Beta-graphite diyne nano-film as well as preparation method and application thereof
A technology of graphdiyne and thin film, which is applied in the field of materials, can solve the problem that allotropic graphyne materials have not been synthesized, and achieve the effect of continuous structure and simple process and process
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Embodiment 1
[0042] The preparation of embodiment 1, β-graphdiyne nano film
[0043] 1) Preparation of tetrakynylethylene:
[0044] At 5°C, add 0.50 ml of tetrabutylammonium fluoride (TBAF) to a solution containing 50.0 mg (0.121 mmol (mmol)) of compound 1 in tetrahydrofuran (THF) ), and the reaction was stirred for 15 minutes under the protection of argon. Afterwards, the reaction solution was diluted with ethyl acetate (30 ml), washed three times with saturated brine, dried over anhydrous magnesium sulfate (5 g), and concentrated to dryness to obtain 9.3 mg, 62%) of tetrakyneethylene (compound 2).
[0045] 2) Preparation of β-graphdiyne nanofilm:
[0046] Such as figure 2As shown in the device, 9.3 mg of tetrakyne ethylene (compound 2) obtained in step 1) was dissolved with 20 ml of acetone and stored in a syringe pump. The syringe pump was placed in a dry ice trap to protect compound 2. Add dropwise to a three-neck flask containing 100ml of a mixture of pyridine and acetone with a ...
Embodiment 2
[0058] The preparation of embodiment 2, β-graphdiyne nano film
[0059] 1) Preparation of tetrakynylethylene:
[0060] With embodiment 1 step 1);
[0061] 2) Preparation of β-graphdiyne nanofilm:
[0062] Dissolve compound 2 with 20ml of acetone and store it in a syringe pump. The syringe pump is placed in a dry ice trap to protect compound 2. At the same time, it is slowly added dropwise to 100ml of pyridine with a volume ratio of 1:9 under the protection of argon. In the there-necked flask of the mixed solution composed of acetone, the dropwise addition time is 10 hours. Using 1.9g of copper foil as the reaction substrate, add 1.54g of tetramethylethylenediamine (TMEDA), and carry out the coupling reaction at a temperature of 45°C for 10 hours. After the reaction, a black film is formed on the copper foil. , wash the copper foil with N,N-dimethylformamide, acetone, and ethylene glycol in turn, and the black film is the β-graphdiyne film provided by the present invention, ...
Embodiment 3
[0064] The preparation of embodiment 3, β-graphdiyne nano film
[0065] 1) Preparation of tetrakynylethylene:
[0066] With embodiment 1 step 1);
[0067] 2) Preparation of β-graphdiyne nanofilm:
[0068] Dissolve compound 2 with 20ml of acetone and store it in a syringe pump. The syringe pump is placed in a dry ice trap to protect compound 2. At the same time, it is slowly added dropwise to 100ml of pyridine with a volume ratio of 1:9 under the protection of argon. In the there-necked flask of the mixed solution composed of acetone, the dropwise addition time is 16 hours. With 1.9g of copper foil as the reaction substrate, 1.54g of tetramethylethylenediamine (TMEDA) was added, and the reaction temperature was 45°C for coupling reaction for 16 hours. After the reaction, a black film was formed on the copper foil. Wash the copper foil with N,N-dimethylformamide, acetone, and ethylene glycol in sequence, and the black film is the β-graphdiyne film provided by the present inve...
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