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Preparation method and application of core-shell type Fe3O4/C magnetic nano solid extracting agent

A solid-phase extraction agent and magnetic nanotechnology, which is applied in the direction of inorganic material magnetism, other chemical processes, chemical instruments and methods, etc., can solve the problems of strong binding ability and difficult elution of target objects, achieve strong extraction ability and fast processing process , the effect of less dosage

Inactive Publication Date: 2010-03-10
RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Carbon materials also have certain disadvantages as solid-phase extraction materials, such as some target substances are too strong to be eluted [6]

Method used

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  • Preparation method and application of core-shell type Fe3O4/C magnetic nano solid extracting agent
  • Preparation method and application of core-shell type Fe3O4/C magnetic nano solid extracting agent
  • Preparation method and application of core-shell type Fe3O4/C magnetic nano solid extracting agent

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1: the preparation method of magnetic nanomaterial extraction agent of the present invention

[0024] The core-shell Fe provided by the present invention 3 o 4 The synthetic schematic diagram of / C magnetic nanomaterial extractant is as figure 1 As shown, its specific preparation method can be divided into the following two steps:

[0025] First, prepare nano-iron oxide. First, 5.2g FeCl 3 ·6H 2 O and 2.0 g FeCl 2 4H 2 O and 0.85mL of concentrated hydrochloric acid were dissolved in 25mL of N 2 In the deoxygenated aqueous solution; under vigorous mechanical stirring, add the above solution dropwise to 250mL 1.5mol / L NaOH aqueous solution, and continue to stir and react for 0.5 hours after the dropwise addition; Nanoparticles are separated.

[0026] Second, the preparation of core-shell Fe 3 o 4 / C magnetic nanomaterials. Take a quarter of the prepared Fe 3 o 4 Magnetic particles, washed three times with deionized water, then washed twice with et...

Embodiment 2

[0027] Embodiment 2: Structural characterization of magnetic nanomaterial extractant of the present invention

[0028] This embodiment is to carry out structural characterization to the magnetic nanomaterial extraction agent prepared in embodiment 1, specifically as follows:

[0029] 1. Particle size and morphology characterization

[0030] The prepared core-shell Fe was observed by transmission electron microscopy (TEM) 3 o 4 / C magnetic nanomaterial, its TEM picture is as figure 2 shown. From figure 2 It can be seen that the prepared Fe 3 o 4 / C nanoparticles are basically spherical, and the darker part of the inner layer is Fe 3 o 4The magnetic core has a particle size of about 10nm, and the lighter part of the outer layer is the coated carbon material. The coating layer is 2-5nm, and the entire nanoparticle presents an obvious core-shell structure.

[0031] 2. Elemental analysis

[0032] Determination of prepared Fe by X-ray energy spectrometer 3 o 4 and Fe ...

Embodiment 3

[0037] Embodiment 3: Adsorption performance test of magnetic nanomaterial extractant of the present invention

[0038] This embodiment selects alkylphenol pollutants bisphenol A (BPA), nonylphenol (4-OP) and octylphenol (4-NP), phthalate pollutants n-propyl phthalate (DPP), n-butyl phthalate (DBP), cyclohexyl phthalate (DCP) and n-octyl phthalate (DOP), polycyclic aromatic hydrocarbon pollutants phenanthrene (PhA), fluoranthene (FluA), pyrene (Pyr), benzene A[a]anthracene (BaA), benzo[b]fluoranthene (BbF), benzo[a]pyrene (BaP), benzo[g,h,i]perylene (BghiP), etc. are common pollutants Representative, the adsorption performance of the magnetic nanomaterial extractant prepared in Example 1 was tested.

[0039] The operation steps of the test are as follows: Figure 6 As shown, the specific experimental process is as follows: add an appropriate amount of standard solutions of various pollutants to the water sample, stir evenly, add the prepared magnetic nanomaterial solid phase ...

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Abstract

The invention relates to a Fe3O4 / C magnetic nano solid extracting agent coated with a novel carbon material, belonging to the field of chemical analysis and test instruments and equipment. The extracting agent simultaneously has large special surface area of nano material, short disperse path, magnetic separation capacity of magnetic material and strong adsorption capacity of carbon material, thereby being very suitable for pretreating large-scale and large-size water samples in batch. In addition, the solid extracting agent is simple to prepare, low in raw material cost, rapid and convenientto extract and friendly to the environment and only needs using a small amount of organic solvent in the whole process.

Description

technical field [0001] The invention belongs to the field of chemical analysis testing instruments and equipment, and relates to a novel carbon material-coated Fe 3 o 4 The magnetic nano solid phase extraction agent is used as a sample pretreatment material to enrich organic pollutants in large-volume environmental water samples. Background technique [0002] The background and development status of this technical field are roughly as follows: Solid phase extraction is a relatively new environmental sample pretreatment method widely used at present. Solid phase extraction has the advantages of short extraction time, high recovery rate, high enrichment factor and less consumption of organic reagents. Nanomaterials have a high specific surface area and excellent adsorption performance, but due to the small particle size of the nanoparticles, it is difficult to carry out the above-mentioned solid-phase extraction loading and passing through the column. Fe 3 o 4 Magnetic na...

Claims

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Application Information

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IPC IPC(8): B01J20/20B01J20/06H01F1/11
Inventor 蔡亚岐张升晓
Owner RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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