Preparation method of M1/M2xP-type monoatomic catalyst
A catalyst, M12L2 technology, applied in catalyst activation/preparation, physical/chemical process catalysts, chemical instruments and methods, etc., can solve problems such as difficult to control metal dispersion, achieve controllable active sites and loading, and simple synthesis , the effect of long service life
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Embodiment 1
[0034] (1) In an inert atmosphere, M 1 Metal organic complex [Ag( i Pr-MeAMD)] 2 Dissolve in anhydrous organic toluene solvent to obtain a solution with a concentration of 15 mg / L;
[0035] (2) Fe from the market 2 P-type metal phosphide is the carrier. Put 1.0g of it in the bottle. Under an inert atmosphere, first add anhydrous toluene solvent (40mL), and slowly drop 4mL of the solution prepared in step (1) into it under stirring. After the addition is complete, continue to reflux and stir under an inert atmosphere for 0.5 h at 110°C, filter and wash with anhydrous toluene to obtain an intermediate product;
[0036] (3) Disperse the intermediate product obtained in step (2) in anhydrous toluene (40 mL), and then add 2 mL of the reducing agent methyl aluminum, let it reflux and stir for 0.5 h at 80°C, filter, and use ether Wash the filter residue 3 times and dry it to obtain the single atom catalyst Ag / Fe 2 P;
[0037] The loading amount of the catalyst prepared in this embodiment i...
Embodiment 2
[0042] (1) In an inert atmosphere, M 1 Metal organic complex [Cu( i Pr-MeAMD)] 2 Dissolve in anhydrous organic tetrahydrofuran solvent to obtain a solution with a concentration of 10mg / L;
[0043] (2) Ni 2 P-type metal phosphide is the carrier. Put 1.0g of it in a bottle, add anhydrous tetrahydrofuran solvent (50mL) under an inert atmosphere, slowly add 15mL of the solution prepared in step (1) to it with stirring, dropwise After completion, stirring was continued at 50°C under an inert atmosphere for 16 hours, filtered and washed with anhydrous tetrahydrofuran to obtain an intermediate product;
[0044] (3) Disperse the obtained intermediate product in anhydrous tetrahydrofuran (50mL), then add 2mL of the reducing agent hydrazine (N 2 H 4 ), let it stir for 10h at 25℃, filter, wash the filter residue with n-hexane solvent 3 times, and dry it to obtain the monoatomic catalyst Cu / Ni 2 P, the load is measured to be 10wt%.
[0045] Using the catalyst prepared in this embodiment to degra...
Embodiment 3
[0049] (1) In an inert atmosphere, M with a specific electron-deficient structure 1 Metal organic complex [Ni( t Bu-DAD) 2 ] Dissolve in anhydrous ether solvent to obtain a solution with a concentration of 15mg / L;
[0050] (2) Fe obtained from the market 2 P-type metal phosphide is the carrier, put 1.0g of it into the bottle, add anhydrous toluene solvent (45mL) under an inert atmosphere, slowly add 6mL of the solution prepared in step (1) to it while stirring, dropwise After completion, continue to stir at 25°C under an inert atmosphere for 24 hours, filter and wash with anhydrous ether to obtain an intermediate product;
[0051] (3) Disperse the obtained intermediate product in anhydrous ether (45 mL), add 3 mL of the reducing agent methyl borane, let it stir at 60°C for 6 hours, filter, and wash the filter residue with n-hexane solvent 3 times , Drying to obtain a single atom catalyst Ni / Fe 2 P single-atom catalyst with a loading amount of 0.08wt%;
[0052] Use the catalyst prepa...
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