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

Inactive Publication Date: 2009-11-11
SHANGHAI INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] It is worth noting that most of the reported rare earth mesoporous functional materials are prepared by grafting rare earth-containing organic small molecules on the surface of mesoporous silica molecular sieves, or by co-doping and post-synthesis. The internal pores of molecular sieves are often covered by these small organic molecules, resulting in reduced mesopore diameter and pore volume, which is not conducive to the entry of active molecules; at the sam

Method used

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  • Mesoporous rare earth phosphate and preparation method thereof
  • Mesoporous rare earth phosphate and preparation method thereof
  • Mesoporous rare earth phosphate and preparation method thereof

Examples

Experimental program
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Effect test

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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Abstract

The invention discloses a mesoporous rare earth phosphate and a preparation method thereof, belonging to the field of porous nano-material. The method, which takes mesoporous silicon dioxide with an ordered pore channel structure as a hard template agent, comprises the steps of adding homogeneous solution of soluble rare-earth salts/strong phosphoric acid/concentrated nitric acid in the silicon dioxide pore channel, removing the nitric acid solvent through direct volatilization, thus precipitating the phosphate in the pore channel; further leading the rare earth phosphate to be cured in the mesoporous pore channel through high-temperature roasting treatment, removing the silicon dioxide hard template agent, thus obtaining the mesoporous rare earth phosphate. The mesoporous rare earth phosphate has the characteristics of high degree of order, adjustable pore diameter and mesoporous structure, large specific surface area, pore diameter, pore volume and the like, with the specific surface area being 100-500m/g, the pore diameter being 3-8nm, and the pore volume being 0.15-1.5cm/g. The prepared mesoporous rare earth phosphate can be used for the embedding treatment of radioactive wastes.

Description

technical field [0001] The invention relates to a mesoporous rare earth phosphate and a preparation method thereof, belonging to the field of porous nanomaterials. Background technique [0002] Mesoporous materials (with a pore size of 2-50 nm) are widely used in the fields of catalysts, adsorption and separation because of their regular and orderly pores, large specific surface area and pore volume. Rare earth elements have very important applications in optical, electrical, and magnetic devices due to their unique 4f electron sublayer structure. If we combine the two to synthesize mesoporous rare earth nanomaterials such as mesoporous rare earth phosphate, then the The prepared mesoporous rare earth materials will have the excellent properties of mesoporous (such as shape selectivity, adsorption, etc.) Functional materials such as drug delivery, porous photoluminescent devices, magnetic adsorption and separation materials have opened up new development paths. [0003] Si...

Claims

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Application Information

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IPC IPC(8): C01B25/26
Inventor 沈绍典罗秋玲毛东森卢冠忠
Owner SHANGHAI INSTITUTE OF TECHNOLOGY
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