Preparation and application of high-capacity magnetic mesoporous silica gel solid phase extracting agent

A mesoporous silica gel and extraction agent technology, applied in other chemical processes, ion exchange, chemical instruments and methods, etc., can solve problems such as pollution, difficulty, and interference with the extraction of target pollutants, and achieve the goal of overcoming the large resistance and large Surface area, the effect of overcoming the separation difficulty of nano extractant and mother liquor

Inactive Publication Date: 2011-06-15
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

[0003] However, surface-modified magnetic nanoparticles also have some problems as solid-phase extraction agents. Due to the strong hydrophobicity of their surface, they are easily aggregated in aqueous solution, forming micron-sized aggregates, which greatly reduce their effective surface area and extraction capacity. It is greatly reduced; and the natural organic matter in the water sample is also easy to interact with the functional groups on the surface and attach to the surface to contaminate it, which seriously interferes with the extraction of target pollutants. Therefore, selective extraction from large volumes of complex water samples There are still some difficulties when targeting pollutants

Method used

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  • Preparation and application of high-capacity magnetic mesoporous silica gel solid phase extracting agent
  • Preparation and application of high-capacity magnetic mesoporous silica gel solid phase extracting agent
  • Preparation and application of high-capacity magnetic mesoporous silica gel solid phase extracting agent

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Effect test

Embodiment 1

[0041] Embodiment 1: The preparation method of the magnetic mesoporous silica gel material extraction agent of the present invention

[0042] C provided by the present invention 18 Modified Fe 3 o 4 / SiO 2 / SiO 2 The schematic diagram of the synthesis of the magnetic mesoporous silica material extractant is as follows: figure 1 As shown, its specific preparation method can be divided into the following four steps:

[0043] Firstly, nanometer ferric oxide was prepared, and the surface was ionized with sodium citrate. 5.2g FeCl 3 ·6H 2 O and 2.0 g FeCl 2 4H 2 O dissolved in 250mL pre-washed with N 2 Deoxygenated deionized water; under 80°C water bath and mechanical stirring, add 25mL 25% NH 3 .H 2 O solution, after the dropwise addition, continue to pass N 2 Insulated and stirred for 0.5 hour reaction; after the reaction, the prepared ferroferric oxide magnetic nanoparticles were separated by an external magnetic field. Wash the obtained ferroferric oxide magnetic ...

Embodiment 2

[0047] Example 2: Optimization of the modified reagent for preparing the magnetic mesoporous silica gel material extractant of the present invention

[0048] When preparing the magnetic mesoporous silica material extractant, select different doses of TEOS to Fe 3 o 4 Magnetic particles were coated with silica gel, different doses of C 18 Silylating reagents for Fe 3 o 4 / SiO 2 / SiO 2 The mesoporous shell of magnetic mesoporous silica particles is modified, and the mass percentage and adsorption capacity of each part of the obtained extractant are different. Therefore, in this implementation, the above-mentioned TEOS and C 18 The dosage of silylating agent is optimized.

[0049] 1. Optimization of the dosage of TEOS

[0050] Carry out Fe 3 o 4 When magnetic particles are coated with silica gel, TEOS and Fe 3 o 4 The ratio of magnetic particles has a great influence on the formation of magnetic silica particles. If the amount of TEOS is too small, the Fe embedded in...

Embodiment 3

[0055] Example 3 : Structural characterization of magnetic mesoporous silica gel material extractant of the present invention

[0056] This embodiment is the structural characterization of the third group of magnetic mesoporous silica gel material extractants optimized in Example 2, specifically as follows:

[0057] 1. TEM photo

[0058] Using JEOL.JEM-200CX transmission electron microscope (TEM) of JEOL, accelerating voltage 160kV, for Fe 3 o 4 / SiO 2 / SiO 2 Magnetic mesoporous silica particles and the C of the second group optimized in Scheme 2 18 Modified Fe 3 o 4 / SiO 2 / SiO 2 The particle size and structure of the magnetic mesoporous silica particles were analyzed. For the determination method and parameter setting, see Yonghui Deng, et al, J.Am.Chem.Soc., 2008, 130(1), 28-29.

[0059] Fe 3 o 4 / SiO 2 / SiO 2 The TEM pictures of the magnetic mesoporous silica particles are as follows: image 3 a, b shown. From image 3 It can be seen from a and b that the...

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Abstract

The invention provides a magnetic mesoporous silica gel material extracting agent used for enriching and/or separating trace organic pollutants in an environment water sample, and a preparation method thereof. A core of the extracting agent provided by the invention is a silicon gel microsphere (i.e. magnetic silicon gel microsphere) wrapped with a plurality of Fe3O4 magnetic nano particles, and a shell of the extracting agent is a mesoporous silicon gel shell layer with inner and outer surfaces modified by C18 silanization. The extracting agent integrates huge special surface area, excellent extracting capacity and ultrahigh extracting volume of a mesoporous material, magnetic separating capacity of a magnetic material, strong extracting capacity of C18 groups and special volume exclusion function of a vertical channel of the mesoporous material. In addition, the extracting agent provided by the invention has the advantages of high extracting efficiency, low preparation cost and simple preparation method, and is very suitable for preprocessing samples of the trace organic pollutants in a bulk-mass water sample.

Description

technical field [0001] The invention belongs to the field of chemical analysis testing instruments and equipment, and relates to a novel magnetic mesoporous silica gel material extractant for enriching and / or separating organic pollutants in environmental water samples. Background technique [0002] Solid-phase extraction is a relatively new environmental sample pretreatment method widely used at present. It has the advantages of short extraction time, high recovery rate, high enrichment factor and low consumption of organic reagents. At present, the more commonly used solid-phase extraction agent is silica gel bonded with organic groups, but due to the large particle size of silica gel, the extraction efficiency and extraction capacity are not high. In order to improve the extraction efficiency and extraction capacity, nanomaterials with smaller particle size and high specific surface area are used as solid-phase extraction agents for the analysis of trace pollutants in env...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/283B01J20/30B01D15/08
Inventor 蔡亚岐张小乐
Owner RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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