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A kind of preparation method of core-shell structure zrO2-ceo2 powder

A technology of core-shell structure and powder, which is applied in the field of micro-nano material preparation, can solve the problems of reduced catalytic hydrogen production capacity, difficulty in controlling product morphology, and small specific surface area of ​​products, achieving controllable particle size, low raw material cost, Simple operation effect

Active Publication Date: 2018-09-11
GUILIN UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Usually, ZrO 2 -CeO 2 Catalyst materials are prepared by co-precipitation and sol-gel methods using nitrates and chlorides, but the ZrO prepared by the above methods 2 -CeO 2 The powder is not easy to control the shape of the product, and it is easy to agglomerate, and the specific surface area of ​​the product is small, resulting in a decrease in the ability of catalytic hydrogen production

Method used

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  • A kind of preparation method of core-shell structure zrO2-ceo2 powder
  • A kind of preparation method of core-shell structure zrO2-ceo2 powder

Examples

Experimental program
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Embodiment 1

[0020] (1) Add 0.2 g of polyvinylpyrrolidone and 0.01 g of citric acid to 20 mL of ethylene glycol, stir for 30 minutes, then add 0.3 mmol of zirconium acetate and 0.7 mmol of cerium acetate, and stir for another 60 minutes to obtain a mixed solution.

[0021] (2) Pour the mixed solution prepared in step (1) into a three-necked flask, transfer the three-necked flask to a heating magnetic stirrer, set the stirring speed to 400 rpm, and the heating rate to 3° C. / min. Raise to 185°C, add 1 mL of ethylenediamine dropwise, and keep warm for 2 hours to obtain a precipitate.

[0022] (3) The precipitate obtained in step (2) was cooled and washed by centrifugation with absolute ethanol for 6 times, and the product after centrifugation was placed in a vacuum drying oven at 80° C. for 8 hours to obtain a precursor product.

[0023] (4) Heat the precursor product prepared in step (3) to 450°C at a rate of 1°C / min in a muffle furnace, keep it warm for 6 hours, and then naturally cool to r...

Embodiment 2

[0025] (1) Add 0.3 g of polyvinylpyrrolidone and 0.05 g of citric acid into 50 mL of glycerol, stir for 60 minutes, then add 0.5 mmol of zirconium acetate and 0.5 mmol of cerium acetate, and stir for another 60 minutes to obtain a mixed solution .

[0026] (2) Pour the mixed solution prepared in step (1) into a three-necked flask, transfer the three-necked flask to a heating magnetic stirrer, set the stirring speed at 350 rpm, and the heating rate at 5° C. / min. Raise to 185°C, add 3 mL of ethylenediamine dropwise, and keep warm for 4 hours to obtain a precipitate.

[0027] (3) The precipitate obtained in step (2) was cooled and washed by centrifugation with absolute ethanol for 6 times, and the product after centrifugation was placed in a vacuum drying oven at 80° C. for 8 hours to obtain a precursor product.

[0028] (4) Heat the precursor product prepared in step (3) to 700°C at a rate of 20°C / min in a muffle furnace, keep it warm for 2 hours, and then naturally cool to roo...

Embodiment 3

[0030] (1) Add 0.5 g of polyvinylpyrrolidone and 0.1 g of citric acid into 50 mL of ethylene glycol and 50 mL of glycerol mixture, stir for 90 minutes, then add 0.7 mmol of zirconium nitrate and 0.3 mmol of cerium nitrate, and stir for another 90 minutes, Prepare a mixed solution.

[0031] (2) Pour the mixed solution prepared in step (1) into a three-necked flask, and transfer the three-necked flask to a heating magnetic stirrer, set the stirring speed at 200 rpm, and the heating rate at 5°C / min. Raise to 185°C, add 5 mL of n-butylamine dropwise, and keep warm for 2 hours to obtain a precipitate.

[0032] (3) The precipitate obtained in step (2) was cooled and washed by centrifugation with absolute ethanol for 6 times, and the product after centrifugation was placed in a vacuum drying oven at 80° C. for 8 hours to obtain a precursor product.

[0033] (4) The precursor product prepared in step (3) was heated to 550°C at a rate of 2°C / min in a muffle furnace, kept for 5 hours, ...

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Abstract

The invention discloses a preparation method of core-shell structure ZrO2-CeO2 powder. Add zirconium salt and cerium salt in rated molar amounts to the alcohol solution in which polyvinylpyrrolidone and citric acid are dissolved, stir and dissolve, then transfer the mixture to a three-necked flask, set the stirring speed and heating rate, and raise the reaction temperature After reaching a certain temperature, add an appropriate amount of amine and react at a constant temperature for a period of time. Then remove the heating device to cool the reactants. The cooled products are centrifugally washed and dried to obtain the precursor product. The precursor product is roasted for a certain period of time to obtain the core-shell structure. ZrO2‑CeO2 powder. The advantages of the present invention are: the preparation method of the core-shell structure ZrO2-CeO2 powder is simple, the precursor material used is low in cost, the synthesis speed is fast, and the entire reaction synthesis process can be flexibly controlled to form a specific structure and phase.

Description

technical field [0001] The invention belongs to the technical field of preparation of micro-nano materials. In particular, a core-shell structure ZrO 2 -CeO 2 The preparation method of powder, the prepared ZrO 2 -CeO 2 The powder can be used as catalyst carrier for methanol and ethanol reforming hydrogen production, and can also be used as catalyst material for automobile exhaust. Background technique [0002] Hydrogen is an ideal energy source for human beings. Among many hydrogen production methods, hydrogen production by ethanol steam reforming is a relatively efficient hydrogen production method. In the hydrogen production process of ethanol steam reforming, highly active and stable catalysts are The key material to realize the efficient hydrogen production from ethanol. [0003] Rare earth oxide materials are usually used as supports for alcohol hydrogen conversion catalysts, where CeO 2 It has good oxygen storage-release capacity and is considered to be an excell...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/10
CPCB01J23/10B01J37/031B01J37/08B01J35/50
Inventor 郑国源龙飞王吉林姜志强
Owner GUILIN UNIVERSITY OF TECHNOLOGY
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