Preparation method and application of Pd/HY molecular sieve and method for selectively loading metal on hierarchical pore molecular sieve
A molecular sieve and selective technology, applied in the direction of molecular sieve catalysts, catalyst activation/preparation, chemical instruments and methods, etc., can solve the problem of low utilization of metal active sites and carrier acid sites, weakening the adsorption of reactants and intermediates, metal - Problems such as poor carrier interaction, to achieve the effect of increased activity, increased accessibility, and small size
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Embodiment 1
[0047] Embodiment 1: (water content 15wt%)
[0048] 10mL Pd(OAc) 2 / CH 2 Cl 2 solution (containing 10.6mg Pd(OAc) 2 ) into a round bottom flask as a hydrophobic solution. Take 450 mg of micro-mesoporous HY molecular sieves calcined in a muffle furnace at 550°C for 4h (the heating rate is 2.5°C / min). Then add 80 μL of ultrapure water and stir to make the water fully contact with the zeolite carrier. The resulting mixture was added to the palladium precursor solution and stirred continuously at room temperature for 24 h. After standing still, the metal precursor solution turns orange to colorless and transparent, and the zeolite precipitate turns yellow or brown. This phenomenon shows that Pd(OAc) 2 Transfer from DCM to HY molecular sieve surface. Then, the dichloromethane was removed by rotary evaporation. The resulting solid was washed with 100 mL CH 2 Cl 2 Wash, filter dry at room temperature, and then dry at 110°C for 12h. The sample powder changed from white to ...
Embodiment 2
[0049] Embodiment 2: (water content 20wt%)
[0050] The specific implementation conditions are similar to Example 1, but the amount of ultrapure water added is 115 μL (the volume of water is equal to the micropore volume of HY). The results of low-temperature nitrogen physical adsorption test show that the specific surface area and micropore volume of Pd / HY(20) are basically similar to those of unsupported HY (Table 1), indicating that palladium metal particles basically do not occupy the micropore channels of the carrier, and more Dispersed in the mesopores and on the outer surface. HAADF-STEM images such as figure 1 As shown in C, the palladium particles are uniformly dispersed on the carrier, and the particle size is 1.53±0.24nm.
Embodiment 3
[0051] Embodiment 3: (water content 30wt%)
[0052] The specific implementation conditions are similar to Example 1, but the amount of ultrapure water added is 200 μL (the volume of water is equal to the total pore volume of HY). The results of low-temperature nitrogen physical adsorption test show that the specific surface area of Pd / HY(30) is larger than that of the original HY zeolite, while the micropore volume remains unchanged (Table 1), indicating that the palladium metal particles do not occupy the micropore channels of the carrier, and all rivets are in the mesopores. and on the outer surface and form a certain degree of accumulation. HAADF-STEM images such as figure 1 As shown in C, the palladium particles are uniformly dispersed on the carrier, and the particle size is 1.74±0.37nm.
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