A kind of chlorine sphere modification method of modifying dialkylphosphinic acid functional group

A technology of dialkylphosphinic acid and monoalkylphosphinic acid, which is applied in the modification of chlorine balls, can solve the loss of extraction agent, affect the stability and cycle performance of extraction resin, and prevent To solve problems such as adsorption, achieve good stability, broad prospects for industrial application, and high mechanical strength

Active Publication Date: 2022-04-05
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 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 of extractant adsorbed on the surface of the base material. In actual application, only the extractant on the surface plays a role, and a large amount of extractant cannot contact with metal ions and cannot achieve adsorption.

Method used

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  • A kind of chlorine sphere modification method of modifying dialkylphosphinic acid functional group
  • A kind of chlorine sphere modification method of modifying dialkylphosphinic acid functional group
  • A kind of chlorine sphere modification method of modifying dialkylphosphinic acid functional group

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Amino-modified chlorine spheres: Weigh 10.2g of dry chlorine spheres, add 150mL of toluene to swell for 18h, add 12.9g of n-hexylamine and 10.6g of triethylamine, and react at 80°C for 18h. Cool down to room temperature, filter, wash with ethanol twice, wash with water until the filtrate is neutral, wash once more with ethanol, and dry in vacuum to obtain amino-modified chlorine spheres.

[0030] (2) Preparation of acid chlorides containing C=C double bonds: add 15.2 g of thionyl chloride to 18.1 g of undecylenic acid, react at 80° C. for 2 h, cool down to room temperature, and remove excess thionyl chloride by rotary evaporator , Add 40mL of anhydrous diethyl ether to obtain a diethyl ether solution of undecylenoyl chloride.

[0031] (3) Chlorine ball grafting C=C double bond: Take 12.0g of amino-modified chlorine balls, add 50mL of anhydrous ether and 8.2g of triethylamine, slowly add the ether solution of undecanoyl chloride through a constant pressure funnel at ...

Embodiment 2

[0034] (1) Amino-modified chlorine spheres: Weigh 20.8g dry chlorine spheres, add 200mL 1,4-dioxane to swell for 12h, add 18.2g diethylenetriamine and 17.6g anhydrous sodium carbonate, and reflux for 12h. Cool down to room temperature, filter, wash with ethanol twice, wash with water until the filtrate is neutral, wash once more with ethanol, and dry at room temperature to obtain amino-modified chlorine spheres.

[0035](2) Chlorine spheres grafting C=C double bonds: Take 25.0g of amino-modified chlorine spheres, add 50mL of tetrahydrofuran and 20.2g of saturated sodium bicarbonate solution, and slowly add 42.2g of undecanoyl chloride through a constant pressure funnel at room temperature. The tetrahydrofuran solution, after the dropwise addition, reacted for 6h. Filter, wash with deionized water until the filtrate is neutral, wash with ethanol, and dry at room temperature.

[0036] (3) Reaction of chlorine balls grafted with C=C double bonds and monohexylphosphinic acid: tak...

Embodiment 3

[0038] (1) Amino-modified chlorine spheres: Weigh 5.2g dry chlorine spheres, add 80mL N,N-dimethylformamide to swell for 10h, add 8.4g 1,6-hexamethylenediamine and 6.6g sodium hydroxide, and reflux Reaction 8h. Cool down to room temperature, filter, wash with ethanol three times, wash with water until the filtrate is neutral, wash with ethanol once more, and dry at room temperature to obtain amino-modified chlorine spheres.

[0039] (2) Preparation of acid chlorides containing C=C double bonds: add 9.2 g of thionyl chloride to 8.1 g of 5-hexenoic acid, react at 80° C. for 2.5 h, drop to room temperature, and remove excess chloride by rotary evaporator sulfoxide, and 20 mL of dry 1,4-dioxane was added to obtain a 1,4-dioxane solution of 5-hexenoyl chloride.

[0040] (3) chlorine ball grafting C=C double bond: get 5.6g amino-modified chlorine balls, add 20mL cyclohexane and 6.2g potassium carbonate solution, slowly add 5-hexenoyl chloride through a constant pressure funnel at r...

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Abstract

The invention discloses a chlorine sphere modification method for modifying dialkylphosphinic acid functional groups, which belongs to the technical field of solid phase extraction and separation. It is characterized in that the chlorine atom on the chlorine ball reacts with the compound containing the primary amine functional group to obtain the amino-modified chlorine ball; then the carbon-carbon double bond is grafted to the chlorine ball by using the amide group generated by the reaction of the amino group and the acid chloride Surface; and then use the free radical addition reaction of carbon-carbon double bond and mono-alkyl phosphinic acid to obtain modified chlorine spheres with functional groups of di-alkyl phosphinic acid. The modification method of chlorine spheres for modifying dialkylphosphinic acid functional groups disclosed by the present invention is simple and easy for industrialization, and the obtained modified chlorine spheres grafted with dialkylphosphinic acid functional groups have good selectivity, high chemical stability, and saturated Large adsorption capacity, no loss of extractant, can be widely used in low-concentration rare earth enrichment, rare earth deep separation, preparation of nuclear-grade zirconium and hafnium, metal ion removal and other fields.

Description

technical field [0001] The invention belongs to the technical field of solid-phase extraction and separation, and in particular relates to the modification of a chlorine sphere and its application in the enrichment of low-concentration rare earths, separation of rare earths, separation of zirconium and hafnium, and removal of impurities of metal ions. 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 per...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F8/40C08F8/32C08F8/10C08F212/08B01J20/26B01J20/28B01J20/30B01D15/20
CPCC08F8/40C08F8/32C08F8/10B01J20/265B01J20/28021B01J20/28011B01D15/206C08F212/08
Inventor 王俊莲赵惠欣陈孝婷
Owner UNIV OF SCI & TECH BEIJING
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