A kind of solid-state heteropolyacid composite catalyst with surface-modified variable-valence metal ions and its preparation method and application
A technology of variable valence metal ions and composite catalysts, applied in organic compound/hydride/coordination complex catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the effective catalytic area and active site reduction, treatment Cost increase, catalyst poisoning and other problems, to achieve the effect of wide application, improved utilization, no secondary pollution
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Embodiment 1
[0053] 1g phosphotungstic heteropoly acid (H 3 PW 12 o 40 , referred to as HPW) dissolved in 100mL deionized water, with KNO 3 For the ion source, control K + The molar ratio of HPW to HPW is 3:1, and the water-insoluble solid-phase heteropolyacid POM is obtained by chemical deposition. The above liquid is centrifuged at 12000r / min for 3min using a centrifuge, and the obtained solid is heated at 105°C Dry in oven. Take out the solid in the centrifuge tube and use an agate mortar to grind the solid to a fine powder state, and place it in a muffle furnace for calcination at 450°C for 2 hours, and re-immerse the calcined POM in 20umol / L Fe(NO 3 ) 3 After 12 hours in the aqueous solution, centrifugation, separation, and drying, a solid-state heteropolyacid composite catalyst modified by iron ions (abbreviated as POM-Fe) was obtained.
Embodiment 2
[0055] 1g phosphotungstic heteropoly acid (H 3 PW 12 o 40 , referred to as HPW) dissolved in 100mL deionized water, with KNO 3 For the ion source, control K + The molar ratio of HPW to HPW is 3:1, and the water-insoluble solid-phase heteropolyacid POM is obtained by chemical deposition. The above liquid is centrifuged at 12000r / min for 3min using a centrifuge, and the obtained solid is heated at 105°C Dry in oven. Take out the solid in the centrifuge tube and use an agate mortar to grind the solid to a fine powder state, and place it in a muffle furnace for calcination at 450°C for 2 hours, and re-immerse the calcined POM in 20umol / L Cu(NO 3 ) 2 After 12 hours in aqueous solution, centrifugation, separation, and drying, a solid heteropolyacid composite catalyst modified by iron ions (abbreviated as POM-Cu) was obtained.
Embodiment 3
[0057] 1g phosphotungstic heteropoly acid (H 3 PW 12 o 40 , referred to as HPW) dissolved in 100mL deionized water, with Cs 2 CO 3 For the ion source, the molar ratio between the ion source and HPW is controlled to be 2.5:1, and the water-insoluble solid-phase heteropolyacid POM is obtained by chemical deposition, and the above liquid is centrifuged at 12000r / min using a centrifuge After 3 minutes, the obtained solid was dried in an oven at 105°C. Take out the solid in the centrifuge tube and use an agate mortar to grind the solid to a fine powder state, and place it in a muffle furnace for calcination at 450°C for 2 hours, and re-immerse the calcined POM in 20umol / L Fe(NO 3 ) 3 In the aqueous solution for 12 hours, after centrifugation, separation and drying, different counter-ionic solid-state heteropolyacid composite catalysts (abbreviated as POM-Fe) decorated with iron ions were obtained. The SEM morphology of the prepared POM-Fe was characterized, and it was found t...
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