Preparation method of cerium-zirconium composite oxide with high oxygen storage capacity
A composite oxide and oxygen storage technology, applied in chemical instruments and methods, catalyst activation/preparation, zirconia, etc. Oxygen storage capacity, saving oxidation time, macropore volume structure and effect of specific surface area
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[0051] The invention provides a method for preparing a cerium-zirconium composite oxide, including the steps of preparing by hydrothermal method, specifically as follows:
[0052] S1, dissolving salts of cerium, zirconium, and rare earth metals respectively, with a total concentration of 20-160g / L;
[0053] S2, add 30% H to the above solution at a molar ratio of hydrogen peroxide to cerium oxide of 1.5-3:1 2 o 2 , stirred and oxidized for 5-35min;
[0054] S3, drop an alkaline precipitating agent, the alkaline precipitating agent is one or more of ammonia water, sodium hydroxide, and amines, preferably ammonia water, and then adjust the pH of the solution to 1.5-2;
[0055] S4, introducing the above solution into a high-pressure reactor, and performing a high-temperature hydrolysis reaction at 120-220° C. for 10-20 hours;
[0056] S5, adding an alkaline precipitant dropwise to the precursor slurry obtained in S3 to adjust the pH to 8-10;
[0057] S6, introducing the precur...
Embodiment 1
[0061] Example 1 provides a cerium-zirconium composite oxide, which is prepared by the following method:
[0062] Take 527.1g of zirconium nitrate, dissolve it with 2000ml of deionized water until it becomes clear, take another 32.1g of yttrium oxide, dissolve it with 82.0g of concentrated nitric acid and mix it with the above solution, then add 159.2g of ammonium cerium nitrate and 23.4g of lanthanum nitrate, and stir until it becomes clear , to obtain solution A, then add 30% H to solution A in the ratio of 2:1 with the molar ratio of hydrogen peroxide and cerium oxide in the obtained composite oxide 2 o 2 , stirred and oxidized for 5 minutes;
[0063] Adjust the pH of the oxidized solution A to 1.5-2 with ammonia water in a 50°C water bath, set the volume to 6400ml, and introduce it into a polytetrafluoroethylene-lined pressure melting bomb. Adjust the pH to about 9.5 with ammonia water to obtain slurry B;
[0064] The slurry B was transferred to a titanium kettle, and s...
Embodiment 2-4
[0067] Embodiment 2-4 is prepared according to the preparation method of embodiment 1 and obtains cerium-zirconium composite oxide (composition is: CeO 2 20%, ZrO 2 65%, La 2 o 3 3.5%, Y 2 o 3 12.5%), the difference is only that in the preparation process, the time for adding 30% hydrogen peroxide to stir and oxidize is different in the mixed salt solution of cerium, zirconium and rare earth metals, and the oxidation time of embodiment 2-4 is respectively 10min, 15min, 20min.
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