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A kind of preparation method of zirconia

A technology of zirconium oxide and zirconium oxychloride, applied in zirconium oxide and other directions, can solve the problems of easy agglomeration of zirconium oxide, and achieve the effects of easy operation, overcoming serious agglomeration and simple reaction process

Active Publication Date: 2016-04-13
HUBEI XITIAN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to provide a new method for preparing zirconia, which uses an ionic liquid to prepare zirconia at normal pressure and lower temperature in a liquid phase system, which can effectively overcome the problem of easy agglomeration of zirconia prepared by precipitation , energy saving and environmental protection, while taking into account the advantages of the hydrothermal method, the prepared zirconia powder has excellent performance

Method used

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  • A kind of preparation method of zirconia
  • A kind of preparation method of zirconia
  • A kind of preparation method of zirconia

Examples

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preparation example Construction

[0028] The preparation method of zirconia provided by the invention comprises:

[0029] Add zirconium oxychloride and sodium hydroxide to ionic liquid-sodium trifluoromethanesulfonate for reaction, the reaction temperature is controlled at 260-300°C, the operating pressure is normal pressure, and the reaction time is 4-20 hours, preferably 6-20 hours. After 14 hours, after the reaction, the reaction product was washed with deionized water and centrifuged, and the obtained solid was treated at high temperature to obtain zirconia powder.

[0030] Wherein, the mass ratio of zirconium oxychloride to sodium hydroxide is 5-20:1. Sodium trifluoromethanesulfonate only acts as a solvent, and its consumption is determined according to actual production needs, and it is advisable to make the reaction go smoothly.

[0031] The particle size of the zirconia separated after the reaction is generally about 10nm. After high-temperature calcination, the physical indicators such as particle si...

Embodiment 1

[0039] Add 1 kg of sodium trifluoromethanesulfonate to the reactor, control the temperature of the oil bath at 300° C., and keep it warm for 2 hours, add 300 g of zirconium oxychloride and 30 g of sodium hydroxide, and keep it warm for 5 hours. The material in the reactor was poured into deionized water, centrifuged after stirring, and the solid was calcined at high temperature to control physical indicators such as particle size and specific surface area to obtain 107g of zirconia powder. Sodium trifluoromethanesulfonate is recovered from the mother liquor after recrystallization.

[0040] figure 1 The XRD spectrum of the product prepared in Example 1 is confirmed to be zirconia after comparing with the standard spectrum.

[0041] figure 2 Transmission electron micrograph (overall) of the product prepared for Example 1.

[0042] image 3 Transmission electron micrograph (microdomain) of the product prepared for Example 1.

[0043] From figure 2 and image 3 It can be...

Embodiment 2

[0045]Add 0.5kg of sodium trifluoromethanesulfonate to the reactor, control the temperature of the oil bath at 280°C, and keep it warm for 2 hours, then add 200g of zirconium oxychloride and 30g of sodium hydroxide, and keep it warm for 8 hours. Pour the contents of the reactor into deionized water, centrifuge after stirring, and calcine the solid at high temperature to control physical indicators such as particle size and specific surface area to obtain 71g of zirconia powder. Sodium trifluoromethanesulfonate is recovered from the mother liquor after recrystallization.

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Abstract

The invention discloses a method for preparing zirconium oxide. The method for preparing the zirconium oxide is characterized in that the zirconium oxide is prepared by reacting zirconium oxychloride and sodium hydroxide in the ion liquid-sodium trifluoromethanesulfonate under normal pressure. The method comprises the following steps: adding the zirconium oxychloride and sodium hydroxide into the ion liquid-sodium trifluoromethanesulfonate to react, wherein the reacting temperature is 260-300 DEG C, the operation pressure is normal pressure and the reaction time is 4-20h, after finishing reaction, washing the reaction product by deionized water, centrifuging and separating, and treating the obtained solid object at high temperature to obtain the zirconium oxide powder. The separated mother solution is treated and the ion liquid-sodium trifluoromethanesulfonate is recovered and recycled. By adopting the method, a high-tension apparatus is not needed, the reaction condition is mild and the treatment of plenty of industrial cleaning waste water is not needed in the process. The zirconium oxide powder prepared by the method is excellent in performance without agglomeration phenomenon. Various zirconium oxide composite powders containing a stabilizer can be produced by additionally adding the stabilizer.

Description

technical field [0001] The invention relates to a preparation method of zirconia, which belongs to the technical field of material preparation technology. Background technique [0002] Zirconia powder is mainly used to make fine ceramics, and has a wide range of applications in industrial fields such as structural ceramics, electronic ceramics, bioceramics, optical fiber communications, sensors, and fuel cells. The physical and chemical indicators of zirconia powder have an important impact on the performance of the product. [0003] The methods of producing zirconia powder mainly include precipitation method, hydrothermal method, sol-gel method and so on. The precipitation method is generally to add a precipitant to the metal zirconium salt solution to form a colloid of zirconium hydroxide, and then calcine the colloid of zirconium hydroxide to obtain zirconia powder. Although this method is simple and easy to implement and the cost is low, during the high-temperature cal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/02C04B35/486C04B35/488
Inventor 邢长生黄勇邹先明陈翔宇
Owner HUBEI XITIAN TECH CO LTD
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