CN101983925B - Preparation method of cerium oxide powder - Google Patents
Preparation method of cerium oxide powder Download PDFInfo
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- CN101983925B CN101983925B CN201010534886XA CN201010534886A CN101983925B CN 101983925 B CN101983925 B CN 101983925B CN 201010534886X A CN201010534886X A CN 201010534886XA CN 201010534886 A CN201010534886 A CN 201010534886A CN 101983925 B CN101983925 B CN 101983925B
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Abstract
The invention belongs to the field of rare earth metallurgy and relates to a preparation method of cerium oxide powder. The key points are as follows: taking cerium chloride solution of 10g/L-300g/L within the temperature range of 500-1000 DEG C as raw material, and baking in a baking furnace for 10-40min; cooling baking residue, and preparing a cerium oxide powder product; and carrying out dust removal and absorption on furnace gas for preparing a concentrated hydrochloric acid product. The technological process can lead the conversion rate of cerium to be more than 99%, and lead the content of cerium oxide in the obtained cerium oxide powder to be greater than 99% by weight; and the process has low production cost, high yield, good product quality, no carbon emission during the production process, no pollution, recyclable chlorine and convenient realization of continuous and automated production.
Description
Technical field
The invention belongs to the rare earth metallurgy field, be specifically related to a kind of preparation method of cerium oxide powder.
Background technology
Along with science and technology development, obtained application more and more widely as the rare earth oxide of one of base mateiral of preparation novel material.Rare earth oxide is modal intermediates in the Rare Earth Production, can be further used for producing rare earth metal, alloy and functional materials etc.And the preparation of rare earth oxide develops towards the direction with specific physical chemical property.As require to prepare rare earth oxide and RE composite powder of different-grain diameter, different specific surface areas etc.
Rare earth metal in air oxidation or in air the oxyhydroxide of calcination rare earth and the rare earth salts (as: oxalate, carbonate, nitrate salt, vitriol etc.) that contains the volatility acid group just can obtain rare earth oxide.General sesquioxide (the RE that forms
2O
3), cerium forms CeO
2, praseodymium forms Pr
6O
11(Pr
2O
34PrO
2), terbium forms Tb
4O
7(Tb
2O
32TbO
2).The industrial method that generally is used in calcination rare earth carbonate in the air or rare-earth oxalate prepares rare earth oxide.
The technology that oxalate precipitation method or carbon ammonium precipitation method prepare rare earth oxide is disclosed in 173 pages of " rare earth metallurgy " that Chemical Industry Press publishes.Wherein the oxalate precipitation method is: will contain the rare-earth chloride solution of 20 ~ 100g/L, regulating pH is about 2 ~ 3, is heated to 80 ~ 90 ℃ then, under agitation condition, adds solid oxalic acid and precipitates.The consumption of oxalic acid is 1.2 ~ 1.4 times of rare-earth oxidation amount, precipitates after 30 minutes, filters and obtains rare earth oxalate, and rare earth oxalate was obtained rare earth oxide in 2 hours 800 ~ 900 ℃ of following calcinations.And this rare earth oxide promptly can be used as commodity selling.It should be noted that oxalic acid has certain toxicity, and it is present in the waste water contaminate environment.Simultaneously no matter oxalate precipitation method or carbon ammonium precipitation method will discharges a large amount of carbonic acid gas in the calcination rare-earth precipitation process, and this makes the carbon emission amount increase of enterprise.In addition, contain a large amount of chlorine roots in the filtrating of this method post precipitation, can't obtain utilizing, also can cause environmental pollution.
One Chinese patent application; Application number is 200410036484.1 to disclose a kind of method for preparing rare earth oxide; This method prepares in the rare earth oxide process for solving oxalate precipitation method or carbon ammonium precipitation method; Labour intensity is big, equipment loss is big, seriously polluted, decompose unbalanced, consistence difference and influence problem such as quality product, proposed a kind ofly can implement calcination decomposition rare earth carbonate continuously or oxalate prepares the technical scheme of rare earth oxide, and designed calcination equipment.This technology can reduce labor intensity, enhances productivity, improve the quality of products.Yet this technology still adopts oxalic acid or carbon ammonium precipitation rare earth, and this can't be avoided the discharging of carbon in the calcination process and the pollution of environment.
Summary of the invention
To the problem that above-mentioned prior art exists, the present invention provides a kind of preparation method of cerium oxide powder, when realizing the cerium high conversion, has reduced carbon emission, reclaims the chlorine resource, has reduced the pollution to environment.
The technical scheme that realizes the object of the invention is:
At first with roasting furnace temperature elevation to 500 ~ 1000 ℃, preheating 10 minutes; Be 10 ~ 300g/L with concentration then, the solution of cerium chloride by oxidation of quality purity more than 99% and sprays in the stoving oven after carrier gas mixes; Roasting 10 ~ 40 minutes; Furnace gas after the roasting through dedusting with separate, the roasting slag after the separation is through naturally cooling, obtains the cerium oxide powder of cerium oxide content greater than 99wt%; Furnace gas after the separation makes hydrochloric acid after absorbing.
Described carrier gas is selected pressurized air or compressed nitrogen for use, and flow velocity is 2 liters/hour;
Granularity < the 0.22mm of described cerium oxide powder;
The concentration of described hydrochloric acid is 80 ~ 200g/L.
Compared with prior art, characteristics of the present invention and beneficial effect thereof are:
Because it is raw material that the present invention adopts Cerium II Chloride, so does not adopt carbon ammonium and virose oxalic acid in the production process, does not produce in the traditional technology and in the calcination process, discharges carbonic acid gas, greatly reduces the pollution to environment;
The chlorine that produces in the technical process of the present invention reclaims and makes hydrochloric acid, not only protects environment but also increase economic benefit;
The present invention has increased substantially the transformation efficiency of cerium, can reach more than 99%.
Embodiment
Below in conjunction with embodiment the present invention is elaborated, but protection scope of the present invention is not limited only to following embodiment:
The stoving oven that following examples adopt; Its structure is: body of heater is a cylinder shape, and outer wall is a stainless steel, and inwall is the aluminum oxide material; Lagging material is installed on the inwall; Body of heater inner chamber top liquor inlet is connected with a shower nozzle, and a material outlet is arranged at sidewall of the furnace body top, and a fuel gas inlet is arranged at the sidewall of the furnace body bottom;
Dedusting of the present invention separates adopts cyclonic separator, and its model is CZT-3.9;
Tail gas of the present invention absorbs and adopts the absorption tower, and its model is M215780.
Embodiment 1: at first with roasting furnace temperature elevation to 500 ℃, and preheating 10 minutes; Be the solution of cerium chloride by oxidation 500ml of 10g/L then with concentration; With flow velocity is that 2 liters/hour carrier of compressed air is mixed, and through the stoving oven shower nozzle, sprays in the stoving oven; After the roasting 40 minutes, the material outlet that makes the roasting slag that contains furnace gas pass through sidewall of the furnace body top gets into cyclonic separator; The roasting slag that separation obtains obtains the cerium oxide powder of cerium oxide content 99.2wt% through naturally cooling, and granularity is 0.12mm; After will feeding the tail gas absorber absorption through cyclonic separator separation and dust separating furnace gas, make the hydrochloric acid that concentration is 80g/L.
Embodiment 2: at first with roasting furnace temperature elevation to 800 ℃, and preheating 10 minutes; Be the solution of cerium chloride by oxidation 530ml of 150g/L then with concentration; With flow velocity is that 2 liters/hour carrier of compressed air is mixed, and through the stoving oven shower nozzle, sprays in the stoving oven; After the roasting 20 minutes, the material outlet that makes the roasting slag that contains furnace gas pass through sidewall of the furnace body top gets into cyclonic separator; The roasting slag that separation obtains obtains the cerium oxide powder of cerium oxide content 99.5wt% through naturally cooling, and granularity is 0.18mm; After will feeding the tail gas absorber absorption through cyclonic separator separation and dust separating furnace gas, make the hydrochloric acid that concentration is 100g/L.
Embodiment 3: at first with roasting furnace temperature elevation to 1000 ℃, and preheating 10 minutes; Be the solution of cerium chloride by oxidation 100ml of 300g/L then with concentration; With flow velocity is that 2 liters/hour carrier of compressed air is mixed, and through the stoving oven shower nozzle, sprays in the stoving oven; After the roasting 10 minutes, the material outlet that makes the roasting slag that contains furnace gas pass through sidewall of the furnace body top gets into cyclonic separator; The roasting slag that separation obtains obtains the cerium oxide powder of cerium oxide content 99.3wt% through naturally cooling, and granularity is 0.22mm; After will feeding the tail gas absorber absorption through cyclonic separator separation and dust separating furnace gas, make the hydrochloric acid that concentration is 200g/L.
Claims (2)
1. the preparation method of a cerium oxide powder is characterized in that carrying out as follows: at first with roasting furnace temperature elevation to 500～1000 ℃, and preheating 10 minutes; Be 10～300g/L with concentration then, the solution of cerium chloride by oxidation of quality purity more than 99% and sprays in the stoving oven after pressurized air or compressed nitrogen mix; Gas flow rate is 2 liters/hour; Roasting 10～40 minutes, the furnace gas after the roasting through dedusting with separate, the roasting slag after the separation is through naturally cooling; Obtain cerium oxide content greater than 99wt%, the granularity < cerium oxide powder of 0.22mm; Furnace gas after the separation makes hydrochloric acid after absorbing.
2. the preparation method of a kind of cerium oxide powder according to claim 1, the concentration of hydrochloric acid that it is characterized in that said acquisition is 80～200g/L.
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|---|---|---|---|
| CN201010534886XA CN101983925B (en) | 2010-11-08 | 2010-11-08 | Preparation method of cerium oxide powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010534886XA CN101983925B (en) | 2010-11-08 | 2010-11-08 | Preparation method of cerium oxide powder |
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| CN101983925A CN101983925A (en) | 2011-03-09 |
| CN101983925B true CN101983925B (en) | 2012-07-18 |
Family
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|---|---|---|---|
| CN201010534886XA Active CN101983925B (en) | 2010-11-08 | 2010-11-08 | Preparation method of cerium oxide powder |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102616826B (en) * | 2012-03-26 | 2013-11-27 | 东北大学 | Pyrolysis method for preparing trivalent rare earth oxide |
| CN102701260B (en) * | 2012-06-11 | 2014-01-08 | 东北大学 | Spray pyrolysis method for aid-containing rare earth chloride solution |
| JP5943529B2 (en) * | 2012-09-13 | 2016-07-05 | エルジー・ケム・リミテッド | Recycling method of waste abrasive containing ceria |
| CN103318939A (en) * | 2013-06-20 | 2013-09-25 | 东北大学 | Method for preparing solid spherical rare earth oxide in one-step spraying thermal decomposition mode |
| CN104449401B (en) * | 2014-12-09 | 2016-07-27 | 东北大学 | A kind of spray-wall interaction prepares method and the device of cerium-based rare earth polishing powder |
| CN105271351B (en) * | 2015-10-27 | 2017-04-12 | 昆明理工大学 | Method for preparing cerium oxide with rare earth cerium chloride |
| CN113800551A (en) * | 2021-10-27 | 2021-12-17 | 福建省长汀金龙稀土有限公司 | Method for preparing rare earth oxide powder by utilizing steam roasting of rare earth chloride |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201530727U (en) * | 2009-10-16 | 2010-07-21 | 马科伟 | Device for directly generating cerium oxide powder by pyrolysis of cerium chloride solution |
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2010
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201530727U (en) * | 2009-10-16 | 2010-07-21 | 马科伟 | Device for directly generating cerium oxide powder by pyrolysis of cerium chloride solution |
Non-Patent Citations (1)
| Title |
|---|
| 李启厚等.喷雾热分解法制备超细粉体材料的特点及应用.《湿法冶金》.2008,第27卷(第4期),第220-224页. * |
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| CN101983925A (en) | 2011-03-09 |
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Effective date of registration: 20191010 Address after: 8 niutao Road, small and medium sized enterprise park, Shihu Township, Donghai County, Lianyungang City, Jiangsu Province Patentee after: Lianyungang High-quality Renewable Resources Co., Ltd. Address before: 110819 Heping Road, Heping District, Liaoning, Shenyang, Lane No. 11, No. 3 Patentee before: Northeast University |