Preparation method of organic phosphinic acid functional group modified silicon-based adsorption material

A technology of phosphinic acid functional and adsorption materials, which is applied in chemical instruments and methods, inorganic chemistry, and other chemical processes, and can solve problems such as inability to absorb, affect the stability and cycle performance of extraction resins, and the loss of extractants. , to achieve the effects of fast adsorption kinetics, simple and easy preparation method, and stable chemical properties

Active Publication Date: 2021-10-22
UNIV OF SCI & TECH BEIJING
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The extractant is easy to lose during the use of this resin, which affects the stability and cycle performance of the extraction resin
For the impregnated resin prepared by the dry method, there are often more than one layer o

Method used

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  • Preparation method of organic phosphinic acid functional group modified silicon-based adsorption material
  • Preparation method of organic phosphinic acid functional group modified silicon-based adsorption material
  • Preparation method of organic phosphinic acid functional group modified silicon-based adsorption material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Silica gel activation: Reflux 20g of 60-80 mesh silica gel particles in 100mL of 6mol / L HCl for 4h, filter and wash repeatedly with deionized water, dry at 105°C for 10h, and store in a vacuum desiccator for later use.

[0026] (2) Grafting carbon-carbon double bonds on the surface of silica gel: dissolve 6.0 g of activated silica gel and 12 mL of allyltriethoxysilane in 50 mL of deionized water-ethanol mixed solvent (V 水 :V 乙醇 =1:1), reacted at 75°C for 24h. The silica gel particles were centrifuged, washed with ethanol for 3 times, and air-dried at room temperature to obtain silica gel particles grafted with carbon-carbon double bonds on the surface.

[0027] (3) Reaction of silica gel grafted with carbon-carbon double bonds and mono(2,3-dimethylbutyl)phosphinic acid: 6.0 g of silica gel particles grafted with carbon-carbon double bonds on the surface, 1.2 g glacial acetic acid, 3.0 g mono(2,3-dimethylbutyl) phosphinic acid, 0.25 g di-tert-butyl peroxide and 20 ...

Embodiment 2

[0029] (1) Fe 3 o 4 @SiO 2 Grafting carbon-carbon double bonds on the surface of magnetic microspheres: 2.0g Fe 3 o 4 @SiO 2 Magnetic microspheres and 12 mL of trimethoxy(7-octen-1-yl) silane were dissolved in 50 mL of toluene, and reacted at 90° C. for 8 h. Filtration, repeated washing with toluene, and vacuum drying at 50 ° C to obtain Fe with carbon-carbon double bonds grafted on the surface 3 o 4 @SiO 2 magnetic microspheres.

[0030] (2) Fe grafted with carbon-carbon double bonds 3 o 4 @SiO 2 Reaction of magnetic microspheres with mono(2,4,4-trimethylpentyl)phosphinic acid: Measure 2.0g of Fe with carbon-carbon double bonds grafted on the surface in a 250mL three-neck flask 3 o 4 @SiO 2 Magnetic microspheres, 10mL xylene, 0.5mL concentrated sulfuric acid, 6.0g mono(2,4,4-trimethylpentyl)phosphinic acid and 0.25g dibenzoyl peroxide were reacted under reflux for 24h (during Add 0.25 g of dibenzoyl peroxide). After cooling down to room temperature, filter, was...

Embodiment 3

[0032](1) SBA-15 surface grafted carbon-carbon double bond: 1.0g SBA-15 and 1mL methylvinyldiethoxysilane were dissolved in 20mL deionized water-1,4-dioxane mixed solvent ( V 水 :V 1,4-二氧六环 =2:1), reacted at 50°C for 16h. After filtration, repeated washing with 1,4-dioxane, and vacuum drying at 60°C, SBA-15 with carbon-carbon double bonds grafted on the surface was obtained.

[0033] (2) Reaction of SBA-15 grafted with carbon-carbon double bonds and mono(cyclohexyl) phosphinic acid: Measure 1.0 g of SBA-15 grafted with carbon-carbon double bonds on the surface, 0.3 mL of concentrated hydrochloric acid, 1.5g of mono(cyclohexyl)phosphinic acid, 0.10g of azobisisobutyronitrile, 0.10g of di-tert-butyl peroxide and 10mL of 1,4-dioxane, sealed, and reacted at 120°C for 36h (during which every 12h added 0.10g tert-butyl hydroperoxide). After cooling down to room temperature, after filtration and washing with 1,4-dioxane for 3 times, vacuum-dried at 60°C to obtain SBA-15 modified w...

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Abstract

The invention relates to a preparation method of an organic phosphinic acid functional group modified silicon-based adsorption material. An organic phosphinic acid functional group is grafted on the surface of the silicon-based material, wherein R4 is an aliphatic substituent with the carbon atom number of 4-12. The method comprises the following steps: firstly, enabling a silicon-based material to react with a silane cross-linking agent with unsaturated carbon-carbon double bonds, grafting the carbon-carbon double bonds on the surface of the silicon-based material, and then grafting an organic phosphinic acid functional group to the surface of the silicon-based material by utilizing free radical addition reaction of the carbon-carbon double bonds and monoalkyl phosphinic acid, wherein R1 is a methyl group, an ethyl group or a beta-methoxyethyl group; R2 is a methyl group, a methoxy group, an ethyoxyl group or a beta-methoxy ethyoxyl group; and R3 is (CH2)n, n= 0-10, or is gamma-methacryloyloxy propyl. The prepared adsorption material is good in mechanical property, stable in chemical property, fast in adsorption kinetics and good in selectivity; the preparation method is simple and easy to implement, large-scale production is easy to achieve, and the grafting rate of organic phosphinic acid functional groups is high. The method can be used in the fields of low-concentration rare earth enrichment, rare earth separation, nuclear-grade zirconium and hafnium separation and the like.

Description

technical field [0001] The invention belongs to the technical field of solid-phase extraction and separation, and in particular relates to the preparation of a functional group-modified silicon-based adsorption material and its application in low-concentration rare earth enrichment, rare earth separation, zirconium and hafnium separation, and the like. Background technique [0002] Organophosphorus / phosphonic acid extractants are widely used in solvent extraction and separation of similar elements such as rare earth, nickel cobalt, zirconium and hafnium. Phosphate), P507 (mono-2-ethylhexyl 2-ethylhexylphosphate) and Cyanex 272 (di(2,4,4-trimethylpentyl)phosphinic acid). As the alkoxy group is replaced by the alkyl group, its acidity decreases in the order of P204>P507>Cyanex 272. The stronger the acidity, the stronger the ability to extract rare earth ions, cobalt nickel, zirconium and hafnium (extraction performance: P204>P507>Cyanex 272), but the separation pe...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/28B01J20/30
CPCB01J20/06B01J20/103B01J20/22B01J20/28011
Inventor 王俊莲刘辉许文
Owner UNIV OF SCI & TECH BEIJING
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