Preparation method of three-dimensional ordered mesoporous molybdenum oxide
A three-dimensional mesopore and sequenced mesopore technology, applied in the direction of molybdenum oxide/molybdenum hydroxide, can solve the problems of poor pore structure regularity, easy channel collapse, and poor universality of the method, achieving low cost, narrow pore size distribution, The effect of simple operation process
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Embodiment example 1
[0024] 1) Synthesis of three-dimensional mesoporous silica powder KIT-6: at room temperature, add 2.7g triblock copolymer (EO) to 100mL 0.5mol / L hydrochloric acid solution 20 (PO) 70 (EO) 20 (PluronicP123), stir until dissolved, slowly (2°C / min) heat up to 35°C, add 2.8g n-butanol while stirring, and keep stirring at 35°C for 1 hour, then add 5.8g ethyl orthosilicate to the above solution Esters (the molar ratio of each substance is: ethyl orthosilicate: triblock copolymer (EO) 20 (PO) 70 (EO) 20: hydrochloric acid: deionized water: n-butanol=1: 0.017: 1.83: 195: 1.31), keep stirring at 35°C for 24 hours, transfer to an autoclave and heat at 100°C for 24 hours, filter, deionized water and ethanol After washing, it was dried at 60°C, and then the temperature was programmed in a muffle furnace (1°C / min) to 550°C and fired at 550°C for 4 hours to obtain a three-dimensional mesoporous silica (KIT-6) white powder. The specific surface area of the resulting KIT-6 is 780m 2 / ...
Embodiment example 2
[0029] 1) The synthesis of three-dimensional mesoporous silica powder KIT-6 is the same as step 1 in Example 1);
[0030] 2) The synthesis of three-dimensional ordered mesoporous carbon is the same as step 2 in Example 1);
[0031] 3) Put 0.5 g of the three-dimensional mesoporous carbon powder prepared in step 2) into an Erlenmeyer flask whose bifurcated end is connected to a dropping funnel with a piston connected to the other end of a vacuum pump, and vacuumize at 90KPa for 60 minutes, wherein, A buffer bottle is connected between the Erlenmeyer flask and the vacuum pump to ensure the vacuum in the Erlenmeyer flask. After vacuuming, turn off the vacuum pump, and then add 20ml of 0.032mol / L (NH 4 ) 6 Mo 7 o 24 The aqueous solution was slowly dropped into the three-dimensional mesoporous carbon from the dropping funnel under vacuum. After the dropwise addition, continue to keep the conical flask at its vacuum degree and ultrasonically disperse for 100 minutes so that the ...
Embodiment example 3
[0034] 1) The synthesis of silicon template KIT-6 is the same as step 1 in Example 1);
[0035] 2) The synthesis of the carbon template is the same as step 2 in Example 1);
[0036] 3) Put 0.5 g of the three-dimensional mesoporous carbon powder prepared in step 2) into an Erlenmeyer flask whose bifurcated end is connected to a dropping funnel with a piston connected to the other end of a vacuum pump, and vacuumize at 90KPa for 60 minutes, wherein, A buffer bottle is connected between the Erlenmeyer flask and the vacuum pump to ensure the vacuum in the Erlenmeyer flask. After vacuuming, turn off the vacuum pump, and then add 20ml of 0.04mol / L (NH 4 ) 6 Mo 7 o 24 The aqueous solution was slowly dropped into the three-dimensional mesoporous carbon from the dropping funnel under vacuum. After the dropwise addition, continue to keep the conical flask at its vacuum degree and ultrasonically disperse for 120 minutes so that the molecules can fully enter the pores of the three-di...
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