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Magnetic MOFs solid phase extraction adsorbent as well as preparation method and application thereof

A solid phase extraction agent and magnetic technology, applied in chemical instruments and methods, adsorption water/sewage treatment, other chemical processes, etc., can solve problems such as not particularly stable, up to 45 minutes, long reaction time, etc., to achieve removal efficiency High efficiency, low cost, and large adsorption capacity

Inactive Publication Date: 2015-12-16
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, MFCs are mainly prepared by solvothermal and layer-by-layer self-assembly methods, which have some defects: solvothermal methods often require higher reaction temperature, longer reaction time and the use of organic solvents such as N,N-di Methylformamide (DMF); although the layer-by-layer self-assembly method is relatively simple, the required reaction time is longer (generally 25 times, each time up to 45 minutes)
On the other hand, these MFCs materials are mainly based on HKUST-1 as the modified material, and HKUST-1 is not particularly stable in contact with water, and the high concentration of Cu 2+ It has certain toxicity to organisms and is easy to cause secondary pollution, so there are certain limitations in application

Method used

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  • Magnetic MOFs solid phase extraction adsorbent as well as preparation method and application thereof
  • Magnetic MOFs solid phase extraction adsorbent as well as preparation method and application thereof
  • Magnetic MOFs solid phase extraction adsorbent as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment l

[0038] 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 then wash the obtained nanoparticles with high-purity water and 0.02molL -1 washed with NaCl until neutral, and finally stored with high-purity water.

[0039] 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 ethanol to...

Embodiment 2

[0043] The difference with Example 1 is: synthetic MFC-N-50: 1.0gFe 3 o 4 SiO 2 Add to 15mL high-purity water, add 5.0g AlCl after ultrasonic dispersion 3 ·6H 2 O, and then ultrasonically mixed for 20 minutes to obtain solution I; 1.68g NaOH, 1.66g terephthalic acid and 1.81g 2-aminoterephthalic acid were mixed with water and ultrasonically dispersed to obtain solution II. Under the condition of stirring at room temperature with a rotation speed of 600 rpm, add solution I dropwise to solution II to form a suspension and continue stirring for 15 hours; then wash with high-purity water and dry at room temperature; then activate in DMF solution at 150°C for 5 hours , and finally washed with ethanol to obtain MFC-N-50 solid-phase adsorbent.

Embodiment 3

[0045] The difference with Example 1 is: synthetic MFC-N-100: 1.0gFe 3 o 4 SiO 2 Add to 15mL high-purity water, add 5.0g AlCl after ultrasonic dispersion 3 ·6H 2 O, and then ultrasonically mixed for 20 minutes to obtain solution I; 1.76g of NaOH and 3.62g of 2-aminoterephthalic acid were mixed with water and ultrasonically dispersed to obtain solution II. Under the condition of stirring at room temperature with a rotation speed of 500 rpm, add solution I dropwise to solution II to form a suspension and continue stirring for 6 hours; then wash with high-purity water and dry at room temperature; then activate in DMF solution at 150°C for 5 hours , and finally washed with ethanol to obtain MFC-N-100 solid-phase adsorbent. Its TEM see image 3 , see SEM Figure 4 , FT-IR see Figure 5 , see XRD Image 6 , magnetic properties see Figure 7 .

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Abstract

The invention discloses a magnetic MOFs solid phase extraction adsorbent as well as a preparation method and application thereof. The preparation method of the adsorbent comprises the following steps: (1) preparing magnetic Fe3O4 nanospheres with the particle size of 10-20 nm by adopting a coprecipitation method; (2) preparing Fe3O4@SiO2 with a core-shell structure by adopting a Stober silica gel coupling method; (3) preparing Fe3O4@SiO2@MOF by adopting an in-situ growth method; (4) adjusting the ratio of organic ligands in the synthesis process of the step 3 to prepare the amino-functionalized magnetic MOFs solid phase extraction adsorbent with different ratios, wherein the prepared magnetic MOFs solid phase extraction adsorbent comprises a magnetic Fe3O4 core as well as an SiO2 layer and an MOF layer covering the Fe3O4 core from the inside to outside in sequence, and the MOF layer is MIL-53(NH2) or MIL-100. The preparation method is simple, novel, low in cost and environment-friendly; the prepared magnetic MOFs solid phase adsorbent has the advantages of being high in adsorption speed, large in adsorption capacity, high in removing efficiency and the like for removing organic dyestuff and metal ions in water body.

Description

technical field [0001] The invention belongs to the field of wastewater treatment, and in particular relates to a preparation method and application of a magnetic MOF adsorbent. Background technique [0002] With the rapid development of industry, a large number of pollutants such as organic dyes and heavy metal ions are continuously discharged into the environment, and environmental pollution is becoming more and more serious, which has become a common concern all over the world. The massive discharge of organic dyes and heavy metals is very harmful to the environment and human health, so it is very important to develop a simple and efficient treatment technology for pollutants in water. At present, water treatment technologies mainly include precipitation, adsorption, membrane separation, etc. Among them, adsorption has been widely used in the field of water treatment because of its advantages of simple operation, fast separation, low cost, and high recovery rate. For ads...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30B01J20/28C02F1/28C02F1/62
Inventor 胡斌黄理金何蔓陈贝贝
Owner WUHAN UNIV
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