In-situ nitrogen doped graphalkyne material and synthesizing and application methods thereof

A synthesis method, nitrogen doping technology, applied in the direction of hybrid capacitor electrodes, nano-carbon, etc., can solve the limitations of in-depth research and application of nitrogen-doped graphyne materials, nitrogen doping amount, position and type can not be adjusted and affected Intrinsic properties of graphyne and other issues, to achieve the effect of good chemical and thermal stability, strong controllability and adjustability, and good purity

Active Publication Date: 2018-08-17
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The stability of the former material is poor, while the latter cannot control the amount, position and type of nitrogen doping, and will lead to the destruction of the alk

Method used

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  • In-situ nitrogen doped graphalkyne material and synthesizing and application methods thereof
  • In-situ nitrogen doped graphalkyne material and synthesizing and application methods thereof
  • In-situ nitrogen doped graphalkyne material and synthesizing and application methods thereof

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Experimental program
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Effect test

Embodiment 1

[0068] The synthesis of embodiment 1 aza-gamma-graphyne (N-gamma-GY):

[0069] Under argon protection, 2,4,6-triethynyl-1,3,5-triazine (76.5mg, 0.5mmol), Pd(PPh 3 ) 4 (Tetrakis(triphenylphosphine)palladium 28.85mg, 0.025mmol), 2,4,6-trichloro-1,3,5-triazine (92mg, 0.5mmol) and CuCl (5mg, 0.05mmol) were added to 500mL In a three-necked flask, 30 mL of N,N-dimethylformamide was added to the mixture. The reaction was stirred at 120° C. for 3 days and then cooled to room temperature. The insoluble solid was obtained by suction filtration, and then fully washed with water, ethanol, methyl alcohol, acetone and chloroform (to remove unreacted monomers, oligomers, catalysts and by-products) ), and then extracted with tetrahydrofuran, methanol, and chloroform for 24 hours, and finally vacuum-dried at 100° C. for 12 hours to obtain a black solid powder (101 mg, yield 88%). The specific surface area of ​​the obtained aza-γ-graphyne is 837m 2 / g, the pore volume is 1.45cm 3 / g, it ha...

Embodiment 2

[0070] The synthesis of embodiment 2 aza 6,6,12 graphyne (N-6,6,12-GY):

[0071] Under argon protection, 2,4,6-triethynyl-1,3,5-triazine (76.5mg, 0.5mmol), Pd(PPh 3 ) 4 (28.85mg, 0.025mmol) and CuCl (5mg, 0.05mmol), then 30mL of N,N-dimethylformamide was added, and tetrachloroethylene (0.038ml, 0.375mmol) was added dropwise. The reaction was stirred at 120°C for three days and then cooled to room temperature. After the insoluble solid was obtained by suction filtration, it was fully washed with water, ethanol, methanol, acetone and chloroform, then extracted with tetrahydrofuran, methanol, and chloroform for 24 hours, and finally vacuum-dried at 100°C for 12 hours to obtain a black solid powder (101mg, 118 %). The specific surface area of ​​the obtained aza 6,6,12 graphyne is 727m 2 / g, the pore volume is 1.23cm 3 / g, it has a micropore diameter of 1.3nm, a mesopore diameter of 2-9nm, and excellent comprehensive properties.

Embodiment 3

[0072] Synthesis of embodiment 3 azagraphdiyne (N-GDY):

[0073] Under argon protection, 2,4,6-triethynyl-1,3,5-triazine (76.5mg, 0.5mmol) and CuCl (50mg, 0.5mmol) were added to a 500ml three-necked flask, and then Add 45 mL of N,N-dimethylformamide. The reaction was stirred at 120°C for 3 days, then cooled to room temperature, and the insoluble solid was obtained by suction filtration, washed thoroughly with dilute hydrochloric acid, ethanol, methanol, acetone and chloroform, then extracted with tetrahydrofuran, methanol, and chloroform for 24 hours, and finally 100°C Drying in vacuo for 12 hours gave a black solid powder (77 mg, 103%). The specific surface area of ​​the obtained azagraphdiyne is 683m 2 / g, the pore volume is 1.89cm 3 / g, it has a micropore diameter of 1.8nm, a mesopore diameter of 3-8nm, and excellent comprehensive properties.

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Abstract

The invention belongs to the field of organic synthesis and relates to an in-situ nitrogen doped graphalkyne or graphdiyne material and synthesizing and application thereof to the field of energy storage. The synthesizing method of the in-situ nitrogen doped graphalkyne material comprises that, under the action of catalysts and solvent, a reaction monomer and tetrahaloethylene or cyanuric halogenperform Sonogashira coupling reaction at 60-150 DEG C under protection of inert gas to produce various types of nitrogen doped graphalkyne materials, wherein the reaction monomer is 2, 4, 6-triethinyl-1, 3, 5-triazine with a structural formula shown as the formula I. The synthesizing method of the in-situ nitrogen doped graphalkyne material has the advantages of being high in stability and simplein preparation, and meanwhile, is high in controllability and adjustability of reaction conditions; the applied catalysts are all commercialized catalysts and accordingly are wide in source and low incost; post-processing of polymerization is simple in process and beneficial to separation. The preparation process of the in-situ nitrogen doped graphalkyne material is applicable to medium and large-scale preparation and favorable to industrial production.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to the synthesis of graphyne materials such as in-situ nitrogen-doped graphyne and graphdiyne and its application in the field of energy storage. Background technique [0002] Nanoporous carbon materials are widely used in energy storage and conversion fields due to their high electrical conductivity, specific surface area, and low density, such as supercapacitors, lithium-ion batteries, and fuel cells. However, due to the low intrinsic activity of pure carbon materials, their specific capacity, energy density and power density are not ideal as electrode materials. Therefore, people have tried many methods to modify traditional pure carbon materials, among which nitrogen doping is a relatively efficient and simple method to improve the performance of carbon materials. Nitrogen doping can increase the charge density of the entire carbon skeleton, increase electron transp...

Claims

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Application Information

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IPC IPC(8): C01B32/15H01G11/24H01G11/30
CPCC01B32/15H01G11/24H01G11/30Y02E60/13
Inventor 任世杰徐雍捷岳勇邓纯王千
Owner SICHUAN UNIV
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