, high graphitic performance, effect of high and medium porosity

Inactive Publication Date: 2018-05-18
HENAN INST OF ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The porous expanded graphite prepared by the traditional high-temperature expansion method has a high specific surface area, but its porosity is very large, and the pore diameter is also large. The diameter of most pores is generally above the micron level, and the excessively large pores limit the performance of porous graphite. application, reducing the application effect; the use of activation drilling can obtain ultra-high specific surface area, but harsh activation will lead to the destruction of graphite crystallites; at the same time, the size of the pores is also an important factor affecting the application of graphite materials, such as in the field of energy storage When used as an electrode material, the micropores and mesopores in graphite act as energy storage sites and mass transfer channels, which will have a greater impact on the energy density and power density of the electrode.

Method used

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  • Preparation method of high-specific-surface-area ribbon-shaped graphite
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  • Preparation method of high-specific-surface-area ribbon-shaped graphite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Prepare a kind of ribbon-shaped graphite with high specific surface area according to the following steps:

[0033] (1) Dissolve 2g of petroleum asphalt in 10 ml of tetrahydrofuran to obtain solution A; add 8 ml of tetraethyl orthosilicate, 1.5 ml of deionized water and 0.8 ml of HF into a stainless steel cup, and stir magnetically at room temperature to form a uniform and transparent Solution B; add solution A to solution B, stir, stir evenly, transfer to a polytetrafluoroethylene reaction tank, and stand at 50°C until petroleum pitch / silicone gel is formed;

[0034] (2) Dry the gel obtained in step (1) at 100 °C, and then pre-oxidize it in an air atmosphere at 250 °C for 12 hours to obtain a pitch / silica composite; put the pitch / silica composite into Carbonization furnace, under the protection of nitrogen atmosphere, the temperature was raised to 600°C at 2°C / min, and then to 900°C at 5°C / min, then kept at 900°C for more than 3 hours, and finally cooled down to room t...

Embodiment 2

[0039] Embodiment 2 prepares a kind of ribbon-shaped graphite with high specific surface area according to the following steps:

[0040] (1) Petroleum pitch / silicone gel was prepared according to step (1) in Example 1;

[0041] (2) Dry the gel obtained in step (1) at 100 °C, and then pre-oxidize it in an air atmosphere at 280 °C for 6 hours to obtain a pitch / silica composite; put the pitch / silica composite into In the carbonization furnace, under the protection of nitrogen atmosphere, the temperature was raised to 600°C at 4°C / min, and then to 900°C at 8°C / min, then kept at 900°C for 1 hour, and finally cooled down to room temperature naturally to obtain a black carbon / silicon dioxide composite thing;

[0042] (3) Add excess hydrofluoric acid to the carbon / silica composite obtained in step (2) and stir for 10 hours to fully wash away the silica template, then wash with distilled water until neutral, dry to obtain mesopores carbon material;

[0043] (4) Put the mesoporous ca...

Embodiment 3

[0046] Prepare a kind of ribbon-shaped graphite with high specific surface area according to the following steps:

[0047] (1) Petroleum pitch / silicone gel was prepared according to step (1) in Example 1;

[0048] (2) Dry the gel obtained in step (1) at 100 °C, and then pre-oxidize it in an air atmosphere at 300 °C for 8 hours to obtain a pitch / silica composite; put the pitch / silica composite into In the carbonization furnace, under the protection of nitrogen atmosphere, the temperature was raised to 600°C at 6°C / min, and then to 800°C at 8°C / min, then kept at 800°C for 3 hours, and finally cooled down to room temperature naturally to obtain a black carbon / silicon dioxide composite thing;

[0049] (3) Add excess hydrofluoric acid to the carbon / silica composite obtained in step (2) and stir for 18 hours to fully wash away the silica template, then wash with distilled water until neutral, dry to obtain mesoporous carbon material;

[0050] (4) Put the mesoporous carbon materia...

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Abstract

The invention discloses a preparation method of high-specific-surface-area ribbon-shaped graphite. The preparation method comprises: making asphalt into a tetrahydrofuran solution, which is recorded as a solution A; adding tetraethoxysilane, deionized water and HF, respectively, to a stainless steel cup, and performing magnetic stirring at the room temperature to obtain a solution B; adding the solution A to the solution B, performing stirring, converting the obtained solution to a polytetrafluoroethylene reaction pot, and performing standing at 40-60 DEG C to form gel; drying the gel, pre-oxidizing the dried gel in an air atmosphere for no less than 3 h, raising the temperature of a carbonization furnace to 600 DEG C in a N2 atmosphere, then raising the temperature to 600-1000 DEG C, maintaining constant temperature for no less than 10 min to obtain a composite product; and washing the composite product in hydrofluoric acid, washing the obtained product with distilled water till the product is neutral, drying the obtained product, putting the obtained product in a graphitization furnace, raising the temperature to no less than 2000 DEG C in argon, and maintaining constant temperature for 10 min-1 h to obtain the high-specific-surface-area ribbon-shaped graphite. The high-specific-surface-area ribbon-shaped graphite is cheap in raw materials, low in preparation cost, and high in specific surface area.

Description

technical field [0001] The invention relates to the technical field of graphite preparation, in particular to a method for preparing ribbon-shaped graphite with a high specific surface area. Background technique [0002] Porous carbon materials are widely used as electrode materials for lithium-ion batteries, fuel cells and supercapacitors, and as adsorbents in separation processes and gas storage processes due to their high specific surface area, porosity, stability, and electrical conductivity. As well as the catalyst carrier in the important catalytic process, porous graphite is obtained after high-temperature graphitization of porous carbon materials. After high-temperature graphitization, porous graphite has excellent properties such as better stability and high electrical conductivity. However, after high-temperature treatment, the graphite microcrystals are arranged in an orderly manner to form graphite sheets, resulting in the disappearance of some pores and a decrea...

Claims

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Application Information

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IPC IPC(8): C01B32/205B82Y40/00
CPCB82Y40/00C01P2004/04C01P2006/12C01P2006/14C01P2006/17
Inventor 李思雨王利娜张晓峰张董王延伟许志忠
Owner HENAN INST OF ENG
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