Sol-gel method for preparing earth silicon/titanic oxide hollow microballoon

A titanium dioxide and silicon dioxide technology, applied in the field of nano-scale hollow microspheres, can solve the problem of only preparing a microsphere shell composed of one kind of inorganic particles, and achieves easy industrial production, simple production equipment and flexible production process. Effect

Inactive Publication Date: 2008-10-01
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The object of the present invention is to provide a kind of improved sol-gel method to prepare the method for silicon dioxide/titania hollow microspheres, aim to overcome existing technological method and be limited to can only prepare the microsph

Method used

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  • Sol-gel method for preparing earth silicon/titanic oxide hollow microballoon
  • Sol-gel method for preparing earth silicon/titanic oxide hollow microballoon
  • Sol-gel method for preparing earth silicon/titanic oxide hollow microballoon

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Add 20mL of styrene into a 300mL three-necked round-bottomed flask equipped with a condenser tube and a protective gas port with 200mL of deionized water inside, then add 0.6g of azobisisobutyl ether hydrochloride (AIBA) and 2.5g of poly Vinylpyrrolidone k30 (PVP), using magnetic stirring to mix evenly, and nitrogen into the reactor to evacuate oxygen for 1h, then use a water bath to heat to 70 ° C, keep warm for 24h. High-speed centrifugation to separate the white precipitate (PS), use Wash with deionized water and absolute ethanol 3 times. figure 1 The TEM photo of the PS microsphere template prepared for this example shows that the microsphere template is very uniform and has a diameter of about 262 nm.

Embodiment 2

[0027]After dispersing 1mL of polystyrene microsphere suspension (3wt%) into 15mL of deionized water and 50mL of isopropanol mixed solution, the solution was added to a 300mL three-neck round-bottomed flask equipped with a condenser tube and a protective gas port, After magnetically stirring for 15 min, 0.15 g of ethyl silicate (TEOS) was added, and the pH value of the solution was adjusted to ~10 with diluted ammonia (5 vol%) solution, and magnetically stirred at room temperature for 2 h. The white precipitate was separated by high-speed centrifugation and washed three times with isopropanol to obtain PS / SiO 2 Composite microsphere particles. figure 2 (a) is the PS / SiO described in this embodiment 2 TEM photo of organic-inorganic hybrid microspheres, the SiO of the resulting composite microspheres 2 The thickness of the shell layer is about 8nm, and the thickness of the shell layer is uniform, and the dispersion of the microspheres is good.

Embodiment 3

[0029] After dispersing 1mL of polystyrene microsphere suspension (3wt%) into 15mL of deionized water and 50mL of isopropanol mixed solution, the solution was added to a 300mL three-neck round-bottomed flask equipped with a condenser tube and a protective gas port, After magnetic stirring for 15 min, 0.6 g of ethyl silicate (TEOS) was added, and the pH value of the solution was adjusted to ~10 with diluted ammonia (5 vol%) solution, and magnetically stirred at room temperature for 2 h. The white precipitate was separated by high-speed centrifugation and washed three times with isopropanol to obtain PS / SiO 2 Organic-inorganic hybrid microsphere particles. When the content of ethyl silicate increases, SiO 2 The thickness of the shell layer also increases, but the dispersion of the microspheres becomes worse, which is due to more SiO 2 The generation of secondary particles leads to aggregation of microspheres. PS / SiO prepared in this embodiment 2 TEM pictures of organic-inorg...

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Abstract

The invention provides a method for preparing an SiO2/TiO2 hollow microsphere by a sol-gel method. The method is mainly characterized in that cation polystyrene microsphere (PS) is used as a formwork; ethyl silicate and butyl titanate are respectively used as raw material and diluted ammonia is taken as regulator of pH value; a multi-layer organic-inorganic hybrid composite microsphere is obtained by the sol-gel reaction under the temperature of 70-80 DEG C. Formwork particle of the obtained deposition is removed by a calcining process to obtain the SiO2/ TiO2 hollow microsphere. By changing the consistency of reactant, content of surfactant and calcining temperature, the SiO2/ TiO2 hollow microsphere with different spherical shell thickness, density and grain size can be obtained. The hollow microsphere prepared by the method has high photo-catalytic activity, overcomes the shortage that existing preparation method of hollow microsphere can only prepare single shell layer microsphere; the multi-layer hollow microsphere can be prepared, the technique is simple, the cost is low and the preparation method of the invention is suitable for industrialized production.

Description

technical field [0001] The invention relates to a sol-gel method for preparing silicon dioxide / titanium dioxide hollow hybrid microspheres, which can be used in photocatalysis, environmental protection, photonic crystals, drug controlled release, etc., and belongs to the field of nanoscale hollow microspheres. Background technique [0002] In recent years, hollow microspheres have been one of the hotspots in material science research, because they have important applications in the fields of controllable drug release, low-density fillings, photocatalysis, chromatography, confinement reactors, photonic crystals, etc. Titanium dioxide is widely used as the shell material of core-shell microspheres and hollow structures due to its non-toxicity, high chemical stability and low cost. [0003] The existing synthesis methods are mainly through the template method, including hard templates (for example, inorganic metal and polymer colloidal particles) and soft templates (for example...

Claims

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Application Information

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IPC IPC(8): B01J13/02C04B35/624
Inventor 高濂宋雪峰
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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