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Preparation method of urchin-like titanium dioxide magnetic microspheres having double-layer cavity structures

A technology of magnetic microspheres and titanium dioxide, applied in chemical instruments and methods, chemical/physical processes, catalysts for physical/chemical processes, etc., can solve problems such as no reports of titanium dioxide magnetic microspheres, and achieve simple and rapid separation and recovery, specific surface area The effect of large and low energy consumption

Inactive Publication Date: 2013-02-27
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the existing patents, there is no report on titanium dioxide magnetic microspheres with a sea urchin-like double-layer cavity structure on the micro-nano scale

Method used

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  • Preparation method of urchin-like titanium dioxide magnetic microspheres having double-layer cavity structures
  • Preparation method of urchin-like titanium dioxide magnetic microspheres having double-layer cavity structures
  • Preparation method of urchin-like titanium dioxide magnetic microspheres having double-layer cavity structures

Examples

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Effect test

example 1

[0023] Step 1: Preparation of monodisperse ferric ferric oxide magnetic microspheres: Add ferric chloride to ethylene glycol at 40°C, add anhydrous sodium acetate under stirring, stir vigorously for 0.5h, and then mix Transfer the solution to an airtight container, control the temperature at 180°C for 10 hours, centrifuge, wash with alcohol, wash with water, and dry to obtain magnetic ferric oxide microspheres with a diameter of 300-700nm for use; wherein, the mass ratio of each material For: ferric chloride: ethylene glycol: anhydrous sodium acetate = 1:41:3;

[0024] Step 2: Ultrasonic disperse the magnetic ferric oxide microspheres prepared in the above steps in 50mL, 0.1 molL -1 In hydrochloric acid, magnetically separate, then add ethanol, deionized water and ammonia water with a volume concentration of 25%-28%, stir mechanically at room temperature, then slowly add a mixed solution prepared by ethyl orthosilicate and ethanol dropwise, and react for 6h , through centrifu...

example 2

[0029] Step 1: Preparation of monodisperse ferric ferric oxide magnetic microspheres: Add ferric chloride to ethylene glycol at 60°C, add anhydrous sodium acetate under stirring conditions, stir vigorously for 1.5h, and then mix Transfer the solution to an airtight container, control the temperature at 100°C for 18 hours, centrifuge, wash with alcohol, wash with water, and dry to obtain magnetic ferric oxide microspheres with a diameter of 300-700nm for future use; wherein, the mass ratio of each material For: ferric chloride: ethylene glycol: anhydrous sodium acetate = 1:20:2;

[0030] Step 2: Ultrasonic disperse the magnetic ferric oxide microspheres prepared in the above steps in 50mL, 0.1 molL -1 In hydrochloric acid, magnetically separate, then add ethanol, deionized water and ammonia water with a volume concentration of 25%-28%, stir mechanically at room temperature, then slowly add the mixed solution prepared by ethyl orthosilicate and ethanol dropwise, and react for 5h...

example 3

[0035] Step 1: Preparation of monodisperse ferric ferric oxide magnetic microspheres: Add ferric chloride to ethylene glycol at 70°C, add anhydrous sodium acetate under stirring conditions, stir vigorously for 2.5 hours, and then mix Transfer the solution to an airtight container, control the temperature at 200°C for 12 hours, centrifuge, wash with alcohol, wash with water, and dry to obtain magnetic ferric oxide microspheres with a diameter of 300-700nm for use; wherein, the mass ratio of each material For: ferric chloride: ethylene glycol: anhydrous sodium acetate = 1:60:5;

[0036] Step 2: Ultrasonic disperse the magnetic ferric oxide microspheres prepared in the above steps in 50mL, 0.1 molL -1 In hydrochloric acid, magnetically separate, then add ethanol, deionized water and ammonia water with a volume concentration of 25%-28%, stir mechanically at room temperature, then slowly add a mixed solution prepared by ethyl orthosilicate and ethanol dropwise, and react for 6h , ...

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Abstract

The invention provides a preparation method of urchin-like titanium dioxide magnetic microspheres having double-layer cavity structures. The method comprises the following steps of: preparing monodisperse ferroferric oxide magnetic microspheres with uniform particle sizes; (2) coating silicon dioxide and titanium dioxide in sequence on the surface of ferroferric oxide with a sol-gel method; (3) adjusting conditions such as the concentration of a sodium hydrate solution, hydro-thermal reaction time and the like to prepare urchin-like titanium-based magnetic microspheres having single / double-layer cavity structures; and (4) treating the titanium-based magnetic microspheres with a hydrochloric acid solution with a certain concentration, and calcining at high temperature to obtain anatase urchin-like titanium dioxide magnetic microspheres having double-layer cavity structures. A material prepared with the method has a high-activity anatase titanium dioxide crystal structure, an urchin-like surface and a large specific surface area; the double-layer cavity structures can accommodate a large quantity of guest molecules; the microspheres have superparamagnetism, and simple and quick separation and recovery of a catalyst can be realized; and the method has the advantages of low preparation cost, controllable process flow, easiness for operating, environmental friendliness and low energy consumption.

Description

technical field [0001] The invention belongs to the field of nanocomposite materials, in particular to a method for preparing titanium dioxide magnetic microspheres with double-layer cavity structure and sea urchin shape. Background technique [0002] Semiconductor photocatalysis technology is currently the most promising technology in the purification of organic pollution. It can be used for the degradation of organic wastewater, the reduction of heavy metal ions, air purification, sterilization, anti-fog, etc. Anatase TiO2 semiconductor photocatalysis technology has the characteristics of high efficiency, environmental protection, low energy consumption, easy operation, can reduce secondary pollution, harmless to human body, etc., and in practical application, the process flow is simple, the operating conditions are easy to control, and it can be used in ultraviolet light Under the irradiation of light, it can effectively oxidize and degrade a variety of toxic pollutants,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/745B01J21/06B01J35/10
Inventor 王戈谭丽杨穆李洁
Owner UNIV OF SCI & TECH BEIJING
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