Three-dimensional structure sulfur-nitrogen codope hierarchical pore graphene and preparation method thereof

A three-dimensional structure and co-doping technology, applied in the field of carbon nanomaterials, can solve the problems of high toxicity, high production cost, difficulty in effectively controlling the position and type of heteroatom doping, etc., and achieve the effect of simple process and low production cost

Active Publication Date: 2015-04-08
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most of the above two types of preparation methods are relatively complex in technology and equipment, and the production cost is high; in addition, small organic molecules containing heteroatoms have problems such as high toxicity and poor safety; more importantly, it is difficult to obtain the doping position and type of heteroatoms. Effective control

Method used

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  • Three-dimensional structure sulfur-nitrogen codope hierarchical pore graphene and preparation method thereof
  • Three-dimensional structure sulfur-nitrogen codope hierarchical pore graphene and preparation method thereof
  • Three-dimensional structure sulfur-nitrogen codope hierarchical pore graphene and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0023] (1) First, 6mmol Mg(NO 3 ) 2 ·6H 2 O, 2mmol Al(NO 3 ) 3 9H 2 O and 16mmol hexamethylenetetramine were mixed and dissolved in 20mL de-carbonated deionized water to prepare a mixed solution; then 20mmol m-sulfanilic acid and 20mmol NaOH were dissolved in 20mL de-carbonated deionized water for neutralization reaction, Sodium m-aminobenzenesulfonate solution was obtained. Under the protection of nitrogen, the above mixed solution and sodium m-aminobenzenesulfonate solution were mixed, stirred evenly, transferred to a 50mL polytetrafluoroethylene-lined autoclave, and placed in an oven at 100°C for 12 hours at a constant temperature. Take out the autoclave and let it cool down to room temperature naturally, filter and wash the filtrate with 800mL deionized water and 200mL ethanol until the pH value of the filtrate is 7, then dry the filter cake at 80°C for 8 hours to obtain the magnesium aluminum hydrotalcite.

[0024] (2) Put the magnesium-aluminum hydrotalcite interc...

Embodiment 2

[0028] (1) First, 10mmol CoSO 4 ·7H 2 O, 4mmol Al(NO 3 ) 3 9H 2 O and 28mmol hexamethylenetetramine were mixed and dissolved in 20mL of de-carbonated deionized water to prepare a mixed solution; then 30mmol of sulfanilic acid and 30mmol NaOH were dissolved in 20mL of de-carbonated de-ionized water for neutralization reaction, Sodium m-aminobenzenesulfonate solution was obtained. Under the protection of nitrogen, mix the above mixed solution and sodium m-aminobenzenesulfonate solution, stir evenly, transfer it to a 50mL polytetrafluoroethylene-lined autoclave, put it in an oven at 120°C for 10 hours, and take it out The autoclave was naturally cooled to room temperature, filtered and washed with 800mL deionized water and 200mL ethanol until the pH value of the filtrate was 7.5, and then the filter cake was air-dried at 70°C for 12 hours to obtain the magnesium aluminum intercalated with m-aminobenzenesulfonate Hydrotalcite.

[0029] (2) Put the above-mentioned sulfanilate...

Embodiment 3

[0032] (1) First, 5.6mmol MgCl 2 ·6H 2 O, 1.6 mmol AlCl 3 ·6H 2 O and 14.4mmol of hexamethylenetetramine were mixed and dissolved in 20mL of de-carbonated deionized water to prepare a mixed solution; then 20mmol of sulfanilic acid and 20mmol of NaOH were dissolved in 20mL of de-carbonated de-ionized water for neutralization , to obtain sodium p-aminobenzenesulfonate solution. Under the protection of nitrogen, mix the above mixed solution and sodium p-aminobenzenesulfonate solution, stir evenly, transfer to a 50mL polytetrafluoroethylene-lined high-pressure reactor, put it in an oven at 90°C for 20 hours, and take out The autoclave was naturally cooled to room temperature, filtered and washed with 800mL deionized water and 200mL ethanol until the pH value of the filtrate was 7, and then the filter cake was air-dried at 60°C for 12 hours to obtain magnesium aluminum intercalated with p-aminobenzenesulfonate Hydrotalcite.

[0033] (2) Put the p-aminobenzenesulfonate intercal...

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Abstract

The invention discloses three-dimensional structure sulfur-nitrogen codope hierarchical pore graphene and a preparation method thereof, and belongs to the technical field of the carbon nano-materials. The graphene is formed by the graphene nano-sheets with 100-300 nanometers of radial dimenstion and 3-8 nanometers of thickness, the graphene nano-sheets are cross-connected to form the three-dimensional structure with 2-50 nanometers of mesopores and more than 50 nanometers of macropores, and the graphene nano-sheets have less than 2 nanometers of micropores. The sulfur element content in the sulfur-nitrogen codope graphene nano-sheets is 1-4at.%, the nitrogen element content is 5-15at.%, and the content of the pyridine nitrogen and the pyrrolic nitrogen is greater than 90%. The sulfur and nitrogen are located in the edges of the graphene nano-sheets or the edges of the micropores in the graphene nano-sheets. The preparation method comprises the following steps: inserting the anions containing sulfur-nitrogen small organic molecules into the lamellar di-hydroxy composite metallic oxide laminations through the hydrothermal reaction so as to obtain the intercalation structure precursor, and obtaining the graphene by the high temperature calcination and acidification reaction. The method has the advantages of adjusting the doping content of the heteroatoms, and the doping type and position of the heteroatoms, and has the simple process and low production cost.

Description

technical field [0001] The invention belongs to the technical field of carbon nanomaterials, in particular to a three-dimensional sulfur-nitrogen co-doped hierarchical porous graphene and a preparation method thereof. Background technique [0002] Due to its unique physical and chemical properties, such as high thermal conductivity, fast electron mobility, excellent mechanical properties, large specific surface area and other advantages, graphene is widely used in fuel cells, lithium-ion batteries, supercapacitors and sensors. a broad application prospect. [0003] Porous graphene can increase the effective specific surface area of ​​graphene and increase the transfer rate of reactants, thereby improving the application performance of graphene. Constructing three-dimensional graphene is an effective way to obtain porous graphene, which usually has mesopores (2-50nm) and macropores (>50nm) stacked pores. Micropores (<2nm) can be formed on the graphene sheet by alkalin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 杨文胜王俊路艳罗陈旭
Owner BEIJING UNIV OF CHEM TECH
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