A kind of preparation method of zirconia nanopowder
A technology of nano-powder and zirconia, applied in zirconia, chemical instruments and methods, nanotechnology, etc., can solve the problems of expensive alkoxide, easy to form agglomerates, waste of resources, etc., and achieve high-efficiency and easy-to-use process The effect of high purification and small particle size of the product
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Embodiment 1
[0013] Dissolve zirconium oxychloride in pure water to make 0.1 mol / L zirconium oxychloride aqueous solution, heat to 40°C, react for 5 hours, and add 0.2L / (m 2 The flow rate of h) flows through the feed liquid side compartment, and the pure water flows at 0.1L / (m 2 The flow rate of h) flows through the side compartment of the diffusion liquid, so that the pH value of the feed liquid reaches 6.5, then the zirconium hydroxide colloidal suspension is filtered through a microfiltration filter, purified, concentrated by a membrane distillation device to form a slurry, and then The hydrothermal reaction is carried out in an autoclave, the reaction temperature is 100°C, the reaction pressure is 9.5MPa, and the reaction time is 3h. After dehydration, solid-liquid separation and drying are carried out to obtain zirconia nanopowder with a particle size of 5-10nm.
Embodiment 2
[0015] Dissolve zirconium oxychloride in pure water to make a 2.0mol / L zirconium oxychloride aqueous solution, heat to 96°C, react for 1.5 hours, and add 0.7L / (m 2 The flow rate of h) flows through the feed liquid side compartment, pure water at 1.0L / (m 2 The flow rate of h) flows through the side compartment of the diffusion liquid, so that the pH value of the feed liquid reaches 4.0, and then the zirconium hydroxide colloidal suspension is filtered through microfiltration and nanofiltration filters, purified, and concentrated by a membrane distillation device to form a slurry Then carry out hydrothermal reaction in an autoclave, the reaction temperature is 150°C, the reaction pressure is 5.0MPa, the reaction time is 1h, and after dehydration, solid-liquid separation and drying are carried out to obtain zirconia nanoparticles with a particle size of 10-30nm. Powder.
Embodiment 3
[0017] Dissolve zirconium oxychloride in pure water to make a 1.0mol / L zirconium oxychloride aqueous solution, heat to 70°C, react for 3 hours, and add 0.5L / (m 2 The flow rate of h) flows through the feed liquid side compartment, and the pure water flows at 0.5L / (m 2 The flow rate of h) flows through the side compartment of the diffusion liquid, so that the pH value of the feed liquid reaches 5.8, then the zirconium hydroxide colloidal suspension is filtered through a nanofiltration filter, purified, concentrated by a membrane distillation device to form a slurry, and then The hydrothermal reaction is carried out in an autoclave, the reaction temperature is 130°C, the reaction pressure is 0.5MPa, and the reaction time is 5h. After dehydration, solid-liquid separation and drying are carried out to obtain zirconia nanopowder with a particle size of 5-20nm.
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