Graphene oxide modified with spirooxazine photochromic group and preparation method of graphene oxide
A photochromic and spirooxazine technology, applied in chemical instruments and methods, color-changing fluorescent materials, organic chemistry, etc., to achieve good film-forming performance, practical, and excellent photochromic performance
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[0043]The preparation method of the material is obtained by using spirooxazine group-containing acrylate and vinyl monomers as comonomers, initiating with an initiator in an organic solvent, and co-polymerizing with graphene oxide. Wherein, the acrylate structural formula containing spirooxazine group is:
[0044]
[0045] Acrylic esters containing spirooxazine groups can be prepared by chemical synthesis, as reported in the literature (catalyzed synthesis of acryloyloxyindoline spironaphthoxazine dyes with triethylamine, Synthetic Materials Aging and Application, 2009 Volume 38, No. 3, pages 24-27) were synthesized by the method.
[0046] The synthesis route of the graphene oxide modified by the spirooxazine photochromic group of the present invention is as follows.
[0047]
[0048] Among them, GO refers to graphene oxide; A is -H or -CH 3 , B is p=1-1000, x=1-1000, y=1-1000.
[0049] The preparation method specifically comprises the following steps:
[0050] S...
Embodiment 1
[0055] Add 30mL of DMF (N,N-dimethylformamide) and 0.03g of graphene oxide into a 100mL round bottom flask, and disperse evenly by ultrasonication for 20min; then add 0.6g of ethyl acrylate and 0.2g of spirooxazine group-containing acrylate , BPO (benzoyl peroxide) 0.03g, stir evenly, ultrasonically disperse for 20min, and reflux for 6h. After the reflux was completed, the mixed solution was cooled to room temperature, and about 6 times the volume of methanol was poured into it, and flocs appeared. Use a 0.22 μm microporous nylon filter membrane to vacuum filter, then wash the filtrate with DMF until the washing solution is colorless, and dry it in vacuum to obtain a crude product. Place the nylon filter membrane adsorbed with the crude product in 30mL THF (tetrahydrofuran), ultrasonically dissolve it for 20min, centrifuge the solution at 4000r / min for 180min, collect the supernatant, and vacuum filter it with a 0.22μm microporous nylon filter membrane, and then The filtrate ...
Embodiment 2
[0057] In a 100mL round bottom flask, add 30mL of DMAC (N,N-dimethylacetamide), 0.03g of graphene oxide, and disperse evenly by ultrasonication for 20min; then add 0.3g of methyl methacrylate, acrylate containing spirooxazine (IV) 0.03g, BPO0.03g, stir evenly, ultrasonically disperse for 20min, and reflux for 2h. After the reflux was completed, the mixed solution was cooled to room temperature, and about 2 times the volume of methanol was poured into it, and flocs appeared. Use a 0.22 μm microporous nylon filter membrane to vacuum filter, then wash the filtrate with DMAC until the washing solution is colorless, and dry it in vacuum to obtain a crude product. Place the nylon filter membrane with the crude product adsorbed in 30mL THF, ultrasonically dissolve it for 20min, centrifuge the solution at 6000r / min for 100min, collect the supernatant, vacuum filter it with a 0.22μm microporous nylon filter membrane, and wash it with THF Filtrate, collect the solid filtrate, and vacuu...
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