Method for preparing porous Fe3O4 (ferroferric oxide) magnetic nanometer microspheres by one-step method and application thereof

A technology of ferroferric oxide and magnetic nanometers, which is applied in the direction of chemical instruments and methods, iron oxide/iron hydroxide, ferrous oxide, etc., can solve the problems of complex preparation process and time-consuming, and achieve simple preparation process , good dispersion effect

Inactive Publication Date: 2017-05-31
HANGZHOU DIANZI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

Currently Fe 3 o 4 The preparation methods of heavy metal ion magnetic adsorbents are mostly limited to the above methods, and the prepared magnetic adsorbents have good adsorption effect, but the preparation process is still relatively complicated and time-consuming.
At present, the preparation of porous Fe suitable for the adsorption of heavy metal ions by one-step method 3 o 4 The methods of nanospheres are rarely reported

Method used

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  • Method for preparing porous Fe3O4 (ferroferric oxide) magnetic nanometer microspheres by one-step method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Take 2.5g FeCl 3 ·6H 2 O, 3.6g NaAc and 4.8g polyethyleneimine (molecular weight 10000) were respectively dissolved in three parts of ethylene glycol, and then the three solutions were mixed (72.5 g of ethylene glycol in total), and a uniform solution was formed after thorough stirring. Put it in a high-pressure reactor and react at 180°C for 24h, collect the product with a magnet, wash it with water and absolute ethanol three times, and dry it in vacuum at 50°C for 24h to obtain polyethyleneimine-modified Fe 3 o 4 Magnetic porous nanospheres. The saturation magnetization of the magnetic microspheres is 74.6emu / g, and the content of polyethyleneimine is 9.4% by thermogravimetric analysis; the specific surface area is 78.5m2 by nitrogen adsorption instrument. 2 / g. Take 0.02g Fe 3 o 4 Microspheres were added to 50mL copper ion wastewater (pH=5.5, Cu 2+ Concentration is 50mg / L), magnetically separated after shaking at 25°C for 2h, Cu 2+ The removal rate reaches 98...

Embodiment 2

[0023] Take 2.0g FeCl 3 ·6H 2 O, 8.0g NaAc and 3.0g polyethyleneimine (molecular weight 10000) were dissolved in three parts of ethylene glycol respectively, then the three solutions were mixed (72.5g of ethylene glycol in total), and a uniform solution was formed after thorough stirring. Put it in a high-pressure reactor and react at 200°C for 6h, collect the product with a magnet, wash it with water and absolute ethanol three times, and dry it in vacuum at 50°C for 24h to obtain polyethyleneimine-modified Fe 3 o 4 Magnetic porous nanospheres. The saturation magnetization of the magnetic microspheres is 75.2emu / g, and the content of polyethyleneimine is 7.5% by thermogravimetric analysis; the specific surface area is 57.7m2 by nitrogen adsorption instrument. 2 / g. Take 0.02g Fe 3 o 4 Microspheres were added to 50mL copper ion wastewater (pH=5.5, Cu 2+Concentration is 50mg / L), magnetically separated after shaking at 25°C for 2h, Cu 2+ The removal rate reaches 95.6%. A...

Embodiment 3

[0025] Take 2.0g FeCl 3 ·6H 2 O, 8.0g NaAc and 0.85g polyethyleneimine (molecular weight 1800) were dissolved in three parts of ethylene glycol respectively, then the three solutions were mixed (72.5g of ethylene glycol in total), and a uniform solution was formed after thorough stirring. Put it in a high-pressure reactor and react at 220°C for 2 hours, collect the product with a magnet, wash it with water and absolute ethanol three times, and dry it in vacuum at 50°C for 24 hours to obtain polyethyleneimine-modified Fe 3 o 4 Magnetic porous nanospheres. The saturation magnetization of the magnetic microspheres is 67.9emu / g, and the content of polyethyleneimine is 2.3% by thermogravimetric analysis; the specific surface area is 28.3m2 by nitrogen adsorption instrument. 2 / g. Take 0.04g Fe 3 o 4 Add microspheres in 50mL lead ion wastewater (pH=5.5, Pb 2+ Concentration is 35mg / L), magnetically separated after shaking at 25°C for 2h, Pb 2+ The removal rate reaches 96.3%. ...

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Abstract

The invention relates to a method for preparing porous Fe3O4 (ferroferric oxide) magnetic nanometer microspheres by a one-step method and application thereof. According to the method, polyethyleneimine is used as an end-capping reagent; the porous Fe3O4 nanometer microspheres are prepared through a solvent thermal reaction one-step method; the additional template agent and template removal step is not needed. The polyethyleneimine end-capping reagent can be used for controlling the crystal grain growth and the piling structure so as to regulate the hole structure and the specific surface area of the magnetic microspheres; meanwhile, the polyethyleneimine attached on the crystal grains has rich amine groups; strong chelation capability is realized on heavy metal. The obtained porous magnetic nanometer microspheres have the advantages that the preparation process is simple; the adsorption volume is great; good application prospects are realized in the field of heavy metal ion adsorption in water bodies.

Description

technical field [0001] The present invention relates to the synthesis of a porous Fe suitable for the removal of heavy metal ions 3 o 4 Magnetic nanometer sphere, and the specific use method of the magnetic nanometer sphere. It is specifically related to the one-step preparation of porous Fe with polyethyleneimine as the end-capping agent. 3 o 4 Magnetic nanospheres and their application in the field of adsorption of heavy metal ions. Background technique [0002] With the continuous development of industrial economy, more and more water bodies are exposed to heavy metal ions (Pb 2+ 、Cd 2+ 、Cu 2+ etc.), seriously endangering the environment and human health. At present, the removal methods for heavy metal ions in water at home and abroad mainly include membrane separation, adsorption, ion exchange, chemical precipitation, biological flocculation and ecological restoration. The chemical precipitation method is limited to wastewater with high concentration of heavy met...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/08B01J20/06B01J20/28C02F1/28
CPCC01G49/08B01J20/06B01J20/28007B01J20/28009B01J20/28019C01P2004/04C01P2004/32C01P2004/62C01P2006/12C01P2006/42C02F1/281
Inventor 吕挺张川赵红挺
Owner HANGZHOU DIANZI UNIV
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