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Method for preparing nano zirconium oxide by gel-hydrothermal process

A nano-zirconia, zirconium oxychloride technology, applied in nanotechnology, energy and wastewater treatment, etc., can solve the problems of high specific surface area, long time, low crystallinity, etc.

Active Publication Date: 2020-10-27
宁德三祥纳米新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a method for preparing nano-zirconia by gel-hydrothermal process, which overcomes the problems of high specific surface area, low crystallinity and long time-consuming in the preparation of zirconia powder by traditional simple hydrothermal method. question

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  • Method for preparing nano zirconium oxide by gel-hydrothermal process

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Experimental program
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Effect test

Embodiment 1

[0032] Take 2mol / L zirconium oxychloride solution (according to the 3Y ratio, the molar ratio of zirconium to yttrium is 97:6) and 2mol / L ammonia solution, drop the ammonia water into the stirred zirconium oxychloride solution until pH =9, obtain precipitate 400g and filter out and wash several times (until the silver nitrate solution of 0.1mol / L detects no chloride ions until the washing liquid); mix the precipitate with 100ml distilled water, 20g acrylamide (AM), 1g N , N'-methylenebisacrylamide, 1ml tetramethylethylenediamine, mixed and stirred evenly; drop 1-2 drops of ammonium persulfate into the mixed slurry, then heat the slurry to 70°C, and let it stand for 10min , to obtain a gel of zirconium hydroxide; place the gel in a reaction kettle, heat it up to 300°C at a rate of 4°C / min after airtight, and keep it warm for 4 hours; then take out the product, filter it, wash it several times, and dry it After calcining for 2 hours, nanometer zirconia can be obtained. X-ray di...

Embodiment 2

[0034] Take 2mol / L zirconium oxychloride solution (according to the 3Y ratio, the molar ratio of zirconium to yttrium is 97:6) and 1mol / L ammonia solution, drop the ammonia solution into the stirred zirconium oxychloride solution until pH =9, obtain precipitate 400g and filter out and wash several times (until the silver nitrate solution of 0.1mol / L detects no chloride ions until the washing liquid); mix the precipitate with 100ml distilled water, 20g acrylamide (AM), 1g N , N'-methylenebisacrylamide, 1ml tetramethylethylenediamine, mixed and stirred evenly; drop 1-2 drops of ammonium persulfate into the mixed slurry, then heat the slurry to 70°C, and let it stand for 10min , to obtain a gel of zirconium hydroxide; place the gel in a reaction kettle, heat it up to 300°C at a rate of 4°C / min after airtight, and keep it warm for 4 hours; then take out the product, filter it, wash it several times, and dry it After calcining for 2 hours, nanometer zirconia can be obtained. X-ray...

Embodiment 3

[0036] A method for preparing nano-zirconia by gel-hydrothermal process, comprising the following steps:

[0037] Step 1: mix zirconium oxychloride and yttrium nitrate, and prepare 1.0mol / L reaction solution A with distilled water; the molar ratio of zirconium oxychloride and yttrium nitrate is 97:6;

[0038] Step 2: In the state of stirring, drop 1.0 mol / L ammonia water into the reaction solution A until the pH=9;

[0039] Step 3: the precipitate in the reaction solution A is filtered and washed several times until no chloride ions are detected in the washing solution with a 0.1mol / L silver nitrate solution;

[0040]Step 4: Weigh the precursor zirconium hydroxide monohydrate with a mass of M1, distilled water with a mass of M2, acrylamide with a mass of M3, and N, N'-methylenebisacrylamide with a mass of M4, and add Tetramethylethylenediamine solution, mixed and stirred evenly, then ammonium persulfate was added dropwise, heated to 70-90°C, and left to stand for 10 minutes t...

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Abstract

The invention relates to the technical field of nano zirconium oxide preparation, in particular to a method for preparing nano zirconium oxide through a gel-hydrothermal process. The preparation method comprises the following steps: washing and filtering a precursor produced by reaction of zirconium oxychloride and ammonia water for multiple times, then uniformly mixing and stirring a monomer, a cross-linking agent and the like with zirconium hydroxide and distilled water, and adding an initiator to prepare zirconium hydroxide gel; putting the gel into a closed reaction kettle, raising the temperature in a closed manner, separating out zirconium oxide crystal grains along with the temperature rise, and decomposing organic matters; and carrying out solid-liquid separation on the product, drying and calcining to obtain the nano zirconium oxide product. According to the method, the advantages of a gel method and a hydrothermal method are combined, the problems of large specific surface area and low cleanliness caused by a pure hydrothermal method are solved, and the problem that a traditional gel method consumes too long time is also solved.

Description

technical field [0001] The invention relates to the technical field of nano-zirconia preparation, in particular to a method for preparing nano-zirconia by a gel-hydrothermal process. Background technique [0002] Nanocomposite zirconia ceramics is a new material with the best mechanical properties among high-tech ceramics. Because zirconia ceramics have high toughness, bending strength and wear resistance, excellent heat insulation performance, and thermal expansion coefficient close to metal, etc., It is the basic raw material for making high-end zirconia special ceramics, photoelectric communication devices, new energy materials, and ceramic materials for 3D printing. It is widely used in optical fiber inserts, dental materials, oxygen sensors, fuel cells, ceramic cutting tools, grinding media, and thermal barriers. Coating and other fields are irreplaceable raw materials for special ceramics. [0003] High-performance zirconia ceramics have higher and higher requirements...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/486C04B35/624C04B35/626B82Y40/00
CPCC04B35/486C04B35/624C04B35/626B82Y40/00C04B2235/3225Y02W10/37
Inventor 周志永骆兵姜波
Owner 宁德三祥纳米新材料有限公司