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Preparation method and application of alkynyl carbon material

A technology of carbon materials and monoacetylene, applied in the direction of nano-carbon, electrical components, battery electrodes, etc., can solve the problems of limited promotion and inability to realize industrialization, and achieve the effect of simplifying equipment and simplifying the process flow

Inactive Publication Date: 2018-08-07
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the existing synthesis of graphdiyne by Cu-catalyzed or high-temperature-catalyzed Glaser-Hay cross-coupling reaction requires the use of the precursor hexaethynylbenzene, which cannot be industrialized at present, which limits the promotion of craftsmanship

Method used

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  • Preparation method and application of alkynyl carbon material
  • Preparation method and application of alkynyl carbon material
  • Preparation method and application of alkynyl carbon material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] With the pellet mass ratio of 1:20, take by weighing hexachlorobenzene (C 6 Cl 6 ) and calcium carbide (CaC 2 ), put it in a ball mill jar, and add absolute ethanol until the grinding material is submerged. Seal the ball mill jar. Ball milled for 18 hours by a planetary ball mill at a rate of 400 rpm. The milled samples were taken out and washed with deionized water to remove unreacted calcium carbide. After drying, wash with hot benzene to remove unreacted hexahalobenzene, and obtain graphyne powder directly.

[0040] Measure 50 ml of methyl orange solution (10 mg / L), add 50 mg of sample, and after standing for 3 hours, irradiate with ultraviolet-visible light to carry out photocatalytic degradation reaction. Every 20 minutes, measure the absorbance change of the solution using UV-vis absorption spectroscopy.

[0041] The full spectrum of X-ray photoelectron spectroscopy of the sample ( figure 2 ) shows that the sample is only composed of carbon elements except...

Embodiment 2

[0043] With the pellet mass ratio of 1:50, take by weighing hexabromobenzene (C 6 Br 6 ) and calcium carbide (CaC 2 ), placed in a vacuum ball mill jar, and added absolute ethanol until the grinding material was submerged. Seal the ball milling jar, and feed nitrogen into the ball milling jar (N 2 ). Ball milled for 12 hours by a planetary ball mill at a rate of 500 rpm.

[0044] After washing and drying the ball-milled sample according to the method described in Example 1, mix the sample with polyethylene glycol, ethyl cellulose, and ethanol according to the mass ratio: 9:9:1:1, and mix the sample at 40~90°C Stir magnetically for 2-10 hours. The obtained slurry is spin-coated on conductive glass, and after drying, it is annealed in a muffle furnace at 260-300°C to remove surfactants such as polyethylene glycol and ethyl cellulose. Use wires, conductive glue, insulating glue, etc. to package the annealed electrode to obtain the working electrode of the sample.

[0045] ...

Embodiment 3

[0047]With the pellet mass ratio of 1:100, take by weighing hexaiodobenzene (C 6 I 6 ) and calcium carbide (CaC 2 ), placed in a vacuum ball mill jar, adding absolute ethanol to fill the ball mill jar. Seal the ball mill jar, and mill it through a planetary ball mill for 12 hours at a speed of 500 rpm, and wash and dry the milled sample according to the method described in Example 1.

[0048] Weigh the active material (graphyne powder), conductive agent (Super P fine powder) and binder (polyvinylidene fluoride) with a mass ratio of 8:1:1, add solvent (1-methyl-2-pyrrolidone ), stirred and mixed into a slurry under a dry atmosphere. Apply the slurry evenly on the copper foil, place it in a vacuum drying oven and dry it at 60°C for 24 hours, cut into discs with a diameter of 14 mm, weigh them and assemble them into CR2016 in a glove box filled with argon. button battery. Among them, metallic lithium was used as the counter electrode, 1 M LiPF 6 The EC / DMC (1:1 volume ratio...

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Abstract

The invention relates to a preparation method and application of an alkynyl carbon material. The carbon material is quasi graphdiyne powder. The preparation method includes: adding C6X6, CaC2 and ball-milling balls into a vacuum ball-milling tank, and adding absolute ethyl alcohol, wherein the mole ratio of C6X6 to CaC2 is (1:6)-(1:18); sealing the ball-milling tank, and vacuumizing the ball-milling tank or feeding inert gas into the ball-milling tank; using a planetary ball mill to perform ball milling for 6-18 hours at a rate of 400-600r / minute; washing, drying, washing and drying to obtainthe quasi graphdiyne powder. Compared with existing cross-coupling reaction, the preparation method which can simplify the technical process has the advantages that required equipment is simple, and the method is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of carbon materials, and in particular relates to a preparation method and application of an alkynyl carbon material. Background technique [0002] Graphyne material is another new type of carbon material known as a super material after graphene. Because of its unique electrical and electrochemical properties, it has broad application prospects in energy, electronics, catalysis and other fields. The ideal graphyne is composed of several alkyne bonds connecting benzene rings to form sp 2 hybridized carbon atoms and sp 3 A carbon material with a two-dimensional planar network structure composed of hybrid atoms. [0003] In 2010, the research group of academician Li Yuliang of the Chinese Academy of Sciences synthesized graphdiyne (Graphdiyne type) for the first time through the Glaser-Hay cross-coupling reaction, which then triggered an upsurge in graphdiyne research. On this basis, Liu Zhongfan, Sakamoto and other r...

Claims

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Application Information

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IPC IPC(8): C01B32/15H01M4/587
CPCC01B32/15H01M4/587Y02E60/10
Inventor 崔晓莉李乔丹
Owner FUDAN UNIV
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