Phenanthroline copper complex catalyst and its preparation method and application
A technology of copper complex and phenanthroline, which is applied in the field of alkyl carbonate, can solve the problems of poor solubility, complex catalyst preparation, difficulty in large-scale equipment, etc., to meet the needs of industrial production processes, good application prospects, structural stable effect
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Embodiment 1
[0020] Dissolve 3.6g (0.02mol) of 1,10-phenanthroline (phen) in 60ml of ethanol, stir for 10 minutes, then slowly add dropwise to 60ml of methanol solution containing 4.467g (0.02mol) of copper bromide, after the addition Stir at room temperature for 30 minutes, let stand for 30 minutes, crystallize, and filter; add 300ml of methanol into a reaction kettle lined with tetrafluoroethylene, suspend the filtered solid in the reaction kettle, and conduct a solvothermal reaction at 130°C for 72 hours , get solid [Cu(phen) 2 Br] 2 [Cu 4 Br 6 ], the yield is 49.2% (in terms of copper).
[0021] In 100ml autoclave, add 20ml (0.494mol) methanol, 0.021g (0.000012mol) [Cu(phen) 2 Br] 2 [Cu 4 Br 6 ] complex catalyst, at room temperature with mixed gas (O 2 : 6%, CO: 94%) to replace the air in the reactor, and then use the mixed gas to pressurize to 5.0MPa. The reaction was carried out at a reaction temperature of 130° C. for 5 hours. After cooling, a clear sample was taken for ga...
Embodiment 2
[0023] Dissolve 4.16g (0.02mol) of 2,9-dimethyl-1,10-phenanthroline (2,9-dimethyl-phen) in 60ml of ethanol, stir for 20 minutes, then slowly add dropwise to 60ml containing 4.467g (0.02mol) methanol solution of copper bromide, after adding, stir at room temperature for 2 hours, let stand for 30 minutes, crystallize, filter; add 300ml acetone in the reactor lined with tetrafluoroethylene, filter the obtained The solid was suspended in the reactor, and reacted solvothermally at 100°C for 15 hours to obtain the solid [Cu(2,9-dimethyl-phen) 2 Br] 2 [Cu 4 Br 6 ], the yield is 62.1% (in terms of copper).
[0024] In a 100ml autoclave, add 20ml (0.494mol) methanol, 2.696g (0.0015mol) [Cu(2,9-dimethyl-phen) 2 Br] 2 [Cu 4 Br 6 ] complex catalyst, at room temperature with mixed gas (O 2 : 6%, CO: 94%) to replace the air in the reactor, and then use the mixed gas to pressurize to 9.0MPa. The reaction was carried out at a reaction temperature of 120° C. for 1.0 hour. After cooli...
Embodiment 3
[0026] Dissolve 4.16g (0.02mol) of 4,7-dimethyl-1,10-phenanthroline (4,7-dimethyl-phen) in 50ml of acetonitrile, stir for 20 minutes, then slowly add dropwise to 60ml containing 4.467g (0.02mol) methanol solution of copper bromide, stirred at room temperature for 2 hours after addition, stirred at room temperature for 2 hours after addition, stood for 30 minutes, crystallized, filtered; Add 300ml of absolute ethanol to the kettle, suspend the filtered solid in the reaction kettle, and conduct a solvothermal reaction at 170°C for 120 hours to obtain a solid [Cu(4,7-dimethyl-phen) 2 Br] 2 [Cu 4 Br 6 ], the yield is 51.7% (in terms of copper).
[0027] In a 100ml autoclave, add 20ml (0.494mol) methanol, 0.899g (0.0005mol) [Cu(4,7-dimethyl-phen) 2 Br] 2 [Cu 4 Br 6 ] complex catalyst, at room temperature with mixed gas (O 2 : 6%, CO: 94%) to replace the air in the reactor, and then use the mixed gas to pressurize to 0.5MPa. The reaction was carried out at a reaction temper...
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