A kind of carbon-supported palladium catalyst and its preparation method and application
A palladium catalyst, carbon-supported technology, used in catalyst supports, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of metal particle growth, low oxidation resistance, poor mechanical stability of activated carbon, etc. effect of action
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Embodiment 1
[0025] (1) take by weighing 1-2g commercially available original nano-diamond ( figure 1 ), put it into the crucible, put the crucible into the tube furnace, feed inert gas, and rise to 500-1100°C at a heating rate of 5K / min (the present embodiment heats up to 900°C and 1100°C respectively), and keep warm for 4 -6 hours. Cool to room temperature under an inert atmosphere to obtain a graphene-like and nano-diamond composite nano-carbon material carrier.
[0026] Such as Figure 2-3 As shown, the obtained carrier has a core-shell structure with nano-diamond as the core and graphene-like as the shell, and the graphene-like is formed by stacking 1-3 layers of graphene materials. The specific surface area of the nano-carbon material carrier is 300-400m 2 / g, the total pore volume is 1.3-1.5cm 3 / g, almost no micropores exist, and there are a large number of fixed palladium particles on the surface.
[0027] (2) Take this carrier 200g, be dispersed in 300mL water, adjust its ...
Embodiment 2
[0029] The 1# catalyst prepared in Example 1 is applied to the Suzuki coupling reaction, the solvent used is 40ml of a mixed solution of ethanol and water, the amount of palladium is 0.0021mmol, the amount of bromobenzene is 4mmol, and the amount of phenylboronic acid is 4.8 mmol, the amount of potassium carbonate is 8mmol. When the reaction temperature was 30°C, the conversion rate of bromobenzene was 28% after 10 minutes of reaction, and when the reaction temperature was 50°C, the conversion rate of bromobenzene was 99% after 10 minutes of reaction.
[0030] The 1# catalyst prepared in Example 1 was applied to catalyze the CO oxidation reaction, and the space velocity was 17040ml h -1 g cat -1 , the volume concentration of CO is 0.9%, CO and O 2 The volume ratio is 1:10, and the corresponding temperature is 70°C when the CO conversion rate reaches 50%.
Embodiment 3
[0032] The 1# catalyst prepared in Example 1 was calcined at high temperature.
[0033] Weigh a certain amount of catalyst and put it into a tube furnace, raise the temperature to 350-800°C at a rate of 5k / min under an inert atmosphere, keep it warm for 6h, and cool to room temperature under an inert atmosphere. Compared with the oxidized carbon nanotube-supported palladium catalyst and the onion-like carbon-supported palladium catalyst, the average particle size of the palladium particles of the 1# catalyst changed from 1.9nm to 2.6nm after calcination at 500°C for 6h. When the calcination temperature increased to 800℃, the palladium particles grew significantly.
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