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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

Active Publication Date: 2018-09-28
NINGXIA BAOTA PETROCHEM SCI & TECH IND DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Zirconium dioxide nanopowder is an important raw material in the modern industry and technical field, and its preparation method has been greatly developed. Among them, the relatively mature methods include alkoxide hydrolysis, neutralization precipitation and hydrolysis precipitation, but the above methods There are many defects: the alkoxide of the alkoxide method is expensive, and the source of raw materials is difficult; the constant boiling time of the hydrolysis precipitation method is long and the energy consumption is large; the neutralization precipitation method is easy to form agglomerates, and the control of process conditions is relatively difficult. Zirconium is used as a raw material. When preparing zirconium hydroxide by the neutralization method, it is necessary to neutralize the precipitated hydrogen chloride. A large amount of ammonia water or sodium hydroxide will be consumed in the process, and a large amount of sodium chloride or chloride containing high concentration will also be produced after neutralization. Ammonium wastewater wastes resources and pollutes the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The invention relates to a preparing method for zirconium dioxide nano-powder. The preparing method comprises the following steps that zirconium oxychloride is dissolved in pure water to be prepared into an aqueous solution with the concentration being 0.1-2.0 mol / L, the aqueous solution is heated to 40-96 DEG C, and the temperature is maintained for 1-5 h; then, the aqueous solution flows into a material liquid side partition chamber of a diffusion dialysis membrane device, hydrogen chloride in the aqueous solution permeates an anion-exchange membrane and enters a diffusion liquid side partition chamber while zirconium hydroxide stays in the material liquid side partition chamber to form colloid suspension liquid, and meanwhile pure water flows into the diffusion liquid side partition chamber; zirconium hydroxide colloid suspension liquid is filtered with a filter and concentrated with a membrane distillation device, zirconium hydroxide paste is formed, the paste is dehydrated and dried, and the zirconium dioxide nano-powder is obtained. According to the zirconium dioxide nano-powder prepared through the method, the purity can reach 99.9% or above, the particle size ranges from 5 nm to 30 nm and is distributed uniformly, the technological process is efficient and saves energy, resources are saved, environment friendliness is achieved, and the scale is flexible.

Description

technical field [0001] The invention belongs to the technical field of chemical materials and relates to a preparation method of zirconium dioxide nanometer powder. Background technique [0002] Zirconium dioxide has excellent physical and chemical properties such as high hardness, high strength, high toughness, high wear resistance, chemical corrosion resistance and self-lubricating property. In recent years, it has become a hot spot in the field of scientific research and is widely used in preparation functions. Ceramic components, thermal barrier coating materials for solid oxide fuel cells, catalyst carriers, lubricating additives, gas-sensitive wear-resistant materials, electronic components, etc. [0003] Zirconium dioxide nanopowder is an important raw material in the modern industry and technical field, and its preparation method has been greatly developed. Among them, the more mature ones include alkoxide hydrolysis method, neutralization precipitation method and hy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/02B82Y40/00C01B7/07
CPCC01B7/07C01B7/0712C01G25/02C01P2004/64C01P2006/80
Inventor 杨惠琳张立忠马金红任立广
Owner NINGXIA BAOTA PETROCHEM SCI & TECH IND DEV
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