A method for preparing nano-zirconia by gel-hydrothermal process
A technology of nano-zirconia and zirconium oxychloride, which is applied in the direction of nanotechnology, energy wastewater treatment, etc., can solve the problems of long time consumption, low crystallinity, high specific surface area, etc. The effect of surface area
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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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