A centimeter-sized graphdiyne synthesized by liquid-liquid interface polymerization and its preparation method and application
A technology of graphyne and solution, which is applied in the field of centimeter-scale graphyne and its preparation, which can solve the problems of difficult uniformity of graphyne film thickness and shape, limit the application of graphyne products, and uncontrollable synthesis, and achieve good continuous uniformity , excellent electronic properties, and structurally stable effects
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Embodiment 1
[0037] Example 1: Preparation of graphite alkyne film with tetras (4-ethynylphenyl) methane as an alkynyl monomer
[0038] 1. Preparation of tetrakis(4-ethynylphenyl)methane
[0039] (1) Under room temperature conditions, the tetraphenylmethane and bromine element were added to the flask and stirred for 5 h, the resulting product was transferred to the environmental conditions of -78 °C, and the ethanol solution was slowly added until the precipitate was no longer generated; the precipitate product was washed and separated with sodium thiosulfate saturated solution, and the separated product was purified by the column to give the white solid product A (510mg, 29%).
[0040] (2) 0.8 g of white solid product A, 108 mg of PdCl 2 Dissolve 24.6 mg of CuI in 30 mL of i-Pr 2 NH and 0.86 mL of trimethylsilyl acetylene solution, and after reacting under nitrogen protection conditions for 42 h, the resulting product was purified by a column to give the off-white solid product B (0.6 g, 67%)...
Embodiment 2
[0057] Example 2 Preparation of graphite alkyne film with tetras (4-ethynylphenyl) methane as an alkynyl monomer
[0058] To perform a reaction similar to that in Example 1, in addition to the concentration of the tetra (4-ethynylphenyl) methane solution in Example 1 becomes 1 mM, the amount of concentration ratio of the substance controlling tetra (4-ethynylphenyl) methane, copper acetate and pyridine is 10: 20: 1. By this reaction, a graphite alkyne film with transverse dimensions in the centimeter level is obtained. Compared with the graphite alkyne film obtained under the conditions of Example 1, the graphite alkyne film obtained under this condition is thinner and more fragile, relatively speaking, the graphite alkyne film structure of Example 1 is more stable.
Embodiment 3
[0059] Example 3 Preparation of graphite alkyne film with tetras (4-ethynylphenyl) methane as alkyne monomer
[0060] To perform a reaction similar to that in Example 1, in addition to the concentration of the tetra (4-ethynylphenyl) methane solution in Example 1 becomes 4 mM, the amount of concentration ratio of the material controlling tetra (4-ethynylphenyl) methane, copper acetate and pyridine is 40: 20: 1. By this reaction, a graphite alkyne film with transverse dimensions in the centimeter level is obtained. Compared with the graphite alkyne film obtained under Example 1, the graphite alkyne film obtained under this condition is thicker, but the cost is higher, and the economic applicability is not as good as In Example 1.
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