Preparation and application of copper (II) tetracarboxyphenyl porphyrin/titanium dioxide composite material with high catalytic activity
A technology of titanium dioxide and phenyl porphyrin, applied in the directions of carbon monoxide, hydrocarbon production from carbon oxides, organic compounds/hydrides/coordination complex catalysts, etc.
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[0042] (2) Preparation of TCPP: Take 6.08 g (40.5 mmol) of 4-formylbenzoic acid and 2.8 g (40.5 mmol) of double-distilled pyrrole, add 120 ml of propionic acid, and heat to reflux for 2 to 3 hours. Then the reacted mixture was cooled to room temperature, and 150 ml of methanol was added, while cooling and stirring in an ice bath for 0.5-1 hour. A precipitate was obtained by centrifugation and washed several times with methanol and heated distilled water until the filtrate was clear. Finally, the obtained purple powder was dried in an oven at 60-80°C for 10-12 hours to obtain 1.587 gTCPP.
[0043] (3) Preparation of CuTCPP: Take TCPP (0.261 g, 0.33 mmol) and CuCl 2 • 2 h 2 O (0.31 g, 1.82 mmol), was added to 20 ml N,N dimethylformamide, refluxed for 4~5 hours, cooled to room temperature, and a red solution was obtained 。 The precipitate was centrifuged and washed several times with a large amount of water until the filtrate was clear, and the solid product was vacuum-dried ...
Embodiment 5、2
[0064] Embodiment 5, 2.0% CuTCPP / P25 m Preparation and performance studies of
[0065] (1) Titanium dioxide P25 treatment: same as Example 1;
[0066] (2) Preparation of TCPP: Same as Example 1;
[0067] (3) Preparation of CuTCPP: Same as Example 1;
[0068] (4) 2.0% CuTCPP / P25 m Preparation: 0.6 g P25 m Add 12 mg CuTCPP to 30 ml ethanol, heat and reflux at 80-90°C for 4-5 hours, centrifuge the mixture, and wash with ethanol several times to remove unbound excess CuTCPP until the filtrate is clear, Dry overnight at ℃ to get 2.0% CuTCPP / P25 m Composite catalyst.
[0069] (5) 2.0% CuTCPP / P25 m CO / CH 4 The total release and yield: total CO / CH under 300 W xenon lamp irradiation 4 They are 1.45 μmol / g / h and 4.12 μmol / g / h respectively.
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