Troger's base conjugated microporous polymer photocatalyst, and preparation method and application thereof
A technology towards Geer bases and microporous polymers, applied in the direction of organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of insufficient absorption and utilization of visible light , to achieve excellent CO2 adsorption capacity, large application potential, and large specific surface area
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Embodiment 1
[0034] The reaction equation of the present embodiment is as follows:
[0035]
[0036] Dissolve 2.369g diiodochauger base (5.0mmol) in 40mL anhydrous N,N-dimethylformamide, add 3.344g carbazole (20mmol), 2.764g potassium carbonate (20mmol), 0.095g iodine Cuprous chloride (0.5mmol) and 0.009g 1,10-phenanthroline (0.05mmol) were reacted at 150°C for 24h under nitrogen protection. Cool to room temperature, remove the solvent, and purify the product by column chromatography (ethyl acetate / petroleum ether=1:3) to obtain a light brown carbazole-based conjugated microporous polymer monomer.
[0037]Disperse 0.203g (0.367mmol) of carbazole-based conjugated microporous polymer monomer in 25mL of anhydrous chloroform, then add 0.595g (3.67mmol) of ferric chloride, and react at 60°C for 24h under nitrogen protection. Then 50 mL of methanol was added to the reaction mixture, and the resulting mixture was stirred for another 1 hour, and the precipitate was collected by filtration and ...
Embodiment 2
[0043] The reaction equation of the present embodiment is as follows:
[0044]
[0045] With 20ml of N,N-dimethylformamide and 20ml of triethylamine mixed solution as the reaction medium, add 0.356g of diiodo Chaoger base (0.75mmol), 0.075g of 1,3,5-triethynylbenzene ( 0.5mmol), 0.029g Pd (pph 3 ) 4 (0.025mmol) and 0.005g CuI (0.025mmol), reacted at 80°C for 24h under nitrogen protection. Collect the precipitate after the reaction, stir the precipitate in hydrochloric acid solution for 1 hour, wash with water, stir in a mixed solution of acetone, toluene and methanol for 1 hour, dry, and perform Soxhlet extraction with a mixed solution of methanol and tetrahydrofuran to obtain a yellow Conjugated microporous polymer in powder form.
[0046] Figure 5 It is the infrared spectrogram of the conjugated microporous polymer prepared in Example 2. Among them at 1316cm -1 and 1097cm -1 It is the stretching vibration absorption peak of C-N outside the ring, which is the carbo...
Embodiment 3
[0050] The reaction equation of the present embodiment is as follows:
[0051]
[0052] With 20ml of N,N-dimethylformamide and 20ml of triethylamine mixed solution as the reaction medium, add 0.356g of diiodochauger base (0.75mmol), 0.063g of 1,4-diethynylbenzene (0.5mmol ), 0.029g Pd (pph 3 ) 4 (0.025mmol) and 0.005g CuI (0.025mmol), reacted at 80°C for 24h under nitrogen protection. Collect the precipitate after the reaction, stir the precipitate in hydrochloric acid solution for 1 hour, wash with water, stir in a mixed solution of acetone, toluene and methanol for 1 hour, dry, and perform Soxhlet extraction with a mixed solution of methanol and tetrahydrofuran to obtain a yellow Conjugated microporous polymer in powder form.
[0053] Figure 8 It is the infrared spectrogram of the conjugated microporous polymer prepared in Example 3. Among them at 1316cm -1 and 1097cm -1 It is the stretching vibration absorption peak of C-N outside the ring, which is the carbon-ni...
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