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Method for grafting dialkyl phosphinic acid functional group on surface of silicon-based material

An alkyl phosphinic acid functional, monoalkyl phosphinic acid technology, applied in chemical instruments and methods, alkali metal oxides/hydroxides, inorganic chemistry, etc., can solve the problem of poor stability and cycle performance of leaching resins , the extraction agent cannot be effectively used, the extraction agent is lost, etc., to achieve the effect of good recycling performance, fast adsorption speed, and fast adsorption kinetics

Active Publication Date: 2021-10-26
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The extractant is easy to lose during the use of this kind of resin, the stability and cycle performance of the extraction resin are poor, and many extractants adsorbed inside the impregnated resin cannot be effectively utilized

Method used

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  • Method for grafting dialkyl phosphinic acid functional group on surface of silicon-based material
  • Method for grafting dialkyl phosphinic acid functional group on surface of silicon-based material
  • Method for grafting dialkyl phosphinic acid functional group on surface of silicon-based material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Silica gel activation: Reflux 100g of 60-80mesh silica gel particles in 180mL 6mol / L HCl for 6h, cool down to room temperature, filter, wash repeatedly with deionized water, and dry at 120°C for 6h to obtain activated silica gel particles.

[0031] (2) Grafting amino groups on the surface of silica gel: 20 mL of 3-aminopropyltriethoxysilane and 200 mL of toluene were added to 20 g of activated silica gel, and the mixture was refluxed for 6 h. After cooling down to room temperature, the supernatant was removed by centrifugation, and the silica gel particles were washed twice with ethanol and twice with acetone, and air-dried at room temperature to obtain silica gel particles grafted with amino groups on the surface.

[0032] (3) Preparation of acid chlorides containing C=C double bonds: add 7.48g thionyl chloride to 10.14g undecylenic acid, react at 60°C for 4h, then react at 80°C for half an hour, drop to room temperature, pass The excess thionyl chloride was remove...

Embodiment 2

[0036] (1) Fe 3 o 4 @SiO 2 Amino groups grafted on the surface of magnetic microspheres: to 20g Fe 3 o 4 @SiO 210 mL of N-cyclohexyl-γ-aminopropylmethyldimethoxysilane and 180 mL of 1,4-dioxane were added to the magnetic microspheres, and the mixture was refluxed for 10 h. After cooling down to room temperature, the supernatant was removed by centrifugation, washed twice with ethanol and twice with acetone, and air-dried at room temperature to obtain Fe with amino groups grafted on the surface. 3 o 4 @SiO 2 magnetic microspheres.

[0037] (2) Fe 3 o 4 @SiO 2 C=C double bond modification on the surface of magnetic microspheres: take 18g of amino-modified Fe 3 o 4 @SiO 2 Add 50mL tetrahydrofuran and 8.6g anhydrous sodium carbonate to the magnetic microspheres, slowly add the tetrahydrofuran solution of undecanoyl chloride through a constant pressure funnel at room temperature, and react for 3 hours after the dropwise addition. Centrifuge, remove supernatant, Fe 3 ...

Embodiment 3

[0040] (1) Amino groups grafted on the surface of SBA-15: Add 15mL N-(β-aminoethyl)-γ-aminopropylmethyl-dimethoxysilane and 150mL 1,4-dioxosilane to 12g SBA-15 Six rings, reflux reaction for 24h. After cooling down to room temperature, the supernatant was removed by centrifugation, washed three times with ethanol and three times with acetone, and air-dried at room temperature to obtain SBA-15 with amino groups grafted on the surface.

[0041] (2) Preparation of acid chlorides containing C=C double bonds: add 4.8g thionyl chloride to 4.2g 5-hexenoic acid, react for 2 hours at 80°C, drop to room temperature, remove excess chlorine by rotary evaporator Sulfoxide was added, and 10 mL of 1,4-dioxane was added to obtain an organic solution of 5-hexenoyl chloride.

[0042] (3) C=C double bond modification on the surface of SBA-15: Take 12g amino-modified SBA-15, add 50mL 1,4-dioxane and 5.5g sodium hydroxide, and slowly add it through a constant pressure funnel at room temperature ...

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Abstract

The invention discloses a method for grafting a dialkyl phosphinic acid functional group on the surface of a silicon-based material, which belongs to the technical field of solid-phase extraction separation. A dialkyl phosphinic acid functional group is grafted on the surface of a silicon-based material through an amide group, and R7 is an aliphatic substituent with the carbon atom number of 4-12. The preparation method comprises the following steps of firstly, enabling a silicon-based material to react with a silane cross-linking agent with amino groups, and grafting amino groups on the surface of the silicon-based material, grafting a carbon-carbon double bond to the surface of the silicon-based material by utilizing an amide group generated by reaction of amino and acyl chloride, and grafting a dialkyl phosphinic acid functional group on the surface of the silicon-based material by using a free radical addition reaction of a carbon-carbon double bond and monoalkyl phosphinic acid. The preparation process is simple, the cost is low, and the prepared silicon-based adsorption material with the dialkyl phosphinic acid functional group grafted on the surface is good in mechanical property, stable in chemical property, fast in adsorption kinetics, large in saturation adsorption capacity and good in selectivity and can be used for low-concentration rare earth enrichment, rare earth separation and nuclear-grade zirconium and hafnium separation.

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] Extraction chromatography has the dual advantages of high selectivity of solvent extraction and simple equipment and high efficiency of ion exchange. It is an effective method for separating and producing a single high-purity rare earth product, which is called the second-generation extraction. system. Compared with the solvent extraction method, the reagent input, consumption and loss of the extraction agent in the extraction chromatography method are greatly reduced. There is no emulsification problem caused by the extraction process, no third phase is formed, and the loss of organic solvents is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30
CPCB01J20/103B01J20/22B01J20/06B01J20/186B01J20/28009
Inventor 王俊莲刘辉徐国栋刘璐
Owner UNIV OF SCI & TECH BEIJING
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