Beta-cyclodextrin/polyethylene imine/graphene oxide composite material, preparation method thereof, composition and detection method
A technology of polyethyleneimine and composite materials, which is applied in the direction of material excitation analysis, fluorescence/phosphorescence, etc., can solve the problems of using toxic reagents, complicated operation, and time-consuming, etc., and achieve the effect of low detection limit and simple operation
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[0031] The present invention also provides a preparation method according to the above-mentioned β-cyclodextrin / polyethyleneimine / graphene oxide composite material, the reaction mechanism diagram is as follows figure 1 Shown, wherein, described preparation method comprises:
[0032] (1) In the presence of the first organic solvent, carry out the first contact reaction of β-cyclodextrin and N,N'-carbonyldiimidazole to prepare N,N'-carbonyldiimidazole-β-cyclodextrin;
[0033] (2) In the presence of a second organic solvent and an organic base, the N,N'-carbonyldiimidazole-β-cyclodextrin is grafted with polyethyleneimine to obtain a β-cyclodextrin-polyethyleneimine Ethylene imine;
[0034] (3) In the presence of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide, the β-cyclodextrin-polyethylene The imine and graphene oxide are subjected to a second contact reaction in a phosphate buffer solution to prepare a β-cyclodextrin / polyethyleneimine / gra...
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[0063] Dissolve 2.1g of β-cyclodextrin and 4.0g of N,N'-carbonyldiimidazole in 25mL of N,N'-dimethylformamide and mix at 25°C for 1h under nitrogen protection to obtain mixture M1; Mixture M1 was placed in diethyl ether at -2°C for 1 hour, and N,N'-carbonyldiimidazole-β-cyclodextrin was obtained after filtration; N,N'-carbonyldiimidazole-β-cyclodextrin was dried and dissolved in 25mL dimethyl sulfoxide to obtain a mixture M3; 7.5g polyethyleneimine was dissolved in 15mL dimethyl sulfoxide to obtain a mixture M4; the mixture M3 and 1.5mL triethylamine were mixed at 40 drops / min The rate was added dropwise into the mixture M4, and left for 5 hours to obtain the mixture M5; the mixture M5 was dialyzed with deionized water for 3 days, and β-cyclodextrin-polyethyleneimine was obtained after freeze-drying.
[0064] Disperse 0.5g of graphene oxide in 25mL of phosphate buffer solution, sonicate for 30min under magnetic stirring, and dissolve 1-(3-dimethylaminopropyl)-3-ethylcarbodiimi...
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