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Preparation and application of amino modified Fe3O4@SiO2@mSiO2 composite particles with mesoporous structure

A technology of amino modification and composite particles, which is applied in water/sludge/sewage treatment, silicon compounds, alkali metal compounds, etc. It can solve the problems of decreased adsorption capacity, weak magnetism, and insufficient specific surface area of ​​materials to improve adsorption capacity. , Good superparamagnetism, increase the effect of small size effect

Inactive Publication Date: 2016-09-28
XI'AN UNIVERSITY OF ARCHITECTURE AND TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But most of the Fe prepared so far 3 o 4 @SiO 2 The material can not meet the actual needs, one is low Fe 3 o 4 The load leads to weak magnetism, and the second is that the specific surface area of ​​the material is not small enough, resulting in a decrease in the adsorption capacity

Method used

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  • Preparation and application of amino modified Fe3O4@SiO2@mSiO2 composite particles with mesoporous structure
  • Preparation and application of amino modified Fe3O4@SiO2@mSiO2 composite particles with mesoporous structure
  • Preparation and application of amino modified Fe3O4@SiO2@mSiO2 composite particles with mesoporous structure

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Embodiment 1

[0055] An amino-modified Fe with mesoporous structure 3 o 4 @SiO 2 @mSiO 2 A method for preparing composite particles, comprising the steps of:

[0056] Step 1: Use a certain amount of ethylene glycol as a solvent, dissolve the ferric ion compound and sodium acetate in ethylene glycol, add an appropriate amount of polyethylene glycol under the condition of magnetic high-speed stirring to continue stirring to obtain a mixed solution, and then transfer to In a high-pressure reactor, heat to a certain temperature to crystallize for several hours, then wash and dry to obtain Fe 3 o 4 The nanoparticle has a diameter of 120nm and a coercive force of 68.95emu / g.

[0057] Crystallization temperature: 200°C, crystallization time: 8h; stirring rate: 600r / min; the molecular weight of polyethylene glycol is required to be 20000; ferric chloride is added to the ethylene glycol solution with a concentration of 0.03mol / L; Anhydrous sodium acetate is 0.08g. The ferric ion compound is: ...

Embodiment 2

[0065] An amino-modified Fe with mesoporous structure 3 o 4 @SiO 2 @mSiO 2 A method for preparing composite particles, comprising:

[0066] Step 1: Preparation of Fe 3 o 4 @SiO 2 powder;

[0067] Step 1.1: Preparation of Fe 3 o 4 Nanoparticles: use ethylene glycol as a solvent, dissolve ferric nitrate and sodium acetate in ethylene glycol, add the concentration of ferric nitrate to 0.03mol / L, and the concentration of sodium acetate to 0.01mol / L after adding to the ethylene glycol solution, stir Then add polyethylene glycol and continue to stir to obtain a mixed solution. The molecular weight of polyethylene glycol is 20,000 to 40,000, and the addition amount is 0.002mol / L, and then transferred to a high-pressure reactor, heated and crystallized, and then washed and dried. Get Fe 3 o 4 Nanoparticles; among them: crystallization temperature: 180°C, crystallization time: 8-24h; stirring rate: 600-900r / min; obtained Fe 3 o 4 The diameter of the nanoparticles is 100-15...

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Abstract

The invention relates to a preparation method of amino modified Fe3O4@SiO2@mSiO2 composite particles with a mesoporous structure. The preparation method comprises the steps: dispersing Fe3O4@SiO2 powder into a mixture solution of ethanol, deionized water, ammonia water and a template agent, so as to obtain a sol solution; then, dropwise adding TEOS into the sol solution, so as to prepare Fe3O4@SiO2@mSiO2 composite particles with the mesoporous structure; drying the Fe3O4@SiO2@mSiO2 composite particles, then, adding ethylene glycol into the dried Fe3O4@SiO2@mSiO2 composite particles, carrying out ultrasonic separation, then, adding a silane reagent, carrying out high-temperature refluxing while carrying out stirring so as to enable the silane reagent to be adsorbed into mesoporous pore passages of SiO2, carrying out a hydrolytic reaction, removing unreacted silane reagent or the silane reagent which is not adsorbed into the mesoporous pore passages, and finally, carrying out vacuum drying, thereby obtaining the amino modified Fe3O4@SiO2@mSiO2. According to the preparation method, SiO2 with a mesoporous structure serves as a shell layer, a nanoparticle Fe3O4 serves as a magnetic core, the stability in an acidic solution system is excellent, the difficult problem of the ordinary adsorbents that the separation is difficult after adsorption can be solved, the efficiency of adsorbing a target product is increased, and the reuse rate of an adsorbent is increased, so that the preparation method has good economic and environmental benefits.

Description

technical field [0001] The invention belongs to the technical field of separation of heavy metals in nanomaterials and water treatment technology, in particular to an amino-modified Fe with a mesoporous structure 3 o 4 @SiO 2 @mSiO 2 Preparation and application of composite particles. Background technique [0002] With the rapid growth of human society's demand for resources, a large amount of waste water containing heavy metals and organic dyes is increasing day by day in the process of production, processing and use. The heavy metals often mentioned mainly refer to elements such as lead (Pb), cadmium (Cd), mercury (Hg), bismuth (Bi), zinc (Zn), cobalt (Co), copper (Cu) and nickel (Ni). There are multiple and complex sources of heavy metal pollution, including smelting processes, exhaust gases from fuel combustion, pollution due to leakage, sewage discharge, litter disposal, and surface runoff from land systems, as well as sewage irrigation and garbage leaching The acc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/06B01J20/10B01J20/28B01J20/30C02F1/28C02F101/20C02F101/38
CPCB01J20/06B01J20/103C02F1/288B01J20/28009C02F2101/38C02F2101/308C02F2101/20
Inventor 马晶薛娟琴徐尚元
Owner XI'AN UNIVERSITY OF ARCHITECTURE AND TECHNOLOGY
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