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.
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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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