Preparation method of echinoid titanium dioxide microspheres in single/double layer cavity structure

A titanium dioxide, single-layer technology, applied in the direction of titanium dioxide, titanium oxide/hydroxide, etc., can solve the problems such as no titanium dioxide cavity microspheres reported, and achieve high yield, low preparation cost, and controllable process flow Effect

Inactive Publication Date: 2011-01-12
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although some have also adopted the template method, for example (China, patent number: CN200710173111.2, patent name: the sol-gel method preparation method of silicon dioxide / titanium dioxide hollow microspheres), but also can only get the surface without complicated appearance. core-shell structure
In the existing patents, there is no report on titanium dioxide hollow microspheres with multi-level complex structures at the micro-nano scale

Method used

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  • Preparation method of echinoid titanium dioxide microspheres in single/double layer cavity structure
  • Preparation method of echinoid titanium dioxide microspheres in single/double layer cavity structure
  • Preparation method of echinoid titanium dioxide microspheres in single/double layer cavity structure

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example 1

[0027] Step 1: Preparation of monodisperse silica microspheres using Method, in a mixture of tetraethyl orthosilicate, absolute ethanol and deionized water, under room temperature (20°C-30°C), magnetic stirring, adding catalyst ammonia water (concentration: 25%-28%), reaction 6 hours, centrifuged, washed with water, and dried to obtain silica microspheres with a diameter of about 300 nm. The molar ratio of each material is: ethyl orthosilicate: ammonia water: water: absolute ethanol = 1: 14: 135: 86.

[0028] Step 2: Disperse the silica microspheres in water for ultrasonic activation, centrifuge, disperse in a large amount of absolute ethanol, add a certain amount of catalyst ammonia water (concentration is 25%-28%), ultrasonically disperse, heat in a water bath at 45°C, and magnetically Stir, and finally add tetrabutyl titanate ethanol solution, react for 2 hours, centrifuge, wash with alcohol, wash with water, and dry to obtain silica / titanium oxide core-shell composite mi...

example 2

[0032] Step 1: Preparation of monodisperse silica microspheres using Method, in a mixture of tetraethyl orthosilicate, absolute ethanol and deionized water, under room temperature (20°C-30°C), magnetic stirring, adding catalyst ammonia water (concentration: 25%-28%), reaction 6 hours, centrifuged, washed with water, and dried to obtain silica microspheres with a diameter of about 300 nm. The molar ratio of each material is: ethyl orthosilicate: ammonia water: water: absolute ethanol=1: 14: 135: 86 (TEOS: NH 3 :H 2 O:EtOH molar ratio is 1:14:135:86).

[0033] Step 2: Disperse the silica microspheres in water for ultrasonic activation, centrifuge, disperse in a large amount of absolute ethanol, add a certain amount of catalyst ammonia water (concentration is 25%-28%), ultrasonically disperse, heat in a water bath at 45°C, and magnetically Stir, and finally add tetrabutyl titanate ethanol solution, react for 2 hours, centrifuge, wash with alcohol, wash with water, and dry to ...

example 3

[0036] Step 1: Preparation of monodisperse silica microspheres using Method, in a mixture of tetraethyl orthosilicate, absolute ethanol and deionized water, under room temperature (20°C-30°C), magnetic stirring, adding catalyst ammonia water (concentration: 25%-28%), reaction 6 hours, centrifuged, washed with water, and dried to obtain silica microspheres with a diameter of about 300 nm. The molar ratio of each material is: ethyl orthosilicate: ammonia water: water: absolute ethanol=1: 14: 135: 86 (TEOS: NH 3 :H 2 O:EtOH molar ratio is 1:14:135:86).

[0037] Step 2: Disperse the silica microspheres in water for ultrasonic activation, centrifuge, disperse in a large amount of absolute ethanol, add a certain amount of catalyst ammonia water (concentration is 25%-28%), ultrasonically disperse, heat in a water bath at 45°C, and magnetically Stir, and finally add tetrabutyl titanate ethanol solution, react for 2 hours, centrifuge, wash with alcohol, wash with water, and dry to ...

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Abstract

The invention relates to a preparation method of echinoid titanium dioxide microspheres in single/double layer cavity structure, belonging to the field of nano composite materials. The method comprises the following steps: (1) preparing monodisperse silicon dioxide microspheres with uniform particle size; (2) by using silicon dioxide as a template, coating a titanium dioxide layer on the surface of the silicon dioxide microspheres by using a sol-gel method to obtain core-shell type silicon dioxide/titanium dioxide composite microspheres; (3) regulating the concentration of sodium hydroxide solution, the hydrothermal reaction time and other conditions, and preparing echinoid titanium-base microspheres in the single/double layer cavity structure in a controllable way; and (4) treating the echinoid titanium-base microspheres in the single/double layer cavity structure with hydrochloric acid with a certain concentration, and calcining at high temperature to obtain anatase-type echinoid titanium dioxide microspheres in the single/double layer cavity structure. The material prepared by the method has the high-activity pure-phase titanium dioxide crystal structure, and has the advantages of large specific area, complete appearance and high yield; the technical process is controllable and easy to operate; and the invention also has the advantages of low preparation cost, no pollution 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 microspheres with a single-layer cavity structure and sea urchin shape. Background technique [0002] As a typical semiconductor material, titanium dioxide has a wide band gap (3.2eV) and unique chemical and physical properties. Materials with a special cavity structure composed of titanium dioxide have extremely important applications in many fields, such as: photocatalysis, treatment of organic pollutants, preparation of sensor devices, slow release of drugs, lightweight filling materials and lithium ions, solar energy battery materials, etc. In addition, titanium dioxide has the characteristics of good stability, non-toxicity and low price, which conforms to the concept of modern green environmental protection and is widely favored by people. Constructing special morphology and multi-level structure at the micro-nano scale plays ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/053
Inventor 王戈谭丽杨穆张晓伟
Owner UNIV OF SCI & TECH BEIJING
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