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Method for preparing TiO2/SiO2 composite microspheres

A technology of composite microspheres and ammonia water, which is applied in the field of nanomaterials, can solve the problems of high processing temperature, low sunlight utilization rate, and many impurities, and achieve the effects of uniform particle size, shortened preparation cycle, and good dispersion

Inactive Publication Date: 2012-11-14
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Titanium dioxide has the characteristics of non-toxic, harmless, high chemical stability, opacity, excellent whiteness and gloss, and good photocatalytic activity. It is an excellent white inorganic pigment and photocatalyst. However, due to the large band gap of titanium dioxide, it needs to be Electron-hole pairs can only be excited under near-ultraviolet light, and the utilization rate of sunlight is small, and there are disadvantages such as easy aggregation, easy deactivation, and difficulty in recycling.
Although the chemical vapor deposition method has the advantages of short cycle and low cost, its TiO 2 / SiO 2 Composite material particles have disadvantages such as wide particle size distribution, uneven particle size distribution, difficult control of Si / Ti ratio, and difficulty in mixing components uniformly, resulting in uneven chemical composition of the product.
The disadvantages of the traditional sol-gel method are high cost, high processing temperature, and easy agglomeration of primary particles.
Co-precipitation method has low production efficiency, the product is not easy to separate and control, and there are many impurities

Method used

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  • Method for preparing TiO2/SiO2 composite microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A kind of TiO 2 / SiO 2 The preparation method of composite microsphere comprises the following steps:

[0023] 1) Dissolve 192.14g (1mol) of citric acid in 300ml of ammonia water with a volume concentration of 25%, then add 0.5mol of ethyl orthosilicate, stir to dissolve the ethyl orthosilicate; after dissolving, add 100ml in sequence Dehydrated ethanol and 64.05g of polyethylene glycol (PEG4000), heated to 50 ° C and stirred to completely dissolve; adjust the pH value to 7.0 with ammonia water to obtain Sol A;

[0024] 2) Dissolve 192.14g (1mol) of citric acid in 300ml of ammonia water with a volume concentration of 25%, then add 0.5mol of butyl titanate, stir to dissolve the butyl titanate; Water ethanol and 64.05g of polyethylene glycol (PEG4000), heated to 50°C and stirred to dissolve completely; adjusted the pH value to 7.0 with ammonia water, and evaporated in a water bath at 80°C until wet gel B was obtained;

[0025] 3) According to the molar ratio of Si:Ti=1...

Embodiment 2

[0029] A kind of TiO 2 / SiO 2 The preparation method of composite microsphere comprises the following steps:

[0030] 1) Dissolve 192.14g (1mol) of citric acid in 300ml of ammonia water with a volume concentration of 28%, then add 0.67mol of ethyl orthosilicate, stir to dissolve the ethyl orthosilicate; after dissolving, add 150ml in sequence Anhydrous ethanol and 96.07g of polyethylene glycol (PEG4000) were heated to 60°C and stirred to dissolve completely; the pH value was adjusted to 8.0 with ammonia water to obtain Sol A;

[0031] 2) Dissolve 192.14g (1mol) of citric acid in 300ml of ammonia water with a volume concentration of 28%, then add 0.67mol of butyl titanate, stir to dissolve the butyl titanate; Water ethanol and 96.07g of polyethylene glycol (PEG4000), heated to 60°C and stirred to dissolve completely; adjusted the pH value to 8.0 with ammonia water, and evaporated in a water bath at 90°C until wet gel B was obtained;

[0032] 3) According to the molar ratio o...

Embodiment 3

[0035] A kind of TiO 2 / SiO 2 The preparation method of composite microsphere comprises the following steps:

[0036]1) Dissolve 192.14g (1mol) of citric acid in 300ml of ammonia water with a volume concentration of 28%, then add 0.55mol of ethyl orthosilicate, stir to dissolve the ethyl orthosilicate; after dissolving, add 120ml in sequence Anhydrous ethanol and 85g of polyethylene glycol were heated to 56°C and stirred to dissolve completely; the pH value was adjusted to 7.5 with ammonia water to obtain Sol A;

[0037] 2) Dissolve 192.14g (1mol) of citric acid in 300ml of ammonia water with a volume concentration of 28%, then add 0.55mol of butyl titanate, stir to dissolve the butyl titanate; Water ethanol and 75g of polyethylene glycol, heated to 50°C and stirred to dissolve completely; adjust the pH value to 7.0 with ammonia water, and evaporate in a water bath at 90°C until wet gel B is obtained;

[0038] 3) According to the molar ratio of Si:Ti=1:6, sol A was added to...

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Abstract

The invention discloses a method for preparing TiO2 / SiO2 composite microspheres. In the method, tetraethoxysilane and tetrabutyl titanate are used as raw materials, ammonia water and absolute ethyl alcohol are used as solvents, citric acid is used as a complexing agent and polyethylene glycol is used as a dispersing agent. The method comprises the following steps of: adding Si-containing sol intoTi-containing wet gel with constantly stirring; evaporating in a water bath, drying and foaming to compound the Si-containing sol and the Ti-containing wet gel constantly; and calcining to obtain theTiO2 / SiO2 composite microspheres. The method of the invention has short preparation period; and the prepared TiO2 / SiO2 composite microspheres are complete spheres of which the particle size is 100 to900nm and have high purity and yield.

Description

technical field [0001] The invention belongs to the technical field of nanomaterials and relates to a TiO 2 / SiO 2 Preparation method of composite microspheres. Background technique [0002] Titanium dioxide has the characteristics of non-toxic, harmless, high chemical stability, opacity, excellent whiteness and gloss, and good photocatalytic activity. It is an excellent white inorganic pigment and photocatalyst. However, due to the large band gap of titanium dioxide, it needs to be The generation of electron-hole pairs can only be excited under near-ultraviolet light, which has a low utilization rate of sunlight, and has the disadvantages of easy aggregation, easy deactivation, and difficulty in recycling and reuse. In addition, due to the strong photocatalytic properties of titanium dioxide, when used as a coating, it is easy to cause yellowing and powdering of the paint film, while TiO2 2 / SiO 2 Composite powder can just improve these defects, thereby broadening the a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J13/02B01J21/08
Inventor 伍媛婷王秀峰
Owner SHAANXI UNIV OF SCI & TECH