Mesoporous rare earth phosphate and preparation method thereof
A rare-earth phosphate and rare-earth nitrate technology, which is applied in the direction of phosphate and phosphorus oxyacids, can solve the problems of mesoporous pore size reduction, pore volume reduction, mesoporous rare earth compound synthesis, etc. High, large pore volume effect
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Embodiment 1
[0050] Disperse 1.0 g of mesoporous silica KIT-6 in 50 ml of n-hexane and stir thoroughly for 30 min, then gradually drop into the homogeneous solution of 3.5 g of yttrium nitrate and 0.3 g of concentrated phosphoric acid dissolved in 3 ml of concentrated nitric acid. Continue to stir until the solvent evaporates to dryness, and further place it in an oven at 100°C for 24h. Put this rare earth yttrium phosphate / KIT-6 compound in a muffle furnace, slowly raise the temperature to 600°C, keep it for 5 hours, stop heating, and take it out after natural cooling. Treat with 40ml of 4% hydrofluoric acid for 20min, further centrifuge, discard the supernatant, repeat 4 times to remove the silica mesoporous hard template, and finally continue washing with deionized water until the pH of the filtrate is neutral, filter ,drying. Thereby the mesoporous yttrium phosphate nanoporous material with three-dimensional cubic Ia3d structure is obtained.
[0051] Structural analysis of the obtain...
Embodiment 2
[0059] Disperse 1.0 g of mesoporous silica SBA-15 in 50 ml of n-heptane and stir thoroughly for 30 min, then gradually drop into the homogeneous solution of 3.5 g of yttrium nitrate and 0.3 g of concentrated phosphoric acid previously dissolved in 3 ml of concentrated nitric acid. Continue to stir until the solvent evaporates to dryness, and further place it in an oven at 100°C for 24h. Put the rare earth yttrium phosphate / SBA-15 compound in a muffle furnace, slowly raise the temperature to 750°C, keep it for 3 hours, stop heating, and take it out after natural cooling. Stir with 40ml of 4% hydrofluoric acid, control the stirring speed to 200-600r r / min, and process for 30min, further centrifuge, discard the supernatant, repeat 3 times to remove the silica mesoporous hard template, Finally, continue washing with deionized water until the pH of the filtrate is neutral, filter, and dry. Thus, a mesoporous yttrium phosphate nanomaterial with a two-dimensional hexagonal structure...
Embodiment 3
[0061] Disperse 1.0 g of mesoporous silica KIT-6 in 45 ml of n-heptane and stir well for 1 h, then gradually drop into a homogeneous solution of 3.5 g of lanthanum nitrate and 0.3 g of concentrated phosphoric acid dissolved in 3 ml of concentrated nitric acid. Continue to stir until the solvent evaporates to dryness, and further place it in an oven at 100°C for 24h. Put the rare earth lanthanum phosphate / KIT-6 compound in a muffle furnace, slowly raise the temperature to 850°C, keep it for 3 hours, stop heating, and take it out after natural cooling. Use 2mol.L at 60°C -1 Sodium hydroxide solution 30ml, stirring treatment, control the stirring speed to 200 ~ 600r r / min, the treatment time is 40min, further centrifugal separation, discard the supernatant, repeat 3 times to remove the silica mesoporous hard template, finally Continue washing with deionized water until the pH of the filtrate is neutral, filter and dry. Thus, a mesoporous lanthanum phosphate nanoporous material ...
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