Preparation method of magnetic metal organic framework material and application of magnetic metal organic framework material

A technology of organic framework and magnetic metal, which is applied in the field of material chemistry and sample pretreatment, can solve the problems of cumbersome preparation steps and long time, and achieve the effect of simple preparation method, low detection limit and good dispersibility

Inactive Publication Date: 2015-04-01
HANGZHOU DIANZI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above preparation methods all need Fe 3 o 4 Particles are functionalized, and then react...

Method used

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  • Preparation method of magnetic metal organic framework material and application of magnetic metal organic framework material
  • Preparation method of magnetic metal organic framework material and application of magnetic metal organic framework material
  • Preparation method of magnetic metal organic framework material and application of magnetic metal organic framework material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1: Fe 3 o 4 Preparation of / MIL-101(Fe):

[0030] Step (1). Preparation of Fe 3 o 4 Nanoparticles:

[0031] FeCl 3 ·6H 2 O (2.35g) and ferrous salt FeCl 2 4H 2 O (0.86 g) was dissolved in 80 mL deionized water under N 2 Under protected conditions, heat in a water bath at 80°C, then slowly drop 30 mL of 5% ammonia water into the above mixture to adjust the pH value to greater than 9, and stir for 1 h. The product is washed with deionized water until the pH of the filtrate is neutral to obtain the nanomagnetic material Fe 3 o 4 ;

[0032] Step (2). Preparation of Fe 3 o 4 / MIL-101(Fe) composite material

[0033] Get the nano-magnetic material Fe of 4 mmol step (1) gained 3 o 4 Sonicate for 10 min and disperse into 100 mL deionized water to obtain uniform Fe 3 o 4 Nanoparticle dispersion; take 5 mL dispersion (containing 0.2 mmol nanomagnetic material Fe 3 o 4 ) for centrifugation for 5 min, discard the supernatant, and add the precipitate t...

Embodiment 2

[0034] Example 2: Fe 3 o 4 The preparation of nanoparticles is the same as described in Example 1 step (1); the preparation of MIL-101 (Fe) material is the same as described in Example 1 step (2), except that Fe is not added 3 o 4 .

[0035] Figure 1~4 Be the Fe that obtains according to embodiment 1~2 of the present invention 3 o 4 / MIL-101(Fe) and MIL-101(Fe), Fe 3 o 4 Electron micrographs, infrared spectra, XRD and hysteresis loop spectra.

[0036] figure 1 a is MIL-101 (Fe) crystal material; figure 1 b is Fe prepared by co-precipitation method 3 o 4 Particles, whose size distribution is uniform, are about 20 nm; by figure 1 c shows that the Fe prepared by this method 3 o 4 / MIL-101(Fe) composite material is Fe 3 o 4 Attached to the surface of MIL-101(Fe) crystals, did not change the morphology of MIL-101(Fe); by figure 1 d, it can be seen that the size of the composite material is uniform.

[0037] Depend on figure 2 It can be seen that Fe 3 o 4 ...

Embodiment 3

[0040] Example 3: Fe 3 o 4 / Characterization of extraction performance of MIL-101(Fe)

[0041] (1). Fe 3 o 4 / MIL-101(Fe) and Fe 3 o 4 Comparison of adsorption performance

[0042] Disperse 20 mg of magnetic material in a sample solution (3 mL) containing six kinds of organophosphorus, including Dichlorvos, Methamidophos, Dimethoate, Parathion-methyl, Malathion (malathion) and parathion (parathion), organic phosphorus concentrations are 20 ng / mL. Adjust the ionic strength to 5% w / v with NaCl, shake for 40 min, so that the organic phosphorus is adsorbed on the surface of the magnetic material; after the adsorption is completed, the magnetic material combined with the organic phosphorus is separated from the sample solution under the action of an external magnetic field; finally , add 200 μL of acetone for ultrasonic desorption for 10 min, desorb twice, combine the desorbed solution, dry it, reconstitute it with 150 μL of ethyl acetate, and measure it with a gas c...

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Abstract

The invention discloses a preparation method of a magnetic metal organic framework material and an application of the magnetic metal organic framework material. The preparation method comprises the steps of synthesizing a nano magnetic material Fe3O4 by adopting a coprecipitation method, adding the nano magnetic material Fe3O4, FeCI3.6H2O and terephthalic acid into DMF, carrying out ultrasonic mixing, and synthesizing Fe3O4/MIL-101(Fe) by adopting a hydrothermal method; separating a product by utilizing a magnetic field, washing with hot ethyl alcohol, and drying overnight so as to obtain the Fe3O4/MIL-101(Fe). The Fe3O4/MIL-101(Fe) obtained by the method is applied to separating and enriching organophosphorus in urine. The magnetic metal organic framework material is uniform in particle size, is relatively strong in magnetism, and is good in dispersibility; MIL-101(Fe) formed by the coordination of oxygen bearing carboxylate ligand and a metal ion F3<3+> is adopted as an adsorption separation medium and is combined with a magnetic solid phase extraction technique for being combined with chromatography so as to determine trace organophosphorus residues in urea, and the magnetic metal organic framework material is relatively high in flexibility.

Description

technical field [0001] The invention belongs to the field of material chemistry and sample pretreatment, and relates to a magnetic metal organic framework material Fe 3 o 4 / MIL-101(Fe) preparation method and its application, specifically preparing the material by hydrothermal synthesis, combined with magnetic solid-phase extraction technology, used to enrich the organic phosphorus residue in the sample solution, and gas chromatographic determination. Background technique [0002] In the field of analytical chemistry, the analysis of trace and ultra-trace substances in biological samples has become the focus of attention. Due to the characteristics of low concentration, complex components, and serious interference of biological samples, it needs to be purified, concentrated and enriched by effective sample pretreatment technology before analysis and determination. Therefore, the development of rapid, highly selective, and environmentally friendly sample pretreatment techni...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/28B01J20/281B01J20/30G01N30/88
CPCB01J20/28009B01J20/28016B01J20/28054B01J20/282C02F1/281G01N30/88
Inventor 张素玲张春晓王海栋
Owner HANGZHOU DIANZI UNIV
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