A kind of organic-inorganic hybrid fluorescent sensing material and its synthesis method and application
A technology of fluorescence sensing and synthesis method, which is applied in the field of organic-inorganic hybrid fluorescence sensor and its preparation, can solve the problems of complexity, high analysis cost, and difficulty in real-time detection, and achieve high selectivity detection, high fluorescence quantum Yield, easy synthesis effect
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Embodiment 1
[0026] Embodiment 1: Synthesis of organic-inorganic hybrid fluorescent sensing material P1
[0027] Weigh 1.225 g (1.4 mmol) heptaisobutyl-propylamino polysilsesquioxane (C 31 h 71 NO 12 Si 8 ), 0.224 g (1.4 mmol) 8-formylquinoline (KL), 10 mL dichloromethane (CH 2 Cl 2 ) into a 50 mL round bottom flask at one time, stirred at room temperature, and the reaction lasted for 12 h. When the solvent dichloromethane was added, the solids of the reactants were all dissolved and turned into a light yellow solution. After 12 h, the color of the solution changed significantly to yellow. The mixture obtained by the reaction was evaporated with a rotary evaporator to remove the solvent to obtain a yellow solid mixture, which was then washed and filtered with 50 mL of methanol, and washed and filtered 5 times repeatedly, and the yield after drying was 67%. Abbreviated as P1.
[0028] The structural formula is as follows:
[0029]
[0030] IR (KBr, cm -1 ): 2965, 2865, 1634, 15...
Embodiment 2
[0031] Embodiment 2: to Fe under solution state (homogeneous phase) 3+ Ion detection
[0032] The THF solution concentration of P1 is 2.5×10 -6 M, using Fe 3+ Ions (0-5.0×10 -4M) Titration, causing the ultraviolet absorption at a wavelength of 286nm to be enhanced, and has a nonlinear correlation, and the correlation coefficient R is 0.992.
[0033] THF solution concentration 2.5 x 10 -6 M, adding Fe 3+ Can lead to fluorescence quenching, the emission at 438nm shows a nonlinear weakening, for Fe 3+ The detection range is 0-2.1×10 -3 M, detection limit 1.6×10 -6 M. Add 5 equivalents of eleven different metal ions: Zn 2+ 、 Cu 2+ , Ca 2+ 、 Al 3+ 、Ni 2+ 、Cr 3+ , Mn 2+ , Pb 2+ 、 Ba 2+ 、Na + , Fe 2+ , and found that they interfere less with iron ions.
[0034] Selective experiments for the sensor to detect iron ions, figure 1 is Fe 3+ Ion titration of the THF solution of P1, the concentration of P1 is 2.5×10 -6 M mol / L, when Fe 3+ The ion concentratio...
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