Method for preparing graphite alkyne film
A graphdiyne and thin film technology is applied in the field of preparing graphdiyne thin films to achieve the effects of simple process and uniform surface
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[0027] Example 1,
[0028] At 8°C, to a tetrahydrofuran (THF) solution containing 43.6 milligrams (mg) (0.066 millimoles (mmol)) of compound 1 was added 0.4 ml of tetrabutylammonium fluoride (TBAF) (1 mole / liter (M) tetrahydrofuran) Solution, 0.4mmol), stirred for 10 minutes under nitrogen protection. Then the reaction solution was diluted with ethyl acetate (20 mL), washed three times with saturated brine, dried over anhydrous sodium sulfate (10 g), and concentrated to dryness to obtain hexaynylbenzene (compound 2) (9.08 mg, 62%). Dissolve compound 2 with 25ml of pyridine, slowly drop it into a three-necked flask containing 50ml of pyridine and copper foil (4 square centimeters) under the protection of nitrogen (the temperature of the reaction solution is 60℃), and add time For 24 hours. Then the stirring reaction was continued at 60°C for 3 days. After the reaction is completed, a black film is formed on the copper sheet, and the copper sheet is washed sequentially with acet...
Example Embodiment
[0037] Example 2,
[0038] At 8°C, to a tetrahydrofuran (THF) solution containing 43.6 milligrams (mg) (0.066 millimoles (mmol)) of compound 1 was added 0.4 ml of tetrabutylammonium fluoride (TBAF) (1 mole / liter (M) tetrahydrofuran) Solution, 0.4mmol), stirred for 10 minutes under nitrogen protection. Then the reaction solution was diluted with ethyl acetate (20 mL), washed three times with saturated brine, dried over anhydrous sodium sulfate (10 g), and concentrated to dryness to obtain hexaynylbenzene (compound 2) (9.08 mg, 62%). Dissolve compound 2 with 25ml of pyridine, slowly drop it into a three-necked flask containing 50ml of pyridine and copper foil (4 square centimeters) under the protection of nitrogen (the temperature of the reaction solution is 50°C), and add time For 24 hours. Then the stirring reaction was continued at 50°C for 3 days. After the reaction, a black film is formed on the copper sheet, and the copper sheet is washed with acetone and N,N-dimethylforma...
Example Embodiment
[0039] Example 3.
[0040] At 8°C, to a tetrahydrofuran (THF) solution containing 43.6 milligrams (mg) (0.066 millimoles (mmol)) of compound 1 was added 0.4 ml of tetrabutylammonium fluoride (TBAF) (1 mole / liter (M) tetrahydrofuran) Solution, 0.4mmol), stirred for 10 minutes under nitrogen protection. Then the reaction solution was diluted with ethyl acetate (20 mL), washed three times with saturated brine, dried over anhydrous sodium sulfate (10 g), and concentrated to dryness to obtain hexaynylbenzene (compound 2) (9.08 mg, 62%). Dissolve compound 2 with 25ml of pyridine, slowly drop it into a three-necked flask containing 50ml of pyridine and copper foil (4 square centimeters) under the protection of nitrogen (the temperature of the reaction solution is 80℃), and add time For 24 hours. Then the stirring reaction was continued at 80°C for 3 days. After the reaction is completed, a black film is formed on the copper sheet, and the copper sheet is washed with acetone and N,N-d...
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