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Metal ion imprinting solid phase extraction small column, preparation and application thereof

A technology of metal ion imprinting and solid-phase extraction cartridges, which is applied in the direction of ion exchange, ion exchange regeneration, ion exchange treatment devices, etc., can solve the problems of limited adsorption capacity of adsorbent and improvement of adsorption selectivity, and achieve low cost, The effect of rapid adsorption and desorption kinetics and mild reaction conditions

Inactive Publication Date: 2010-01-13
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] After searching the prior art, it is found that the synthesis of molecularly imprinted-sol-gel materials generally adopts the surface imprinting method (Dai, et al. Imprint-coating synthesis of selective functionalized ordered mesoporous sorbents for separation and sensors. USP, 6,251,280, June 26, 2001; Fang Guozhen, Tan Jin, Yan Xiuping. Synthesis method and adsorption material of sulfhydryl functionalized adsorption material imprinted with cadmium ions on the surface of silicon balls, CN, 1621146, 2005, 6). The disadvantage is that the adsorption capacity of the adsorbent is limited , the adsorption selectivity also needs to be improved

Method used

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Embodiment 1

[0028] (1) Preparation of lead ion imprinted adsorbent

[0029] Synthesis of lead ion imprinted organic-inorganic hybrid adsorbent: 0.397g Pb(NO 3 ) 2 Dissolve 0.73g of CTMAB in 18.7g of water, then add 0.491g of functional monomer 3-mercaptopropyltrimethoxysilane (MPS), stir for 1h to fully complex. At the same time, 2.083g TEOS was dissolved in 2mL methanol and stirred for 30min to form a sol. Then the sol was added to the aforementioned complex solution, and 3.8 mL of 1M NaOH was added under stirring. The mixed solution was stirred and reacted at room temperature for 48 h, then reacted at 90° C. for 24 h, and filtered to obtain a yellow solid. Put the solid product into a Soxhlet extractor and extract it with absolute ethanol for 72 hours to remove the surfactant, wash it with 0.5M dilute nitric acid to remove lead ions, wash it twice with deionized water until the pH is 4-5, and dry it in vacuum at 80°C for 12 hours After that, the lead ion-imprinted organic-inorganic ...

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Abstract

The invention relates to a metal ion imprinting solid phase extraction small column, which comprises the small column which takes a metal ion imprinting absorbent of 50-200mg as a filling matrix and has a polypropylene outer shell with the diameter of 6-10mm; and the preparation comprises the steps of dissolving metal ions, CTMAB and functional monomers in DDW, adding a mixed sol of alkoxy silane and methanol, further adding a catalyst, stirring, filtering and drying; then placing in a Soxhlet extractor, removing the CTMAB and the metal irons, washing and drying for preparation; and weighing the metal ion imprinting absorbent, filling in the solid phase extraction small column with the polypropylene outer shell and filling the column by homogenization under the vacuum-pumping state. The filler synthesis process of the solid-phase extraction small column is simple, the cost is low, the reaction conditions are mild, the prepared metal ion imprinting solid phase extraction small column can be applied in selective separation and enrichment of trace metal ions in environmental water samples, compared with the ordinary liquid-liquid extraction method, the operation is simple, rapid and highly efficient.

Description

technical field [0001] The invention belongs to the field of molecularly imprinted solid phase extraction column and its preparation and application, in particular to a metal ion imprinted solid phase extraction column and its preparation and application. Background technique [0002] Due to the low content of heavy metal elements in environmental and food samples, and the complex components and many interferences of environmental and food samples, they usually have to be separated and enriched before analysis and determination. The purpose of separation and enrichment is to concentrate trace metal ions, reduce the minimum detection concentration, remove interfering substances, and improve the accuracy and sensitivity of the determination. Liquid-liquid extraction is a widely used technology for pre-enrichment and separation of metal ions. Although this technology has a high enrichment rate and good reproducibility, the operation process is cumbersome, time-consuming, and us...

Claims

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Application Information

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IPC IPC(8): B01D15/08B01J20/281
Inventor 王丽敏周美华宫建龙
Owner DONGHUA UNIV
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