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Preparation method of double-shell phosphonyl modified silica magnetic microsphere for extracting uranium from brine

A technology of silica and magnetic microspheres, which is applied in the preparation of microspheres, chemical instruments and methods, microcapsule preparations, etc., can solve the problems of easy dissolution of magnetic substances, and achieve easy magnetic separation, high adsorption capacity, and fast adsorption rate Effect

Inactive Publication Date: 2017-05-10
EAST CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problem that magnetic substances are easy to dissolve when using silica magnetic microspheres to extract uranium from brine, and to improve the adsorption capacity and adsorption selectivity of silica magnetic microspheres for uranium, the invention provides a double-shell phosphono-modified The preparation method of silica magnetic microspheres, using double-shell phosphono-modified silica magnetic microspheres to extract uranium from brine has the advantages of fast adsorption rate, high adsorption capacity, and good adsorption selectivity, and the magnetic microspheres have good Excellent chemical stability, mechanical strength and uranium adsorption performance, easy to magnetic separation; good adsorption selectivity and high adsorption capacity for U(VI) in brine

Method used

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  • Preparation method of double-shell phosphonyl modified silica magnetic microsphere for extracting uranium from brine

Examples

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Effect test

Embodiment 1

[0024] (1) Preparation of monolayer-coated silica magnetic microspheres (Fe 3 o 4 @SiO 2 )

[0025] 0.1g nano Fe 3 o 4 Add it to 50mL of absolute ethanol, 25mL of deionized water, and 1.5mL of ammonia-water mixture, and disperse evenly by ultrasonic. Then add 0.1g tetraethyl orthosilicate, microwave heating and stirring reaction at 80°C for 5-10h, after centrifugation to obtain solid phase product, the solid phase product is fully washed with deionized water, dried at 60°C to obtain silica magnetic Microspheres.

[0026] (2) Preparation of double-shell phosphono-modified magnetic silica microspheres

[0027] In 60mL absolute ethanol, 80mL deionized water, 1.5mL ammonia water and 1.5mL porogenic template agent (polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, P123) mixed solution Add 0.2g Fe 3 o 4 @SiO 2 , ultrasonically dispersed for 30 minutes, and then added 0.2 g of tetraethyl orthosilicate (TEOS) and 0.01 g of phosphono functionalizat...

Embodiment 2

[0030] Preparation of double-shell phosphono-modified magnetic silica microspheres

[0031]In 60mL absolute ethanol, 80mL deionized water, 1.5mL ammonia water and 1.5mL porogenic template agent (polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, P123) mixed solution Add 0.2g Fe 3 o 4 @SiO 2 , Ultrasonic dispersion for 30min. Then add 0.2 g of tetraethyl orthosilicate (TEOS) and 0.02 g of phosphono functionalization reagent (diethylphosphonotriethoxysilane, DPTS) according to 10% of the mass ratio of DPTS / TEOS, and place the resulting mixture in the reaction kettle , stirred at 40°C for about 1h, then heated to 80°C for microwave hydrothermal treatment for 6h, magnetically separated to obtain a solid product and washed thoroughly, the washed product was redispersed in 100mL acidic ethanol solution, and refluxed at 60°C for 12h to remove Templating agent (P123). The obtained product is magnetically separated, fully washed with deionized water and ...

Embodiment 3

[0035] Preparation of double-shell phosphono-modified magnetic silica microspheres

[0036] In 60mL absolute ethanol, 80mL deionized water, 1.5mL ammonia water and 1.5mL porogenic template agent (polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, P123) mixed solution Add 0.2g Fe 3 o 4 @SiO 2 , Ultrasonic dispersion for 30min. Then add 0.2 g of tetraethyl orthosilicate (TEOS) and 0.03 g of a phosphono functionalization reagent (diethylphosphonotriethoxysilane, DPTS) according to 15% of the mass ratio of DPTS / TEOS, and place the resulting mixture in a reaction kettle , stirred at 40° C. for about 1 h, then heated to 80° C. for microwave hydrothermal treatment for 6 h, magnetically separated to obtain a solid product, and then fully washed. The washed product was redispersed in 100 mL of acidic ethanol solution, and refluxed at 60° C. for 12 h to remove the templating agent (P123). The obtained product is magnetically separated, fully washed with d...

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Abstract

The invention discloses a preparation method of a double-shell phosphonyl modified silica magnetic microsphere for extracting uranium from brine. An inner shell of the double-shell phosphonyl modified silica magnetic microsphere is a compact silica layer and is used for coating a magnetic substance Fe3O4 in a core, so that dissolution of Fe3O4 during a using process is avoided; an outer shell of the double-shell phosphonyl modified silica magnetic microsphere is a phosphonyl modified silica layer having a developed and ordered mesoporous structure, so that the uranium can conveniently enter a hole for adsorption. The preparation method of the double-shell phosphonyl modified silica magnetic microsphere comprises the following steps: firstly coating the compact silica layer on the surfaces of magnetic Fe3O4 nanoparticles, then further coating a porous phosphonyl functionalized silica layer, and finally removing a template agent (P123) through reflux extraction, thus obtaining the double-shell phosphonyl modified silica magnetic microsphere. The double-shell phosphonyl modified silica magnetic microsphere disclosed by the invention can be used as an adsorbent, and can be used for realizing high-efficiency uranium extraction from the brine through adsorption by taking salt making brine in sea salt production as a raw material.

Description

technical field [0001] The invention relates to a method for preparing double-shell phosphono-modified silicon dioxide magnetic microspheres for extracting uranium from brine, and belongs to the field of inorganic functional materials. Background technique [0002] Sea salt production brine can be considered as concentrated seawater, its uranium concentration is much higher than that of seawater, up to hundreds of μg / L; and some salts (such as NaCl) have been precipitated during the evaporation and enrichment process, which is conducive to the adsorption of uranium. Therefore, These brines are also important uranium resources, which need to be further developed and utilized. The brine after uranium extraction can be comprehensively utilized by the existing salt chemical technology. However, due to the high salinity of brine, uranyl ions have complex forms and a large number of interfering ions (such as Na + 、K + , Mg 2+ Wait). Conventional adsorbents (such as ion exchang...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/10B01J20/28B01J20/30B01J13/02C22B7/00C22B60/02
CPCB01J13/02B01J20/103B01J20/28009B01J20/3085C22B7/00C22B60/0265Y02P10/20
Inventor 周利民
Owner EAST CHINA UNIV OF TECH
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