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Thiohydroxy-modified magnetic MOFs adsorbent and preparation method and application thereof

An adsorbent and magnetic technology, applied in the field of thiol-modified magnetic MOFs adsorbent and its preparation, can solve the problems of not being particularly stable, weak interaction, poor selectivity, etc., and achieve large adsorption capacity, good stability, and low cost Effect

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, the currently prepared MFCs often lack certain functional units, have weak interactions with mercury, and poor selectivity. Therefore, it is necessary to further post-functionalize MFCs to improve their selectivity and adsorption capacity.
On the other hand, most of the current MFCs materials are mainly based on HKUST-1 as the modified material, and HKUST-1 is not particularly stable when 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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  • Thiohydroxy-modified magnetic MOFs adsorbent and preparation method and application thereof
  • Thiohydroxy-modified magnetic MOFs adsorbent and preparation method and application thereof
  • Thiohydroxy-modified magnetic MOFs adsorbent and preparation method and application thereof

Examples

Experimental program
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Embodiment l

[0039] 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.

[0040] Preparation of Fe with core-shell structure by St?ber silica gel coupling method 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 wa...

Embodiment 2

[0045] The difference from Example 1 is: Synthesis of MFC-S-2: Disperse 2 mmol of mercaptoglycolic acid in water, add KOH to adjust the pH to 7, then add 400 mg of activated MFC-O, let stand, and heat under the protection of Ar gas to 40 o C, kept for 40 hours; then washed with water and methanol in sequence, and dried at room temperature to obtain the mercapto-modified magnetic MOFs adsorbent MFC-S-2.

Embodiment 3

[0047] The difference from Example 1 is: Synthesis of MFC-S-3: Disperse 3 mmol of mercaptoglycolic acid in water, add KOH to adjust the pH to 7, then add 400 mg of activated MFC-O, let stand, and heat under the protection of Ar gas to 25 o C, kept for 72 hours; then washed with water and methanol in sequence, and dried at room temperature to obtain the mercapto-modified magnetic MOFs adsorbent MFC-S-3. 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 thiohydroxy-modified magnetic MOFs adsorbent and a preparation method and application thereof. The preparation method 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 silicone coupling method; (3) preparing Fe3O4@SiO2@MOF through a solvothermal in-situ growth method; (4) carrying out thiol-functionalization on Fe3O4@SiO2@MOF synthesized in the step (3) in a solvent auxiliary ligand exchange manner, and preparing the thiol-functionalized magnetic MOFs adsorbent with different proportions through adjusting the proportion of mercaptoacetic acid to Fe3O4@SiO2@MOF. According to the invention, the preparation method is mild in reaction conditions, low in cost, and simple and convenient to operate; the prepared magnetic MOFs adsorbent has the advantages of being high in adsorption speed, large in adsorption capacity and good in selectivity when removing the metal ions in water.

Description

technical field [0001] The invention belongs to the field of waste water treatment, and in particular relates to a mercapto-modified magnetic MOFs adsorbent and a preparation method and application thereof. Background technique [0002] With the rapid development of modern industry, a large amount of heavy metals are discharged into the environment. At present, heavy metal pollution has become one of the major hazards that threaten human health. Removing heavy metal ions in aqueous solution by traditional methods such as precipitation is not only costly and complicated to operate, but also often produces a large amount of toxic waste, forming secondary pollution. Environmental workers and researchers have done a lot of work on the treatment of heavy metal pollution such as low development cost and simple operation. [0003] Mercury, as a highly toxic heavy metal element, especially in the water environment, can enter the human body through direct ingestion, bioaccumulation,...

Claims

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Application Information

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