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Nanometer ceria-zirconium solid solution and preparation method thereof

A cerium zirconium solid solution and nanotechnology, applied in the field of solid solution and its preparation, can solve the problems of requiring high pressure equipment, inability to mix uniformly, and not suitable for large-scale production, etc.

Active Publication Date: 2012-07-18
方复(上海)新材料科技有限公司
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Problems solved by technology

[0007] The invention patent of Chinese patent No. CN1552517A discloses the preparation method of nano-scale cerium-zirconium rare earth composite oxide solid solution-based catalyst. After the cerium-zirconium mixed solution is neutralized and precipitated by alkaline substances, it is filtered, washed, added deionized water, and placed in Hydrothermal reaction in an autoclave, filtration, and supercritical drying with ethanol to obtain a solid solution with small grains, uniform distribution, and good thermal stability. Calcined at 1000°C for 6 hours, the specific surface is 45-50m 2 / g, but the manufacturing cost of this method is too high to be suitable for mass production
[0011] The invention patent of Chinese patent No. CN101637721B discloses a porous yttrium cerium zirconium solid solution and its preparation method, the invention is by adding protective agent, mixed rare earth metal salt solution and active polystyrene microsphere emulsion, normal temperature precipitation, 80-100 Aging at ℃, collecting the precipitate, washing with water, drying, and roasting to obtain the target product. In this invention, the polystyrene microsphere emulsion and the metal salt solution cannot be mixed evenly, which easily leads to poor uniformity and stability of the product
[0012] The invention patent of Chinese patent No. CN100496745C has announced a kind of linear or rod-shaped polycrystalline Ce0.6Zr0.3Y0.1O2 Solid solution preparation method, this patent is by adding cetyltrimethylammonium bromide as surfactant, through The precursor is obtained by hydrothermal treatment, and the target product is obtained by burning. This invention patent requires high-pressure equipment through hydrothermal treatment, which is not conducive to industrial production.

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  • Nanometer ceria-zirconium solid solution and preparation method thereof

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preparation example Construction

[0037] On the other hand, the preparation method of nanometer cerium-zirconium solid solution of the present invention, it comprises the steps:

[0038] (1) Preparation of acidic solution A: dissolving zirconium carbonate with concentrated nitric acid, adding cerium nitrate and other mixed rare earth nitrates according to the composition of cerium-zirconium solid solution, dissolving, then adding structure-directing agent, and aging;

[0039] (2) Preparation of alkaline solution B: get an appropriate amount of concentrated ammonia or ammonium bicarbonate to be mixed with alkaline solution B at a concentration of 4mol / L;

[0040] (3) Precipitation reaction: add the acidic solution A into the alkaline solution B at a certain speed to generate a precipitate, add metered hydrogen peroxide, and then age for a certain period of time to obtain a solid-liquid mixed system C;

[0041] (4) Washing: dehydrating the solid-liquid mixed system C, rinsing, and filtering to obtain wet cake D;...

Embodiment 1

[0050] Dissolve 150kg of zirconium carbonate with 100Kg of nitric acid, add 76.0kg of cerium nitrate, 13.3Kg of lanthanum nitrate, and 17.0Kg of yttrium nitrate, stir and dissolve, then add 6Kg of cetyltrimethylammonium bromide, add pure Water to 500L, aged at 80°C for 4h to obtain acidic solution A.

[0051] Dilute 400Kg of ammonia water and pure water to 1200L, and keep it at 70°C for 1 hour to obtain alkaline solution B.

[0052] Under stirring, add the above-mentioned acidic solution to the alkaline solution B at a rate of 5 L / min to obtain a gray precipitated solid-liquid system, control the pH value of the end point to 9, add 14.8Kg of 30% hydrogen peroxide, and then Aging 4h. Obtain solid-liquid mixed system C. Filter, rinse with 600Kg hot water, and filter. Get wet cake D.

[0053] The wet cake D and water were repulped at a mass ratio of 2:1, 80Kg of lauric acid was added, and the slurry E was obtained by shearing and dispersing. The slurry E was calcined at 750°...

Embodiment 2

[0056] Dissolve 150kg of zirconium carbonate with 100Kg of nitric acid, add 76.0kg of cerium nitrate, 13.3Kg of lanthanum nitrate, and 13.1Kg of neodymium nitrate, stir and dissolve, then add 6Kg of cetyltrimethylammonium bromide, add pure Water to 500L. Aged at 75°C for 4h to obtain acidic solution A.

[0057] Dilute 400Kg of ammonia water and pure water to 1200L, and keep it at 70°C for 1 hour to obtain alkaline solution B.

[0058] Under stirring, add the above-mentioned acidic solution to the alkaline solution B at a rate of 5 L / min to obtain a gray precipitated solid-liquid system. Control the pH value of the end point to 10, add 14.8Kg of 30% hydrogen peroxide, and then Aging 4h. Obtain solid-liquid mixed system C. Filter, rinse with 600Kg hot water, and filter. Get wet cake D.

[0059] The wet cake D and water were repulped at a mass ratio of 2:1, 80Kg of lauric acid was added, and the slurry E was obtained by shearing and dispersing. The slurry E was calcined at ...

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Abstract

The invention aims to disclose a nanometer ceria-zirconium solid solution and a preparation method thereof. The nanometer ceria-zirconia solid solution comprises the following components according to weight percent: 15 to 65% of cerium oxide, 12 to 70% of zirconia and 10 to 30% of compound oxide composed of other tombarthite oxide except for ceria and zirconium. Compared with the conventional products, the nanometer ceria-zirconium solid solution obtains larger pore diameter and pore volume through modification of a structural directing agent and a dispersing agent, has a favorable capability of resisting high temperature and ageing, and has the advantages of high oxygen storage capability and high speed in oxygen storage and discharge, so that the purposes of the invention are achieved.

Description

technical field [0001] The invention relates to a solid solution and a preparation method thereof, in particular to a nano-cerium-zirconium solid solution suitable for use as a catalyst carrier and auxiliary agent for exhaust gas purification or catalytic combustion such as motor vehicle exhaust purification catalysts, organic waste gas elimination, and natural gas catalytic combustion. and its preparation method. Background technique [0002] Reducing vehicle exhaust pollution, protecting the quality of the atmospheric environment, and realizing the sustainable development of the ecological environment and society are one of the important issues of my country's environmental protection at present and in the future for a long time. [0003] In order to reduce pollution, breakthroughs must be made in three aspects: improving the quality of gasoline, improving the combustion state of the engine, and increasing the catalytic efficiency of exhaust gas purification. So far, the ...

Claims

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Application Information

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IPC IPC(8): B01J23/10B01J35/10B01D53/94B01D53/86F23G7/07
Inventor 郭昌文赵月昌高玮尹先升赵秀娟贾嘉
Owner 方复(上海)新材料科技有限公司
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