A method for preparing monofluoromethane with PD-M alloy supported catalyst
A supported catalyst, fluoromethane technology, applied in the field of single-atom alloy catalyst preparation, can solve the problems of low conversion rate of gas-phase fluorination synthesis route, by-product methane has no economic value, unsatisfactory catalyst life, etc., to achieve environmental protection of synthesis process route , Moderate hydrogenation capacity, moderate acid-base performance
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Embodiment 1
[0026] 39mL of 0.02mol / L Cu(NO 3 ) 2 ·3H 2 O aqueous solution, 50mL of 0.01mol / L PVP aqueous solution and 50mL of 0.1mol / L ascorbic acid aqueous solution were mixed and placed under nitrogen atmosphere and stirred for 0.5h. Then add 10 mL of 0.1 mol / L sodium borohydride aqueous solution dropwise to the mixed solution, and continue stirring for 0.5 h; then add 1 g of AlF to the above solution 3 powder, continue to stir for 0.5~1h, ultrasonic for 5 minutes; filter, dry for 12h, and then place the dried solid in air at 300°C for 4h to obtain Cu / AlF 3 ; The above-baked Cu / AlF 3 After calcination and reduction at 250°C under a hydrogen atmosphere for 2 hours, passivation was calcined at 250°C for 1 hour under a nitrogen atmosphere, cooled to room temperature, and then placed in 9.4mL palladium nitrate aqueous solution (the concentration of palladium element is 0.0001mol / L) under a nitrogen atmosphere Continue to stir for 0.5~1h, the temperature of the mixed solution is 50°C, an...
Embodiment 2
[0029] Mix 18mL of 0.02mol / L ZnCl aqueous solution, 50mL of 0.01mol / L PVP aqueous solution and 50mL of 0.1mol / L sodium citrate aqueous solution and stir for 2h under a nitrogen atmosphere. The flow rate is 10mL / min. Then, 10 mL of 0.1 mol / L sodium borohydride aqueous solution was added dropwise to the mixture, and stirring was continued for 1 h; then 1 g of MgF 2 powder, continue to stir for 0.5~1h, ultrasonic for 5 minutes; filter, dry for 12h, and then place the dried solid in air at 300°C for 4h to obtain Zn / MgF 2 ; The above-mentioned roasted Zn / MgF 2 After calcination and reduction at 250°C under a hydrogen atmosphere for 2 hours, passivation was calcined at 250°C for 1 hour under a nitrogen atmosphere, cooled to room temperature, and then placed in 9.4mL aqueous solution of chloropalladium acid under a nitrogen atmosphere (the concentration of palladium element is 0.0001mol / L) Stirring was continued for 0.5~1h, the temperature of the mixture was 50°C, and the flow rate...
Embodiment 3
[0032] Mix 18mL of 0.02mol / L ZnCl aqueous solution, 50mL of 0.01mol / L PVP aqueous solution and 50mL of 0.1mol / L sodium citrate aqueous solution and stir under a nitrogen atmosphere for 0.5~1h. The temperature of the mixed solution is 50°C. The flow rate of nitrogen is 10mL / min. Then add 10mL of 0.1mol / L sodium borohydride aqueous solution to the mixture dropwise, and continue to stir for 0.5~1h; then add 1g of MgF to the above solution 2 powder, continue to stir for 0.5~1h, ultrasonic for 5 minutes; filter, dry for 12h, and then place the dried solid in air at 300°C for 4h to obtain Zn / MgF 2 ; The above-mentioned roasted Zn / MgF 2 After being reduced for 2 hours under a hydrogen atmosphere at 250°C, passivation was calcined at 250°C for 1 hour under a nitrogen atmosphere, cooled to room temperature, and then placed in 9.4mL palladium nitrate aqueous solution (the concentration of palladium element is 0.0001mol / L) under a nitrogen atmosphere to continue Stir for 0.5~1h, the te...
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