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Magnetic nano-material extractant and preparation method thereof

A magnetic nanometer and magnetic nanoparticle technology, which is applied in the fields of microsphere preparation, inorganic material magnetism, chemical instruments and methods, etc., can solve the problem of difficulty in extracting target pollutants, difficulty in solid-phase extraction through the column, and the particle size of nanoparticles is too small. and other problems, to achieve the effect of fast extraction speed, strong surface adsorption, and short diffusion path.

Inactive Publication Date: 2011-08-31
RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the large size of silica gel particles, the extraction efficiency is not high, and nanomaterials have high specific surface area and excellent adsorption performance, but because the particle size of nanoparticles is too small, it is difficult to pass through the column during solid phase extraction; the preparation has Superparamagnetic organic group-modified nanoparticles can solve this problem, so in recent years C 18 Modified magnetic nano-Fe 3 o 4 (Fe 3 o 4 -C 18 ) is used for solid-phase extraction of organic pollutants, please refer to I.J.Bruce, T.Sen.Langmuir 21 (2005) 7029-7035 for related literature; H.H.Hsiao, H.Y.Hsieh, C.C.Chou, S.Y.Lin, A.H.J.Wang, K.H.Khoo. Journal of Proteome Research 6(2007) 1313-1324; and Y.Liu, H.F.Li, J.M.Lin.Talanta.77(2009) 1037-1042
[0003] However, Fe 3 o 4 -C 18 There are also some problems as a solid phase extraction agent, due to Fe 3 o 4 -C 18 The surface has strong hydrophobicity, which makes it difficult to disperse stably in aqueous solution, and the protein in the water sample is also easy to react with long-chain alkyl groups and denature, thus attaching to its surface and contaminating it, so it is difficult to achieve The purpose of extracting target pollutants from large volumes of complex water samples

Method used

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  • Magnetic nano-material extractant and preparation method thereof
  • Magnetic nano-material extractant and preparation method thereof
  • Magnetic nano-material extractant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Example 1 : The preparation method of magnetic nano material extraction agent of the present invention

[0039] Chitosan polymer-coated Fe provided by the present invention 3 o 4 -C 18 The schematic diagram of the synthesis of magnetic nanomaterial extractant is as follows: figure 1 As shown, its specific preparation method can be divided into the following three steps:

[0040] First, prepare nano-iron oxide. 2.0g FeCl 3 ·6H 2 O and 5.2 g FeCl 2 4H 2 O and 0.85mL of concentrated hydrochloric acid were dissolved in 25mL of N 2 Deoxidized deionized water; under 80°C water bath and mechanical stirring, add the above solution dropwise to N 2 In the protected 250mL 1.5 (mol / L) NaOH aqueous solution, continue to pass N 2 Insulate and stir for 0.5 hours to react; after the reaction, use an external magnetic field to separate the prepared iron oxide magnetic nanoparticles.

[0041] Second, the preparation of Fe 3 o 4 -C 18 Magnetic Nanomaterials. will get Fe ...

Embodiment 2

[0043] Example 2 : The modification reagent optimization of preparation magnetic nano material extraction agent of the present invention

[0044] When preparing the magnetic nano-extractant, different doses of C 18 Modified by silylating reagent, coated with chitosan and sodium tripolyphosphate solution with different concentrations and proportions, the mass percentage and adsorption capacity of each part of the obtained extractant are different. Therefore, in this implementation, the above-mentioned C 18 The dosage of silylating agent and the concentration ratio of chitosan and sodium tripolyphosphate were optimized.

[0045] 1.C 18 Optimization of the dosage of silylating reagent

[0046] to Fe 3 o 4 Granules for C 18 During silanization modification, since the active hydroxyl groups on the particle surface are limited, the combination of C 18 The amount of silane groups is also limited. If the dosage is too small, the modified magnetic nanoparticles have fewer adso...

Embodiment 3

[0056] Example 3 : Structural characterization of magnetic nanomaterial extractant of the present invention

[0057] This embodiment is the structural characterization of the fourth group of magnetic nanomaterial extractants optimized in Example 2, specifically as follows:

[0058] 1. Specific surface area and pore volume

[0059]The specific surface area and pore volume of the magnetic nanoparticles were measured by a Gemini 2375V4.01 nitrogen adsorption BET specific surface area analyzer (Norcross, USA). For the measurement method and parameter settings, see IanJ.Bruce, et al, Journal of Magnetism and Magnetic Materials 284 (2004) 145-160. The result of measuring magnetic nanomaterial extractant of the present invention is: specific surface area is 90.3124 (m 2 / g); the pore volume is 0.361007(cm 3 / g).

[0060] 2. EDX spectrum

[0061] Adopt DX-4 type X-ray energy spectrometer (Philips company) to measure the EDX energy spectrum figure of magnetic nanoparticle, the r...

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Abstract

The present invention provides a magnetic nano-material extractant used for enriching and / or separating organic pollutant in an environmental water sample, and a preparation method thereof. The extractant is characterized in that the core of the extractant is magnetic nano-grain decorated by a hydrophobic group; the external layer thereof is wrapped by a hydrophilic polymer; and the following extractant is preferably selected: the Fe3O4 magnetic nano-material extractant decorated by C18 silanes and wrapped by a chitosan polymer. The extractant has the advantages of large specific surface area of the nano material, magnetic separation capability of the magnetic material, strong extraction capability of the C18 and excellent hydrophilicity and volume excluding function of the chitosan polymer. Furthermore, the method for preparing the extractant is simple, has low cost and is extremely suitable for the batch pretreatment of large-scale large-volume water samples.

Description

technical field [0001] The invention belongs to the field of chemical analysis testing instruments and equipment, and relates to a novel magnetic nanomaterial extractant for enriching and / or separating organic pollutants in environmental water samples. Background technique [0002] Solid phase extraction is a relatively new type of pretreatment method for environmental samples that is widely used at present. It has the advantages of short extraction time, high recovery rate, high enrichment factor and low consumption of organic reagents. Currently, the most commonly used solid phase extraction agent is bonded organic Group of silica gel. Due to the large size of silica gel particles, the extraction efficiency is not high, and nanomaterials have high specific surface area and excellent adsorption performance, but because the particle size of nanoparticles is too small, it is difficult to pass through the column during solid phase extraction; the preparation has Superparamagn...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286B01J20/32B01J13/02H01F1/11
Inventor 蔡亚岐张小乐
Owner RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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