Magnetic MOFs solid-phase extractant, and preparation method and application thereof

A solid-phase extraction agent, magnetic technology, applied in chemical instruments and methods, other chemical processes, water/sludge/sewage treatment, etc., to achieve the effect of large adsorption capacity, low cost and fast adsorption speed

Inactive Publication Date: 2015-01-28
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation of magnetic nano-Fe by in situ transformation 3 o 4 Composites with MOFs have not been reported

Method used

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  • Magnetic MOFs solid-phase extractant, and preparation method and application thereof
  • Magnetic MOFs solid-phase extractant, and preparation method and application thereof
  • Magnetic MOFs solid-phase extractant, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment l

[0048] Preparation of Magnetic Fe with a Particle Size of 10-20nm by Co-precipitation 3 o 4 Nanospheres: Dissolve 11.68g of ferric chloride and 4.30g of ferrous chloride in 200mL of high-purity water, stir and heat to 85°C under nitrogen protection. Then add 20 mL of 30% NH 3 ·H 2 O, the color of the solution rapidly changed from orange to black. After reacting for half an hour, stop the reaction, cool to room temperature, and the obtained nanoparticles are washed with high-purity water and 0.02mol L -1 washed with NaCl until neutral, and finally stored with high-purity water.

[0049] Preparation of Fe with Core-Shell Structure by Silica Coupling 3 o 4 SiO 2 : Remove half of the Fe 3 o 4 Put the nanoparticles into a mixed solvent containing 160mL ethanol and 40mL high-purity water, and add 5mL of 30% NH 3 ·H 2 O and 6 mL of tetraethoxysilane (TEOS), then mechanically stirred at room temperature for 12 h. After the reaction, wash with high-purity water and ethano...

Embodiment 2

[0055] The difference from Example 1 is: Synthesis of Bi-I modified magnetic MOFs solid-phase extraction agent: Weigh 200mg of Fe after drying at 150°C for 12h 3 o 4 SiO 2 HKUST-1 was placed in a 50mL round bottom flask, 20mL of anhydrous ether was added, and then 100mg of Bi-I was added to the suspension, and the reaction was carried out at room temperature for 24 hours under magnetic stirring. After the reaction was completed, it was washed with anhydrous ether (30 mL×5), and dried under vacuum at room temperature.

[0056] Adopt transmission electron microscope (TEM) to observe the core-shell type magnetic MOFs solid-phase extraction agent and its intermediate prepared in embodiment 2, and its TEM photograph is as follows Figure 2-5 shown. From figure 2 It can be seen that the prepared magnetic Fe 3 o 4 SiO 2 Nanoparticles have a spherical structure, and the darker part of the inner core is Fe 3 o 4 , the particle size is 10-20nm, and the lighter part of the midd...

Embodiment 3

[0071] The difference from Example 1 is: Synthesis of Bi-I modified magnetic MOFs solid-phase extraction agent: Weigh 200mg of Fe after drying at 150°C for 12h 3 o 4 SiO 2 HKUST-1 was placed in a 50mL round-bottomed flask, 20mL of anhydrous ether was added, and then 150mg of Bi-I was added to the suspension, and magnetically stirred at room temperature for 24 hours. After the reaction was completed, it was washed with anhydrous ether (30 mL×5), and dried under vacuum at room temperature.

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Abstract

A preparation method for a magnetic MOFs solid-phase extractant comprises the following steps: 1, employing a coprecipitation process to prepare a magnetic Fe3O4 nanosphere with the particle size of 10-20 nm; 2, employing Stober silica gel coupling process to prepare Fe3O4@SiO2 with a shell-core structure; 3, employing an in-situ precipitation process to prepare Fe3O4@SiO2@Cu(OH)2; 4, employing an in-situ conversion manner to synthesize Fe3O4@SiO2@HKUST-1; and 5, performing post-functionalization on Fe3O4@SiO2@HKUST-1 synthesized in the step 4 to synthesize the Bi-I modified magnetic MOFs solid-phase extractant. The advantages comprise that the provided method is simple, convenient, low in cost and friendly to environment. The prepared magnetic MOFs solid-phase extractant has the advantages of rapid adsorption speed, large adsorption capacity, high removal efficiency and the like, and efficient removal of low-concentration Hg<2+> can be realized.

Description

technical field [0001] The invention belongs to the field of wastewater treatment, and in particular relates to a magnetic MOFs solid-phase extraction agent and a preparation method and application thereof. Background technique [0002] Among many sample pretreatment techniques, compared with other separation and enrichment techniques (such as liquid phase extraction and precipitation), solid phase extraction has the advantages of simple operation, high enrichment factor, fast phase separation speed, and less organic solvent consumption. and other advantages, and has received widespread attention. At present, the development of new solid phase extraction materials with good performance is a research hotspot. [0003] Metal-organic frameworks (MOFs) are a class of porous organic-inorganic hybrid materials that use metal ions or metal clusters as ligand centers to form strong chemical bonds with oxygen- or nitrogen-containing organic ligands. Because of its super large speci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30C02F1/28
CPCB01J20/226B01J20/28009B01J20/3085B01J2220/46C02F1/285C02F2101/20
Inventor 胡斌黄理金何蔓陈贝贝
Owner WUHAN UNIV
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