Preparation method for biomass-based nitrogen-doped thin layer graphitized carbon material

A thin-layer graphite, nitrogen-doped technology, applied in chemical instruments and methods, inorganic chemistry, carbon compounds, etc., can solve the problems of uncontrollable surface structure, low degree of graphitization, and thick graphitic carbon-carbon layer, and achieve thin graphite. layer, the synthesis method is simple, and the effect of good graphitization degree

Inactive Publication Date: 2018-07-17
JIANGSU UNIV OF TECH
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Problems solved by technology

[0006] In order to solve the defects of low graphitization degree, thick graphitic carbon layer, low specific surface area and uncontrollable surface structure in the preparation of carbon materials using lignin as carbon source in the prior art, the present invention provides a biomass-based nitrogen-doped Preparation method of heterothin layer graphitized carbon material

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  • Preparation method for biomass-based nitrogen-doped thin layer graphitized carbon material
  • Preparation method for biomass-based nitrogen-doped thin layer graphitized carbon material
  • Preparation method for biomass-based nitrogen-doped thin layer graphitized carbon material

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Embodiment 1

[0022] (1) First put 1g of lignin into a round bottom bottle, add 10mL of 0.1mol / L acetic anhydride solution and 10ml of 0.1mol / L nitric acid, stir at room temperature for 5h, then add 1mol / L sodium hydroxide solution Adjust the pH to neutral, and finally extract with tetrahydrofuran to obtain nitrated lignin;

[0023] (2) Take 0.5g of nitrolignin obtained in step 1) and dissolve it in 50% ethanol solution, add a little iron powder, drop in 2ml of hydrochloric acid, heat up to 130°C, react for 6h, then add dropwise sodium hydroxide solution (1mol / L) adjusting the pH to alkaline, centrifuging, washing, and drying to obtain nitrogen-doped lignin;

[0024] (3) The nitrogen-doped lignin precursor obtained in step 2) was placed in a high-temperature furnace, and the temperature was raised to 1200 °C at a rate of 2 °C / min in an argon atmosphere, and the flow rate of the inert gas was 50 mL / min. After carbonizing at 1200° C. for 3 hours, cool naturally to room temperature to obtain...

Embodiment 2

[0027] (1) First put 1g of lignin into a round bottom bottle, add 10mL of 0.1mol / L acetic anhydride solution and 10ml of 0.1mol / L nitric acid, stir at room temperature for 5h, then add 1mol / L sodium hydroxide solution Adjust the pH to neutral, and finally extract it with tetrachloromethane to obtain nitrified lignin;

[0028] (2) Take 0.5g of nitrated lignin obtained in step 1) and dissolve it in 50% ethanol solution, add a little iron powder, drop in 2ml of hydrochloric acid, heat up to 130°C, react for 6h, and then add dropwise sodium hydroxide solution (1mol / L) adjusting the pH to alkaline, centrifuging, washing and drying to obtain nitrogen-doped lignin.

[0029] (3) The nitrogen-doped lignin precursor obtained in step 2) was placed in a high-temperature furnace, and the temperature was raised to 1200 °C at a rate of 2 °C / min in an argon atmosphere, and the flow rate of the inert gas was 50 mL / min. After carbonization at 1000° C. for 3 h, it was naturally cooled to room ...

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Abstract

The invention relates to a preparation method for a biomass-based nitrogen-doped thin layer graphitized carbon material. The method is characterized by comprising the following steps that 1) lignin isused as a carbon source, through a nitration reaction, nitryl is introduced into lignin functional groups, then nitryl is reduced into amidogen, and nitrogen-doped lignin is obtained; 2) nitrogen-doped lignin is carbonized in an inert atmosphere; 3) the nitrogen-doped thin layer graphitized carbon material is obtained through a chemical insertion layer method. The nitrogen-doped thin layer graphitized carbon material has a high graphitized degree and a thin graphite layer, the synthesis method is easy, renewable lignin is used as the carbon source, and the material is environmentally friendlyand sustainable.

Description

technical field [0001] The invention belongs to the technical field of biomass-based carbon materials, in particular to a preparation method of biomass-based nitrogen-doped thin-layer graphitized carbon materials. Background technique [0002] In recent years, carbon materials doped with heteroatoms (such as nitrogen, boron, phosphorus, sulfur, cobalt, etc.), especially carbon nanomaterials with a thin layer structure, have higher The advantages of electrical conductivity, as well as good physical and chemical stability, have a wide range of applications in the fields of catalysis, adsorbents, electrode materials and batteries. On the one hand, after heteroatoms are introduced into the carbon structure, due to the difference in bond length, valence electrons, and atomic size with carbon atoms, defects appear in sites near adjacent carbon atoms, the charge distribution is uneven, and the electrical neutrality of carbon materials is destroyed. It is more conducive to construc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/205
CPCC01P2002/01C01P2002/72C01P2002/80C01P2002/82
Inventor 秦恒飞赵晶艳李康尧吕申杰林號刘维桥
Owner JIANGSU UNIV OF TECH
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