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A kind of preparation method and product of ultra-high specific surface area sulfur-nitrogen co-doped porous graphene

A technology of ultra-high specific surface area, porous graphene, applied in graphene, chemical instruments and methods, nano-carbon, etc., can solve the problem that polymer precursors and organic gases are toxic and harmful, graphene specific surface area is not high, and the preparation process is complicated. and other problems, to achieve the effect of improving application value, benefiting large-scale production and wide-ranging sources

Active Publication Date: 2017-08-11
南京同宁新材料研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the specific surface area of ​​graphene prepared by these two methods is generally not high 2 / g, and the preparation process is relatively complicated, graphene oxide needs to be prepared first and then mixed, or a complex organic gas environment is required, which is not conducive to its promotion, and polymer precursors and organic gases are toxic and harmful, seriously threatening human health
In addition, CN201510201085.4 discloses an animal bone-based graphene-like lithium-ion battery negative electrode material and its preparation method, which uses animal bone as a raw material, and obtains graphene through carbonization, activation and graphitization, combined with heat treatment at a certain temperature , this method requires high-temperature activation, and after activation, high-temperature conversion into graphene is required. The preparation process is complicated and the cost is high. The graphene obtained is ordinary non-doped graphene with a layered structure.

Method used

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  • A kind of preparation method and product of ultra-high specific surface area sulfur-nitrogen co-doped porous graphene
  • A kind of preparation method and product of ultra-high specific surface area sulfur-nitrogen co-doped porous graphene
  • A kind of preparation method and product of ultra-high specific surface area sulfur-nitrogen co-doped porous graphene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] 1) Wash the pig hair and dry it. As for the argon atmosphere of the tube furnace, heat up to 300°C for initial carbonization. The holding time is 2 hours, and the heating rate is 1°C·min -1 ;

[0047] 2) Place the sample prepared in step 1) in a vacuum glove box at 0.5mol L -1 In KOH, adsorb under reduced pressure for 2 hours, set the air pressure to 10pa, and dry in an ordinary drying oven at 80°C for 12 hours;

[0048] 3) Put the sample in step 2) in the tube furnace, keep the argon atmosphere, raise the temperature to 350°C, keep it for 0.5h, then raise the temperature to 800°C, keep it for 1h, the heating rate is 5°C·min -1 , and then naturally cooled;

[0049] 4) Grinding the product obtained in step 3) and impregnating it in 0.5mol·L -1 H 2 SO 4 After pickling at constant temperature at 80°C for 8 hours in the solution, filter with suction and wash with water until neutral;

[0050] 5) The sample obtained in step 4) was placed in a vacuum drying oven (at a p...

Embodiment 2

[0053] 1) Wash the chicken feathers and dry them. As for the argon atmosphere in the tube furnace, heat up to 250°C for initial carbonization. The holding time is 3 hours, and the heating rate is 2°C·min. -1 ;

[0054] 2) Place the prepared sample in step 1) in the glove box 0.7mol L -1 In NaOH, absorb under reduced pressure for 1h, set the air pressure to 5pa, and dry in an ordinary drying oven at 90°C for 11h;

[0055] 3) Put the sample in step 2) in the tube furnace, keep the argon atmosphere, raise the temperature to 200°C, keep it for 1h, then raise the temperature to 700°C, keep it for 1h, the heating rate is 3°C·min -1 , and then naturally cooled;

[0056] 4) Grind the product obtained in step 3) and impregnate it in 0.3mol·L -1 After pickling at a constant temperature of 90°C for 5 hours in HCl solution, filter with suction, and wash with water until neutral;

[0057] 5) The sample obtained in step 4) was placed in a vacuum drying oven (at a pressure of 40 Pa, at a...

Embodiment 3

[0060] 1) Wash the duck feathers and dry them. As for the argon atmosphere of the tube furnace, heat up to 200°C for initial carbonization. The holding time is 4 hours, and the heating rate is 1.5°C·min. -1 ;

[0061] 2) Place the prepared sample in step 1) in the glove box 0.8mol L -1 In KOH, absorb under reduced pressure for 3 hours, set the air pressure to 20pa, and dry in an ordinary drying oven at 100°C for 10 hours;

[0062] 3) Put the sample in step 2) in the tube furnace, keep the argon atmosphere, raise the temperature to 300°C, keep it for 1h, then raise the temperature to 600°C, keep it for 0.5h, the heating rate is 4°C·min -1 , and then naturally cooled;

[0063] 4) Grinding the product obtained in step 3) and impregnating it in 0.6mol·L -1 After pickling in a hydrochloric acid solution at a constant temperature of 90°C for 10 hours, filter with suction, and wash with water until neutral;

[0064] 5) The sample obtained in step 4) was placed in a vacuum drying ...

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Abstract

The invention discloses a preparation method and product of ultrahigh-specific-area sulphur-nitrogen-co-doped porous graphene.The method includes the steps of selecting a keratin-containing biomass material as the raw material, using the biomass material as the solid carbon, nitrogen and sulphur raw material at the same time, conducting preliminary carbonization, conducting pressure reduction adsorption through an alkaline solution, conducting high-temperature activating, conducting acid pickling and vacuum drying to obtain graphene, and directly converting biomass keratin into the ultrahigh-specific-area sulphur-nitrogen-co-doped porous graphene.The nitrogen content of the graphene can reach up to 5.0 at.% or above, the sulphur content reaches 1.0 at.% or above, the specific area reaches up to 1500 m<2> / g or above, and the graphene is of a porous foam-shaped structure.The used raw material is wide in source and low in price, the application of the raw material is improved after the raw material is prepared into the graphene, the environment pollution caused by abandoned waste is effectively solved, and the method has the advantages of being simple and efficient in preparation, low in cost, and the like.

Description

technical field [0001] The invention belongs to the field of graphene material preparation, and more specifically relates to a preparation method and product of sulfur and nitrogen co-doped porous graphene with ultra-high specific surface area. Background technique [0002] Among many carbon materials, graphene has become a research hotspot due to its special structure and properties. Graphene is a two-dimensional periodic structure composed of carbon six-membered rings. This special structure makes it have many peculiar properties, such as room temperature quantum Hall effect, ferromagnetism, superconductivity and giant magnetoresistance effect. In addition, graphene also has excellent thermal properties, electrical properties, mechanical properties, high chemical stability and thermodynamic stability, making it suitable for nano-devices, batteries / supercapacitors, composite materials, hydrogen storage materials, catalysts and other fields. potential application prospects....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/184
CPCC01B2204/32C01P2002/82C01P2002/85C01P2004/04
Inventor 黄云辉张建胡培
Owner 南京同宁新材料研究院有限公司