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Cerium oxide-zirconium oxide based composite rare-earth oxide with high specific surface area and high oxygen storage capacity and preparation method thereof

A technology based on rare earth oxides and zirconia, which is applied in the direction of rare earth metal compounds, catalyst activation/preparation, zirconia, etc., can solve the problems of phase separation and unstable texture performance, catalyst performance degradation, and insufficient specific surface area. Achieve the effect of high fresh specific surface area, large total pore volume and concentrated distribution

Active Publication Date: 2013-07-10
CHAOZHOU THREE CIRCLE GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The cerium-zirconium catalyst prepared by the traditional method can maintain good oxygen storage performance at high temperature, which can meet the requirements of high-performance automobile exhaust purification three-way catalyst for oxygen storage performance and high-temperature stability of oxygen storage materials, but the cerium-zirconium solid solution can The thermal stability of the lower structure is poor, and the specific surface area is relatively small
As reported, after the prepared cerium-zirconium oxygen storage material is calcined at 1000°C for 4 hours, the oxygen storage capacity at 200°C can still reach more than 300 μmol / g, but the specific surface area is less than 10g / m 2
The three-way catalyst must have strong durability at high space velocity, and traditional cerium-zirconium materials dissociate tetragonal ZrO at higher temperatures 2 , so that the single cubic phase transforms into multi-phase coexistence, phase separation and instability of texture properties will lead to a serious decline in catalyst performance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A method for preparing a ceria-zirconia-based composite rare earth oxide, the method comprising the following steps:

[0028] (1) Heat 25wt% zirconium oxychloride solution at room temperature, add 10wt% sodium sulfate solution at a rate of 5ml / min, control the heating rate, so that the temperature rises to 95°C when sodium sulfate is added, and then keep it warm for 60min to form basic sulfuric acid A zirconium composite salt precursor, wherein the quality of sulfate ions accounts for 30% of the quality of zirconium oxychloride;

[0029] (2) adding 20wt% cerium nitrate solution and 20wt% lanthanum nitrate solution into the basic zirconium sulfate compound salt precursor solution obtained in step (1), stirring evenly to obtain a slurry;

[0030] (3) Precipitate the slurry obtained in step (2) with 400 g of basic sodium carbonate solution to obtain a precipitate, wherein the sodium hydroxide content in the basic sodium carbonate solution is 80 g, and the sodium carbonate ...

Embodiment 2

[0035] A method for preparing a ceria-zirconia-based composite rare earth oxide, the method comprising the following steps:

[0036] (1) Heat 20wt% zirconium nitrate solution at room temperature, add 15wt% potassium sulfate solution at a rate of 5ml / min, control the heating rate, so that the temperature rises to 90°C when potassium sulfate is added, and then keep it warm for 100min to form a basic zirconium sulfate compound Salt precursor, wherein, the quality of sulfate ion accounts for 45% of zirconium nitrate quality;

[0037] (2) Add 25wt% cerium chloride solution and 25wt% scandium nitrate solution to the basic zirconium sulfate compound salt precursor solution obtained in step (1), and stir evenly to obtain a slurry;

[0038] (3) Precipitate the slurry obtained in step (2) with 450 g of basic sodium oxalate solution to obtain a precipitate, wherein the ammonia water content in the basic sodium oxalate solution is 100 g, and the sodium oxalate content is 20 g;

[0039] (...

Embodiment 3

[0043] A method for preparing a ceria-zirconia-based composite rare earth oxide, the method comprising the following steps:

[0044] (1) Heat 25wt% zirconium oxalate solution at room temperature, add 10wt% ammonium sulfate solution at a speed of 4ml / min, control the heating rate, so that the temperature rises to 92°C when the ammonium sulfate is added, and then keep it warm for 20min to form a basic zirconium sulfate compound Salt precursor, wherein, the mass of sulfate ion accounts for 60% of the mass of zirconium oxalate;

[0045] (2) adding 20wt% cerium carbonate solution and 20wt% yttrium nitrate solution into the basic zirconium sulfate compound salt precursor solution obtained in step (1), stirring evenly to obtain a slurry;

[0046] (3) Precipitate the slurry obtained in step (2) with 200 g of basic sodium carbonate solution and 200 g of basic sodium oxalate solution to obtain a precipitate, wherein the content of sodium hydroxide in the basic sodium carbonate solution ...

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Abstract

The invention discloses a method for preparing a cerium oxide-zirconium oxide based composite rare-earth oxide. The method comprises the following steps of: (1) heating a zirconium salt solution at room temperature, slowly adding sulfate ions, controlling the temperature rise rate so that the temperature is increased in the range of 90-95 DEG C when the sulfate ions are added completely, and then preserving heat for 20-100 minutes, thereby forming a zirconium basic sulfate composite salt precursor; (2) adding a cerium salt and a rare-earth metal salt to the precursor solution and stirring evenly, thereby obtaining a slurry; (3) settling the slurry by using basic carbonate and / or a basic oxalate solution, thereby obtaining a precipitate; and (4) filtering and washing the precipitate obtained in the step (3), removing purities, and calcining the washed precipitate. The cerium oxide-zirconium oxide based composite rare-earth oxide prepared by the method by controlling raw materials and process conditions has the characteristics of being high in total fine pore volume, high in fresh specific surface area, high in oxygen storage capacity and the like.

Description

technical field [0001] The invention relates to a ceria-zirconia-based composite rare earth oxide and a preparation method thereof, in particular to a ceria-zirconia-based composite rare-earth oxide with high specific surface area and high oxygen storage capacity and a preparation method thereof. Background technique [0002] Because the tail gas emissions of automobiles, motorcycles and tractors, especially motor vehicles such as automobiles, have become the main source of air pollution in large and medium-sized cities in the world, and the most effective measure to control motor vehicle exhaust emissions is to install off-board vehicle exhaust purifiers. As the activated carbon layer of the carrier of the automobile exhaust purifier, the cerium-composite material has become an indispensable material for the automobile catalyst. The cerium-composite material has good oxygen storage capacity and high-temperature hydrothermal stability, which can effectively widen the air-fue...

Claims

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Application Information

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IPC IPC(8): B01J23/10B01D53/94
CPCB01J23/10C01G25/02B01J37/031B01J37/0036C01P2002/50C01P2004/82C01P2006/12C01P2006/14C01P2006/90C01G25/06C01F17/32B01J35/40B01J35/613B01J35/635B01J35/66
Inventor 黄壮昌郭喜斌
Owner CHAOZHOU THREE CIRCLE GRP
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