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Process for preparing nanometer zirconium dioxide powder by double liquid phase hydrolysis

A technology of zirconia and two-liquid phase, which is applied in the direction of zirconia, etc., can solve the problems of high cost, easy agglomeration of precursors, and inability to obtain zirconia nanopowders, etc., to achieve high raw material utilization rate, simple process, and realize flow The effects of sex work

Inactive Publication Date: 2008-10-22
TSINGHUA UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

[0008] There is a spontaneous hydrolysis equilibrium in the aqueous solution of zirconium oxychloride or zirconyl nitrate, and the hydrolysis products HCl and HNO can be decomposed after a long time of boiling. 3 All volatilized, so as to obtain the precursor of zirconia powder, zirconium hydroxide or zirconium oxyhydroxide, after drying and firing, zirconia nanopowder can be obtained, but in the general drying and firing process, the precursor is easy to agglomerate , but zirconia nanopowders cannot be obtained, some people can prepare zirconia nanopowders by using more complex and costly drying processes such as supercritical drying

Method used

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  • Process for preparing nanometer zirconium dioxide powder by double liquid phase hydrolysis

Examples

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example 1

[0020] Example 1: 50ml toluene, add 0.15g dioctyl sodium succinate sulfonate, stir for 10min; drop in 0.1mol / L ZrOCl 2 5ml, stir vigorously, heat to 85°C and boil for 3 hours; when the volume of the liquid phase is less than 25ml, the precipitation of zirconium hydroxide in the organic phase will be obtained, dry to remove ZrO 2 ·nH 2 O moisture, fired at 600°C for 4 hours to obtain spherical nanoparticles of zirconia. figure 1 Shown is a transmission electron micrograph of zirconia.

example 2

[0021] Example 2: 130ml toluene, add 0.45g dioctyl sodium succinate sulfonate, stir for 10min; drop in 0.5mol / L ZrOCl 2 20ml of aqueous solution, vigorously stirred and boiled at 85°C for 5 hours; the solution was turbid, the condensate was recovered, the liquid was separated, the lower layer was hydrochloric acid solution, the upper layer was toluene, hydrochloric acid and toluene were separated; when the water phase was no longer precipitated, the mixture was precipitated and dried , remove ZrO 2 ·nH 2 O moisture, to obtain primary embryo body, 700 ° C for 2 hours to obtain zirconia spherical nanoparticles.

example 3

[0022] Example 3: 130ml toluene, add 1.0g dioctyl sodium succinate sulfonate, stir for 10min; drop in 0.8mol / L ZrOCl 2 20ml of aqueous solution, vigorously stirred and boiled at 85°C for 8 hours; the solution was turbid, the condensate was recovered, the liquid was separated, the lower layer was hydrochloric acid solution, the upper layer was toluene, and hydrochloric acid and toluene were separated; when the water phase was no longer precipitated, the mixture was precipitated and dried , remove ZrO 2 ·nH 2 O moisture to obtain the primary embryo body, which was fired at 750°C for 2 hours to obtain spherical nanoparticles of zirconia.

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Abstract

The present invention discloses double-liquid phase hydrolysis process of preparing nano zirconia powder in the field of chemical material preparation. Hydrolysis of zirconium oxychloride or zirconyl nitrate is completed in double-liquid phase, i. e., via water-oil azeotropic process; the hydrolysis product HCl or HNO3 is eliminated; and through further stoving and roasting treatment, homogeneous and dispersed spherical nano zirconia powder of about 10 nm size is produced. The product is used in information ceramic and structural ceramic and as chemical material. The technological process is simple, easy to operate, high in material utilization and low in power consumption, and may be realized in production line.

Description

technical field [0001] The invention belongs to the technical field of chemical raw material preparation, and in particular relates to a method for preparing zirconium dioxide nanometer powder by a two-liquid phase hydrolysis method. Background technique [0002] Zirconia ceramics have excellent heat resistance, corrosion resistance and plasticity, and are important basic raw materials in the field of new materials. They are widely used in the manufacture of piezoelectric elements, ceramic capacitors, gas sensors, solid electrolyte batteries, ceramic internal combustion engines, optical glass and Zirconia fiber and catalyst, etc. Zirconia nanopowder is a kind of catalyst carrier with good application prospect. Due to its special interaction with the active phase, its chemical properties are better than those of the classical carrier γ-Al 2 o 3 , Silica gel is more inert, and the catalyst made has outstanding activity and selectivity. The use of high-purity, ultra-fine, un...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G25/02
Inventor 罗天勇梁彤祥李辰砂符晓铭唐春和
Owner TSINGHUA UNIV
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