Preparation method and application of modified superparamagnetic Fe3O4 nanoparticle

A nanoparticle and superparamagnetic technology, applied in chemical instruments and methods, alkali metal oxides/hydroxides, inorganic chemistry, etc., can solve problems such as environmental pollution, mercury metal loss, secondary pollution, etc., and meet the preparation conditions The effect of low requirements, simple preparation process and large specific surface area

Active Publication Date: 2016-06-22
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] There is a large amount of mercury in many industrial wastewaters. The existence of these mercury compounds will not only cause environmental pollution, threaten human health, but also cause a large amount of mercury metal loss
Due to the existence of many forms in mercury-containing wastewater, it is difficult to remove it by general methods
At present, the precipitation method is the main method for removing mercury in industry. Its principle is to use a precipitant to precipitate mercury in mercury-containing wastewater, but the precipitate generated in this process is not easy to separate, and the used precipitant will also cause Secondary pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The preparation method of this thiol-amino-modified superparamagnetic nanometer material is as follows:

[0017] (1) Add 20mol of FeCl 3 .6H 2 O and 10mol FeCl 2 .4H 2 O was dissolved in 1 L of deionized water, then 3 L of NH 4 OH solution (0.50mol / L), mechanically stirred at 60°C; 3 o 4 The nanoparticles were separated from the suspension and washed repeatedly with deionized water to obtain nano-Fe 3 o 4 particle.

[0018] (2) Add nano-Fe at a ratio of 16g / L 3 o 4 Ultrasonic dispersion in a mixed solution of ethanol and water (the volume ratio of ethanol and water is 20:1) to obtain a suspension, add ammonia solution (commercially available; 25wt%) to the suspension at a ratio of 17ml / L, and keep stirring During the process, add tetraethyl orthosilicate to the mixed solution at a ratio of 20ml / L, and continue stirring at 60°C for 4h to obtain Fe 3 o 4 SiO 2 nanoparticles, and then magnetized the Fe 3 o 4 SiO 2 The nanoparticles are separated from the su...

Embodiment 2

[0023] The preparation method of this thiol-amino-modified superparamagnetic nanometer material is as follows:

[0024] (1) Add 21mol of FeCl 3 .6H 2 O and 10.5 mol of FeCl 2 .4H 2 O was dissolved in 1 L of deionized water and then 3.1 L of NH 4 OH solution (0.55mol / L), mechanically stirred at 70°C; 3 o 4 The nanoparticles were separated from the suspension and washed repeatedly with deionized water to obtain nano-Fe 3 o 4 particle.

[0025] (2) Add nano-Fe at a ratio of 17g / L 3 o 4 Ultrasonic dispersion in a mixed solution of ethanol and water (the volume ratio of ethanol and water is 10:1) to obtain a suspension, add ammonia solution (commercially available; 25wt%) to the suspension at a ratio of 20ml / L, and keep stirring During the process, add tetraethyl orthosilicate to the mixed solution at a ratio of 21ml / L, and continue stirring at 55°C for 5h to obtain Fe 3 o 4 SiO 2 nanoparticles, and then magnetized the Fe 3 o 4 SiO 2 The nanoparticles are separated fr...

Embodiment 3

[0030] The preparation method of this thiol-amino-modified superparamagnetic nanometer material is as follows:

[0031] (1) Add 22mol of FeCl 3 .6H 2 O and 11 mol of FeCl 2 .4H 2 O was dissolved in 1 L of deionized water and then 3.5 L of NH 4 OH solution (0.55mol / L), mechanically stirred at 80°C; 3 o 4 The nanoparticles were separated from the suspension and washed repeatedly with deionized water to obtain nano-Fe 3 o 4 particle.

[0032] (2) Add nano-Fe at a ratio of 16.5g / L 3 o 4 Ultrasonic dispersion in a mixed solution of ethanol and water (the volume ratio of ethanol and water is 20:1.5) to obtain a suspension, add ammonia solution (commercially available; 25wt%) to the suspension at a ratio of 18ml / L, and keep stirring During the process, add tetraethyl orthosilicate to the mixed solution at a ratio of 22ml / L, and continue stirring at 50°C for 6h to obtain Fe 3 o 4 SiO 2 nanoparticles, and then magnetized the Fe 3 o 4 SiO 2 The nanoparticles are separate...

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PUM

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Abstract

The invention discloses a preparation method and application of a modified superparamagnetic Fe3O4 nanoparticle, belonging to the field of treatment of industrial wastewater. The method comprises the following steps of preparing the superparamagnetic Fe3O4 nanoparticle by adopting a coprecipitation method; by taking superparamagnetic Fe3O4 as a core, coating the surface of Fe3O4 with one or more layers of silica shells by adopting hydrolysis; modifying coated silica by applying a coupled reaction principle; by taking 3-aminopropyl trimethoxysilane as a modification reagent, modifying on a core-shell structure and connecting to an amino group; finally, using chloromethyl thiirane to synthesize a chelate which simultaneously contains nitrogen and sulfur by a nucleophilic substitution reaction; then using the chelate to adsorb heavy metal mercury, and in particular to selectively adsorb Hg<2+> at normal temperature, wherein the adsorption efficiency of the chelate is significantly higher than that of a chelate which is previously synthesized and only contains a sulfur ligating atom. The modified superparamagnetic Fe3O4 nanoparticle has the advantage of easiness in recovery and regeneration.

Description

technical field [0001] The invention relates to a modified superparamagnetic Fe 3 o 4 The preparation method and application of nano particles belong to the field of industrial waste water treatment. Background technique [0002] A large amount of mercury exists in many industrial wastewaters. The existence of these mercury compounds will not only cause environmental pollution, but also pose a threat to human health, and cause a large amount of mercury metal loss. Since there are many forms of mercury-containing wastewater, it is difficult to remove it by general methods. At present, the precipitation method is the main means of mercury removal in industry. Its principle is to use a precipitant to precipitate mercury in mercury-containing wastewater, but the precipitate generated in this process is not easy to separate, and the used precipitant will also cause Secondary pollution. Contents of the invention [0003] The object of the invention is to provide a modified s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28C02F1/28C02F101/20
CPCB01J20/223B01J20/28009B01J20/28016C02F1/285C02F1/288C02F2101/20
Inventor 汤立红包双友李凯宁平张冬冬孙鑫郭惠斌朱婷婷宋辛金旭张秀英
Owner KUNMING UNIV OF SCI & TECH
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