Nanometer zirconia sol and preparation method thereof

A nano-scale, zirconium-based technology, used in chemical instruments and methods, zirconium compounds, inorganic chemistry, etc., can solve problems such as unsuitable industrial production applications, low zirconia sol content, and complex equipment and equipment, saving labor resources, particle size, etc. The effect of narrow distribution and low reaction temperature

Inactive Publication Date: 2009-09-30
WUHAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The main disadvantages of this method are: (1) the equipment used in this preparation method is complex and demanding; (2) the precursor solution concentration used in this preparation method is very low, only 0.001~0.5mol / L, the obtained Zirconia sol content is too low, not suitable for industrial production applications

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  • Nanometer zirconia sol and preparation method thereof

Examples

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Comparison scheme
Effect test

Embodiment 1

[0016] A nano-scale zirconium sol and its preparation method: first, under the condition of stirring at 25-35°C, industrial zirconium oxychloride solution with a concentration of 0.1-0.3 mol / L and ammonia water with a concentration of 1.0-1.3 mol / L are mixed Slowly add it dropwise into the ammonium chloride buffer solution with a concentration of 0.1-0.4 mol / L, control the pH value of the mixed solution to 8-10, and continue stirring for 0.5-1 hour to obtain the precursor hydrated zirconium hydroxide precipitate. Then the hydrated zirconium hydroxide precipitate is washed with water and suction filtered for 2 to 4 times to obtain a filter cake; then the filter cake is dispersed in the In water, add nitric acid solution dropwise while stirring to obtain emulsion. Finally, add 0.1-0.4% polyethylene glycol 400 and 0.5-0.8% acetone to the emulsion respectively, and keep stirring for 0.25-0.5 hours; heat in a water bath at 85-90°C for 6-9 hours , to obtain a clear and transparent ...

Embodiment 2

[0019] A nano-scale zirconium sol and its preparation method: first, under the condition of stirring at 25-35°C, an industrial zirconium oxychloride solution with a concentration of 0.3-0.5 mol / L and ammonia water with a concentration of 1.3-1.5 mol / L are mixed Slowly add dropwise to the ammonium chloride buffer solution with a concentration of 0.2-0.5 mol / L, control the pH value of the mixed solution to 8-10, and continue stirring for 0.5-1 hour to obtain the precursor hydrated zirconium hydroxide precipitate. Then the hydrated zirconium hydroxide precipitate is washed with water for 2 to 4 times and suction filtered to obtain a filter cake; then the filter cake is dispersed in the In water, add nitric acid solution dropwise while stirring to obtain emulsion. Finally, add 0.2-0.5% polyethylene glycol 400 and 0.8-1.0% acetone to the emulsion respectively, and keep stirring for 0.25-0.5 hours; heat in a water bath at 85-90°C for 7-10 hours , to obtain a clear and transparent n...

Embodiment 3

[0021] A nano-scale zirconium sol and its preparation method: first, under the condition of stirring at 25-35°C, an industrial zirconium oxychloride solution with a concentration of 0.5-0.7 mol / L and ammonia water with a concentration of 1.5-1.7 mol / L are mixed Slowly add it dropwise into the ammonium chloride buffer solution with a concentration of 0.3-0.6 mol / L, control the pH value of the mixed solution to 8-10, and continue stirring for 0.5-1 hour to obtain the precursor hydrated zirconium hydroxide precipitate. Then the hydrated zirconium hydroxide precipitate is washed with water and suction filtered for 2 to 4 times to obtain a filter cake; then the filter cake is dispersed in the In water, add nitric acid solution dropwise while stirring to obtain emulsion. Finally, add 0.3-0.6% acetic acid and 1.0-1.2% acetone to the emulsion respectively, and keep stirring for 0.25-0.5 hours; heat in a water bath at 85-90°C for 8-11 hours to obtain clear Transparent nano-sized zirco...

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Abstract

The invention relates to a nanometer zirconia sol and a preparation method thereof. The proposal comprises the following steps that: firstly, an industrial zirconium oxychloride solution with a concentration of between 0.1 to 3 mol/L and ammonia water with a concentration of between 1 and 3.5 mol/L are slowly dripped into an ammonium chloride buffer solution with a concentration of between 0.1 and 1.5 mol/L at a temperature of between 25 and 35DEG C under stirring conditions, the pH value of the mixed solution is controlled to be between 8 and 10, and the mixed solution is continuously stirred for 0.5 to 1 hour to obtain a precursor, namely a zirconium hydroxide hydrate precipitate; then the zirconium hydroxide hydrate precipitate is scrubbed and carried out suction filtration for 2 to 4 times to obtain a filter cake; then the filter cake is dispersed into water according to the mol ratio that the zirconium hydroxide hydrate to nitric acid solution to the water is 1: 0.8-1.5: 40-200, and the nitric acid solution is dripped during the stirring to obtain an emulsion; and finally, a surfactant which accounts for 0.1 to 1.5 percent of the volume of the emulsion and a complexing agent which accounts for 0.5 to 3 percent of the volume of the emulsion are added into the emulsion respectively, the mixture is continuously stirred for 0.25 to 0.5 hour, and the mixture is heated for 6 to 20 hours in water bath at a temperature of between 85 and 90 DEG C to obtain the nanometer zirconia sol. The nanometer zirconia sol and the method have the characteristics of low cost, energy conservation, simple process, low equipment requirement and broad application range.

Description

technical field [0001] The invention belongs to the technical field of sol preparation. Specifically relates to a nano-scale zirconium sol and a preparation method thereof. Background technique [0002] The research on sol-gel technology was first started from the study of silica gel in the mid-nineteenth century. However, it was not until the 1930s that it was demonstrated that oxide films could be prepared by hydrolysis of metal alkoxides. In the late 1960s and early 1970s, due to the increasingly high requirements for new materials in electronics, communication technology, energy technology and other high-tech fields, sol-gel technology has been extensively and deeply researched, and has entered a rapid development. stage of development. [0003] Zirconia is widely used in many fields due to its unique excellent properties. Zirconia has a high melting point, high structural strength at high temperatures, stable chemical properties, high chemical inertness to acids and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/00
Inventor 赵惠忠张寒余俊徐兵聂建华贺中央
Owner WUHAN UNIV OF SCI & TECH
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