Preparation method of amino and 18-crown-6 modified magnetic solid-phase extraction agent based on rubidium extraction

A technology of hexadecanocrown and solid-phase extraction agent, which is applied in chemical instruments and methods, liquid solution solvent extraction, process efficiency improvement, etc., can solve the problems of low selectivity of liquid-liquid extraction technology, and achieve recovery rate High, enhanced hydrophilic performance effect

Inactive Publication Date: 2019-06-11
QINGHAI UNIVERSITY
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0004] The object of the present invention is to provide a method for preparing a magnetic solid-phase extraction agent modified based on rubidium-extracted amino groups and hexadecimal ether, which solves the problem that the selectivity of the existing liquid-liquid extraction technology is not strong

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  • Preparation method of amino and 18-crown-6 modified magnetic solid-phase extraction agent based on rubidium extraction
  • Preparation method of amino and 18-crown-6 modified magnetic solid-phase extraction agent based on rubidium extraction
  • Preparation method of amino and 18-crown-6 modified magnetic solid-phase extraction agent based on rubidium extraction

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Embodiment 1

[0027] A preparation method based on rubidium-extracted amino and octadecadecine-modified magnetic solid-phase extraction agent, comprising the following steps: (1) preparing magnetic Fe by solvothermal method 3 o 4 Nanoparticles: weigh 1.89g anhydrous FeCl 3 , put in a 250mL flask, add 70mL ethylene glycol, place it on a magnetic stirrer and stir at room temperature for about 30min until anhydrous FeCl 3 Dissolve, then add 4.8g of anhydrous sodium acetate into the solution, continue to stir until the solution is clear, transfer the reaction solution into a polytetrafluoroethylene reactor, place it in an oven, gradually raise the temperature in the oven to 200°C, and keep the temperature constant After reacting for 10 hours, after the reaction was completed, the tetrafluoroethylene reactor was cooled to room temperature, and the reaction product was removed, washed several times with pure water, ethanol, and ultrasonically washed several times, and then dried in a vacuum oven...

Embodiment 2

[0034] A preparation method based on rubidium-extracted amino and octadecadecine-modified magnetic solid-phase extractant, selectively adsorbing rare precious metal rubidium ions in aqueous solution, comprising the following steps: (1) preparing stock solution: preparing a concentration of 1.5 mol / L hydrochloric acid solution; prepare a pH=13 buffer solution with ammonia water and ammonium chloride, accurately pipette a 10 mg / mL rubidium standard sample, and use ammonia water ammonium chloride buffer solution with a pH of 13 to make it 0.5 mg / mL, 1.0mg / mL, 2.5mg / mL, 5mg / mL, 7.5mg / mL standard solution as the standard curve solution of atomic absorption method; The sodium ion concentration is respectively prepared to contain Na+20g / L and contain K+14g / L stock solution; (3) solid phase extractant activation step: accurately weigh 20 mg of magnetic solid phase extractant prepared, and use 5mL ammonia water-chlorine Ammonium chloride buffer solution (pH=13) was activated for 30min,...

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Abstract

The invention discloses a preparation method of an amino and 18-crown-6 modified magnetic solid-phase extraction agent based on rubidium extraction. According to the preparation method, ferroferric oxide is taken as a magnetic core, and aminopropyl triethoxysilane and 4-carboxybenzo-18-crown-6 are taken as reaction raw materials. According to the preparation method disclosed by the invention, selectivity of rubidium hydrate ions is enhanced by using a synergistic effect of 18-crown-6 and amino; the magnetic property of ferroferric oxide is utilized, so that the purpose of conveniently and rapidly separating rubidium ions from a complex matrix containing a large amount of alkali metal ions is achieved under an additional magnetic field; a prepared solid-phase extraction agent is used for separating and enriching rubidium in a water solution, so that pretreatment time of a sample is shortened; the enrichment factor of the rubidium ions can reach 100 times or above, selectivity of the extraction agent to rubidium is good, and interfering ions such as K<+>, Na<+> and the like can almost be completely removed, so that background interference is eliminated, the content of rubidium can bedetected only by a conventional atomic absorption method, and detection precision is greatly improved.

Description

technical field [0001] The invention relates to the technical field of a new generation of magnetic extractant, in particular to a preparation method of a magnetic solid-phase extractant based on rubidium-extracted amino and octadecadectadexyl ether modification. Background technique [0002] In analytical chemistry, sample pretreatment is a very important step, accounting for more than 60% of the entire analysis time. Rubidium is a rare and precious metal. Although my country has large reserves, the content in the sample matrix is ​​small. If you want to develop and utilize rubidium resources, First of all, it is necessary to solve the problem of accurate detection of rubidium. The current detection problem is that the aqueous solution containing rubidium often contains a large amount of K+, Na+, Ca 2+ , Mg 2+ Plasma, conventional atomic absorption spectrophotometry and inductively coupled plasma detection methods have large background interference and are difficult to dete...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D11/04B01J20/06B01J20/28B01J20/281C22B3/24C22B26/10B01J20/30
CPCY02P10/20
Inventor 付华宋维君张爱华孙春燕宋浩宇陈亚军刘强陶政远钱业程
Owner QINGHAI UNIVERSITY
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