Method for preparing large-specific-surface-area rare earth oxides or composite oxides through spray pyrolysis

A technology of rare earth oxide and large specific surface area, which is applied in the field of materials, can solve the problems of narrow size distribution, reduce the preparation temperature and time, and achieve the effects of simple operation and low cost

Active Publication Date: 2016-08-31
连云港高品再生资源有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After decades of development, the spray pyrolysis method has become an important micropowder preparation process. At present, there are many patents (CN201010534886.X, CN201010534886.X, CN201210081225.5, CN201210190297.3, CN201410741766, CN201510311060) reported using this method The method can prepare rare earth oxides or composite oxides with small particle size, narrow size distribution, purity greater than 99%, and uniform composition distribution, but for the preparation of specific surface area exceeding 80m 2 .g -1 However, there are few reports on rare earth oxides or composite oxides. Such rare earth oxides or composite oxides with large specific surface area have important applications in the preparation of three-way catalysts (TWCs) for automobile exhaust purification, which can improve the oxygen storage capacity of catalysts. The role of capacity, catalyst activity and stability

Method used

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  • Method for preparing large-specific-surface-area rare earth oxides or composite oxides through spray pyrolysis
  • Method for preparing large-specific-surface-area rare earth oxides or composite oxides through spray pyrolysis
  • Method for preparing large-specific-surface-area rare earth oxides or composite oxides through spray pyrolysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] The method for preparing cerium oxide by spray pyrolysis, the process steps are: dissolving cerium chloride in water to make a solution with a concentration of 350g / L, adding citric acid and stirring evenly, wherein the amount of citric acid is determined by the molar ratio of citric acid to cerium ions The ratio is 3:1; with air as the carrier gas, the mixed solution is sprayed into the roasting furnace for roasting, the air flow rate is 122L / h, the roasting temperature is 600°C, the residence time of the particles in the pyrolysis furnace is 0.6s, and the roasting produces A carbon-supported cerium oxide precursor; the carbon-supported cerium oxide precursor was calcined at 500° C. for 2.5 hours to obtain a cerium oxide solid.

[0039] The hydrochloric acid gas produced by roasting enters the tail gas absorption tower for recovery and reuse.

[0040] Experimental results: figure 1 The XRD pattern of the carbon-supported cerium oxide precursor is provided, showing tha...

Embodiment 2

[0042] The method for preparing cerium oxide by spray pyrolysis, the process steps are: dissolving cerium chloride in water to make a solution with a concentration of 10g / L, adding lactic acid and stirring evenly, wherein the consumption of lactic acid is 1.5 with the molar ratio of lactic acid and cerium ion: 1 meter; the mixed solution is sprayed into the roasting furnace with air as the carrier gas for roasting, wherein the air flow rate is 140L / h, the roasting temperature is 400°C, the residence time of the particles in the pyrolysis furnace is 2.5s, and the roasting generates carbon-loaded oxidation Cerium precursor: calcining the carbon-supported cerium oxide precursor at 600° C. for 2 hours to obtain a cerium oxide solid.

[0043] The hydrochloric acid gas produced by roasting enters the tail gas absorption tower for recovery and reuse.

[0044] Experimental results: Figure 4The XRD pattern of the carbon-supported cerium oxide precursor is provided, showing that the p...

Embodiment 3

[0046] The method for preparing cerium oxide by spray pyrolysis, the process steps are: dissolving cerium chloride in water to make a solution with a concentration of 100g / L, adding tartaric acid and stirring evenly, wherein the consumption of tartaric acid is 2 with the mol ratio of tartaric acid and cerium ion: 1 meter; the mixed solution is sprayed into the roasting furnace with air as the carrier gas for roasting, wherein the air flow rate is 100L / h, the roasting temperature is 500°C, the residence time of the particles in the pyrolysis furnace is 1.6s, and the roasting generates carbon-loaded oxidation Cerium precursor: Calcining the carbon-supported cerium oxide precursor at 600° C. for 3 hours to obtain a cerium oxide solid.

[0047] The hydrochloric acid gas produced by roasting enters the tail gas absorption tower for recovery and reuse.

[0048] Experimental results: Figure 7 The XRD pattern of the carbon-supported cerium oxide precursor is provided, showing that t...

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Abstract

The invention provides a method for preparing large-specific-surface-area rare earth oxides or composite oxides through spray pyrolysis. The method includes dissolving rare-earth chlorides, or the rare-earth chlorides and metal chlorides, in water to obtain a solution, and adding carboxylic acid for evenly stirring; spraying the mixed solution into a calcinator for calcination by taking the air as a carrier gas at the temperature of 400-1700 DEG C and keeping particles in a pyrolyzing furnace for 0.5-2.5 seconds to obtain carbon loaded rare earth oxide precursors; calcinating the precursors at the temperature of 500-1000 DEG C for 1-10 hours to obtain the rare earth oxides or composite oxides with the specific surface area of 26-83m<2>.g<-1>. The method has the advantages that the rare-earth chlorides, or the rare-earth chlorides and the metal chlorides, serve as raw materials, the carboxylic acid is added, the carbon loaded rare earth oxide precursors in a micro crystalline state or in a micro-crystalline and amorphous mixed solid solution state are obtained through spray pyrolysis, and further, the large-specific-surface-area rare earth oxides or composite oxides are calcinated.

Description

technical field [0001] The invention belongs to the technical field of materials, in particular to a method for preparing rare earth oxides or composite oxides with large specific surface area by spray pyrolysis. Background technique [0002] In recent years, rare earth oxides or composite oxides have been widely used in the fields of catalysts, functional ceramics, oxygen ion conductors, and solid fuel cells. Experiments have confirmed that rare earth oxides or composite oxides have unique crystal structures, electromagnetic properties, and high oxidation and reduction catalytic activities. Their preparation methods and applications have become a hot topic in the fields of catalytic materials, functional materials, etc. Preparation methods of rare earth oxides or composite oxides with physical and chemical properties, such as preparation of rare earth oxides and rare earth composite powders with different particle sizes and specific surface areas. [0003] At present, the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00
CPCC01F17/00C01F17/206C01P2002/72C01P2004/03C01P2004/04C01P2006/12
Inventor 吴文远王振峰边雪岑鹏
Owner 连云港高品再生资源有限公司
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