Preparation method of graphdiyne

A technology of graphdiyne and reaction substrate, which is applied in the field of preparation of graphdiyne, can solve the problems of controllable preparation but not substantively solved, and achieves easy transfer and spreading, simple process, and controllability of reaction temperature and time. strong effect

Active Publication Date: 2015-11-04
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its essence is to subject the synthesized graphyne to high temperature treatment so that it can be rearranged in a certain range to improve its semiconductor performance. There is no substantial solution to the controllable preparation of graphyne and the problems that arise during the preparation process.

Method used

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  • Preparation method of graphdiyne
  • Preparation method of graphdiyne

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] In an argon (purity ≥ 99.999%) gas environment, the substrate (1,3,5-tripynylbenzene) 192mg (1.0mmol) and the catalyst (tris(tert-butoxy)(2,2-di Methpropynyl) tungsten) 47.0mg (0.1mmol) into a Schlenk bottle, 15mL of toluene (anhydrous and anaerobic treatment) dissolved. Heated in an oil bath, slowly raised to 75°C, and reacted for 24 hours; during the process, the solution was vacuumed (6 times, 25s each time) to remove the by-product 2-butyne, and the solvent lost in the vacuum was compensated by adding 3 mL of new solvent; the reaction After the end, a gel-like solid was produced. After repeated washing with toluene, the target product graphyne was obtained by suction filtration. The chemical equation of this reaction is as follows:

[0036]

[0037] figure 1 It is the solid carbon-13 NMR spectrum of the graphyne prepared in Example 1, and the test results show that the graphyne has kept the basic characteristic structure of the benzene ring and the alkyne bond;...

Embodiment 2

[0046] Argon (purity ≥ 99.999%) gas environment, 192mg (1.0mmol) substrate (1,3,5-tripynylbenzene) and 23.5mg (0.05mmol) catalyst (tri(tert-butoxy) ( 2,2-Dimethylpropynyl)tungsten) into a Schlenk bottle, and dissolved in 60mL of toluene (anhydrous and oxygen-free). Heated in an oil bath, slowly raised to 75°C, and reacted for 24 hours; during the process, the solution was vacuumed (5 times, 20s each time) to remove the by-product 2-butyne, and the solvent lost in the vacuum was compensated by adding 7.5mL of new solvent; After the reaction, a gel-like solid was produced. After repeated washing with toluene, the target product graphyne was obtained by suction filtration.

Embodiment 3

[0048] Under nitrogen (purity ≥ 99.999%) gaseous environment, 1.92g (10.0mmol) substrate (1,3,5-tripynylbenzene) and 0.705g (1.5mmol) catalyst (three (tert-butoxy) ( 2,2-Dimethylpropynyl)tungsten) into a Schlenk bottle, and dissolved in 15 mL of toluene (anhydrous and oxygen-free). Heat in an oil bath, slowly rise to 50°C, and react for 192h; during the process, the solution is vacuumed (8 times, 30s each time) to remove the by-product 2-butyne, and the solvent lost in vacuum is compensated by adding 4mL of new solvent; After the end, a gel-like solid was produced. After repeated washing with toluene, the target product graphyne was obtained by suction filtration.

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Abstract

The invention relates to a preparation method of graphdiyne. The preparation method comprises that 1, in a nitrogen or argon protective atmosphere, a reaction substrate 1,3,5-tripropargylbenzene and a catalyst are put into a reaction container, a solvent is added into the reaction container to dissolve the materials in the reaction container, and the solution undergoes a heating reaction, 2, in the reaction process in the step 1, the solution is subjected to vacuum pumping process multiple times so that a reaction side product 2-butyne is removed and a solvent is supplied to make up for a loss of the solvent, and 3, after the reaction, the reaction product is purified so that the product graphdiyne is obtained. Compared with the prior art, the preparation method has simple processes. The prepared graphdiyne has the uniform surface and a low oxidation degree and can stably exist in air.

Description

technical field [0001] The invention relates to the field of semiconductors, in particular to a preparation method of graphyne. Background technique [0002] With the development of the two major fields of catalysis science and material science, nano-carbon structure materials have attracted extensive scientific attention and achieved a series of breakthroughs, which have produced considerable impacts in the fields of energy research and development, sustainable development, and ecological environment. Positive effect. There are two main forms of allotropes of carbon in nature - diamond and graphite, and their structural characteristics are represented by sp 3 and sp 2 Hybridized carbon atoms extend to build the skeleton; and the discovery of fullerenes, carbon nanotubes, and graphene enriches sp 2 Types of hybrid carbon materials, and have been applied as zero-dimensional, one-dimensional and two-dimensional materials, respectively. Theoretically, allotropes of carbon c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C15/54C07C2/38
Inventor 肖胜雄吴彬李和兴刘泰峰李满荣邱晓艳刘珍凤
Owner SHANGHAI NORMAL UNIVERSITY
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