CN1532147A - Process for preparing nano cerium dioxide - Google Patents
Process for preparing nano cerium dioxide Download PDFInfo
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- CN1532147A CN1532147A CNA031072720A CN03107272A CN1532147A CN 1532147 A CN1532147 A CN 1532147A CN A031072720 A CNA031072720 A CN A031072720A CN 03107272 A CN03107272 A CN 03107272A CN 1532147 A CN1532147 A CN 1532147A
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- preparation
- cerium
- gel
- ethanolic soln
- cerous nitrate
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Abstract
The preparation process of nano cerium dioxide with cerium nitrate, cerium dichloride or cerium dioxide as material includes the following steps: converting cerium nitrate, cerium dichloride or cerium dioxide into ethanol solution of concentration 0.20-0.40 mol/L; compounding ammonia water into ethanol solution of concentration 1-3 mol/L as precipitant; dropping the cerium containing ethanol solution into the precipitant to obtain gel at reaction temperature of 25-40 deg.c and pH 9-12; ageing the gel in mother liquid for 12-24 hr, sucking filtering and washing; exchange with absolute ethyl alcohol to eliminate water from gel; drying at 80-120 deg.c for 5-10 hr; and roasting at 400-550 deg.c for 2-5 hr to obtain nano CeO2 particle.
Description
Technical field
The present invention relates to a kind of cerium dioxide (CeO
2) the preparation method, relate in particular to a kind of preparation method of nano ceric oxide.
Background technology
The nano ceric oxide that the present invention proposes is one of important source material of commercial catalysts, vehicle emission pollution cleaning catalyst, electronic industry and high-performance ceramics.
Nano material has the katalysis that is unsurpassed in excellence for most catalyzed reactions, reduce combustion initiation temperature, the quickening rate of catalysis reaction of catalyzed reaction, has fabulous selectivity etc., in the catalytic field application theoretical meaning is arranged not only, with practical value again, for novel, effective catalyst research and development have proposed new preparation thinking.
Nano ceric oxide is used for catalyzer and has peculiar function as effective auxiliary agent, improves the physical strength of support of the catalyst; Improve the stability of catalyzer, play the dual function of stablizing crystalline structure and stoping volumetric shrinkage; The more important thing is that cerium has appraising at the current rate of form, CeO
2Have oxidation, restoring function, when causing the instantaneous anoxic of exhaust at the instantaneous rich oil of engine, chemical valence state is quadrivalent cerium (CeO
2) can be transformed into trivalent cerium (Ce
2O
3) and emit oxygen, on the contrary in conjunction with oxygen,
。Here it is, and so-called oxygen stores and release action, and this function is very important in catalyzer uses, and presents the characteristic that conventional catalytic material does not possess, and at the catalysis ambit broad prospect of application is arranged.
Summary of the invention
The object of the present invention is to provide a kind of CeO
2The preparation method, the nano Ce O that the present invention makes
2Particle size is little, and specific surface area is big.The present invention has used the reverse precipitation method, and may command prepares nano Ce O
2Size distribution is in certain scope.
It is raw material that preparation method provided by the invention adopts the solubility cerium, be made into ethanolic soln, and prepare certain density ammoniacal liquor-ethanolic soln as precipitation agent, and will contain the cerium ethanolic soln then and be added drop-wise to and obtain gel in the precipitation agent, obtain nano Ce O through washing, drying and roasting
2Particulate.
It is raw material that the present invention adopts cerous nitrate, cerium dichloride and cerium dioxide, earlier cerous nitrate or cerium dichloride or cerium dioxide is changed into the ethanolic soln of cerous nitrate, and its concentration is 0.20-0.40molL
-1It is 1-3molL that ammoniacal liquor is mixed with its concentration
-1Ethanolic soln as precipitation agent; To contain the cerium ethanolic soln then and be added drop-wise to and obtain gel in the precipitation agent, the temperature of reaction of preparation gel is 25-40 ℃, and pH is 9-12; The gel that obtains in mother liquor ageing 12-24 hour, filtering and washing; For the moisture content in the gel is removed as far as possible, available dehydrated alcohol exchanges, and removes the moisture content in the gel; In 80-120 ℃ of dry 5-10 hour, 400-550 ℃ roasting 2-5 hour, obtain nano Ce O
2Particulate.
Description of drawings
In order further to understand the present invention, elaborate with embodiment below, and drawn accompanying drawing and described the present invention and obtain nano Ce O
2The sign of the feature of particulate, wherein:
Fig. 1 is nano Ce O
2The transmission electron microscope of sample (TEM) photo;
Fig. 2 is nano Ce O
2The selected area electron diffraction photo of sample.
Embodiment
Embodiment 1: raw material is a cerous nitrate, is mixed with 0.25molL
-1Ce (NO
3)
3Ethanolic soln 500ml.Precipitated liquid is ammoniacal liquor 2molL
-1Ethanolic soln 500ml.Under 30 ℃ of powerful agitation conditions, with 0.25molL
-1Ce (NO
3)
3Ethanolic soln 500ml is added drop-wise in the precipitated liquid, and the gel of preparation gained is ageing 18 hours suction filtration then in mother liquor, with deionized water wash 3-5 time, exchanges in the gel moisture content for several times with dehydrated alcohol and removes, and after 120 ℃ of dryings, 500 ℃ of roasting 3h promptly obtain nano Ce O
2Particulate.
Embodiment 2: raw material is that cerium dichloride is mixed with 0.25molL
-1CeCl
2Ethanolic soln 500ml.Under 30 ℃ of powerful agitation conditions, with 0.25molL
-1CeCl
2Ethanolic soln 500ml is added drop-wise in the precipitated liquid, gel ageing in mother liquor of preparation gained, and digestion time 18h is suction filtration then, with deionized water wash 3-5 time, exchange in the gel moisture content for several times with dehydrated alcohol and remove, after 120 ℃ of dryings, 500 ℃ of roasting 3h promptly obtain nano Ce O
2Particulate.
Embodiment 3: raw material be can not be water-soluble CeO
2, need use H
2O
2And HNO
3Dissolving is made into 0.25molL behind the evaporate to dryness
-1Ce (NO
3)
3Ethanolic soln.All the other conditions are with embodiment 1.
Sample X-ray diffraction (XRD) measurement result sees that the sample characteristic diffraction peak that the present invention is worth is CeO
2Nanocrystalline.
Please referring to Fig. 1, from Fig. 1 sample transmission electron microscope (TEM) pattern photo, particle size has the little block of part particles agglomerate at 20-50nm.
Please referring to Fig. 2, from the selected area electron diffraction figure of Fig. 2 sample, have diffraction spot to occur, interpret sample is CeO
2Nanocrystalline.
Claims (7)
1, a kind of preparation method of nano ceric oxide comprises the following steps;
A) solubility cerium salt is raw material, is mixed with cerous nitrate-ethanolic soln;
B) ammoniacal liquor is precipitation agent, and being mixed with concentration is 1-3molL
-1Ammoniacal liquor-ethanolic soln;
C) stir down, cerous nitrate-ethanolic soln is added drop-wise in the precipitation agent, form gel;
D) gel is in mother liquor ageing 12-24 hour;
E) filter, use deionized water wash;
F) in 80-120 ℃ of dry 5-10 hour;
G) in 400-550 ℃ of roasting 2-5 hour, obtain nano Ce O
2Particulate.
2, preparation method according to claim 1 is characterized in that, described solubility cerium salt is that cerous nitrate, cerium dichloride are or/and cerium dioxide.
3, preparation method according to claim 1 is characterized in that, the concentration of cerous nitrate is 0.20-0.40molL in described cerous nitrate-ethanolic soln
-1
4, preparation method according to claim 1 is characterized in that, ammonia concn is 1-3molL in described ammoniacal liquor-ethanolic soln
-1
5, preparation method according to claim 1 is characterized in that, with behind the deionized water wash, uses the absolute ethanol washing gel again among the described step e.
6, preparation method according to claim 1 is characterized in that, the temperature of reaction of preparation gel is 25-40 ℃.
7, preparation method according to claim 1 is characterized in that, the preparation gelating soln keeps pH=9-12.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03107272 CN1215981C (en) | 2003-03-21 | 2003-03-21 | Process for preparing nano cerium dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03107272 CN1215981C (en) | 2003-03-21 | 2003-03-21 | Process for preparing nano cerium dioxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1532147A true CN1532147A (en) | 2004-09-29 |
| CN1215981C CN1215981C (en) | 2005-08-24 |
Family
ID=34282924
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03107272 Expired - Fee Related CN1215981C (en) | 2003-03-21 | 2003-03-21 | Process for preparing nano cerium dioxide |
Country Status (1)
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|---|---|
| CN (1) | CN1215981C (en) |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1312044C (en) * | 2005-07-15 | 2007-04-25 | 清华大学 | Process for synthesizing nano cerium oxide crystal material |
| CN100341787C (en) * | 2005-03-29 | 2007-10-10 | 中国科学院大连化学物理研究所 | Cerium oxide nano materials and its preparation and use |
| CN100398448C (en) * | 2005-07-26 | 2008-07-02 | 中国科学院物理研究所 | Flower shape structured nano-cerium oxide and its preparation method and use |
| CN101386419B (en) * | 2007-09-12 | 2010-09-29 | 北京有色金属研究总院 | Composite nano cerium dioxide sol preparation method |
| CN101584981B (en) * | 2009-06-12 | 2010-12-01 | 华中师范大学 | Low-temperature preparation method of ceria nano-crystalline microsphere of graduation structure |
| CN101977873A (en) * | 2008-02-12 | 2011-02-16 | 圣戈本陶瓷及塑料股份有限公司 | Ceria material and method of forming same |
| CN102600790A (en) * | 2011-01-20 | 2012-07-25 | 中国科学院金属研究所 | Nanometer cerium oxide hydrate-based arsenic removing material, preparation method thereof and application in arsenic removing |
| CN101269971B (en) * | 2007-08-06 | 2012-09-12 | 深圳市德方纳米科技有限公司 | Method of preparing nano-particle |
| CN101541912B (en) * | 2006-11-20 | 2012-12-12 | Lg化学株式会社 | Method for preparing cerium oxide powder using organic solvent and cmp slurry comprising the same |
| CN102923753A (en) * | 2012-11-05 | 2013-02-13 | 昆明理工大学 | Method for preparing cerium dioxide material with high specific surface area |
| CN103787399A (en) * | 2013-12-10 | 2014-05-14 | 天津大学 | Preparation method of hollow-structure cerium dioxide photocatalyst |
| CN103983777A (en) * | 2014-05-07 | 2014-08-13 | 大连理工大学 | Nanometer cerium dioxide bionic oxidase-based microcystic toxin colorimetric detection method |
| CN115084543A (en) * | 2022-05-26 | 2022-09-20 | 深圳航天科技创新研究院 | Composite catalyst for alkaline fuel cell, preparation method of composite catalyst and alkaline fuel cell |
-
2003
- 2003-03-21 CN CN 03107272 patent/CN1215981C/en not_active Expired - Fee Related
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100341787C (en) * | 2005-03-29 | 2007-10-10 | 中国科学院大连化学物理研究所 | Cerium oxide nano materials and its preparation and use |
| CN1312044C (en) * | 2005-07-15 | 2007-04-25 | 清华大学 | Process for synthesizing nano cerium oxide crystal material |
| CN100398448C (en) * | 2005-07-26 | 2008-07-02 | 中国科学院物理研究所 | Flower shape structured nano-cerium oxide and its preparation method and use |
| CN101541912B (en) * | 2006-11-20 | 2012-12-12 | Lg化学株式会社 | Method for preparing cerium oxide powder using organic solvent and cmp slurry comprising the same |
| CN101269971B (en) * | 2007-08-06 | 2012-09-12 | 深圳市德方纳米科技有限公司 | Method of preparing nano-particle |
| CN101386419B (en) * | 2007-09-12 | 2010-09-29 | 北京有色金属研究总院 | Composite nano cerium dioxide sol preparation method |
| CN104828852A (en) * | 2008-02-12 | 2015-08-12 | 圣戈本陶瓷及塑料股份有限公司 | Ceria material and method of forming same |
| CN101977873A (en) * | 2008-02-12 | 2011-02-16 | 圣戈本陶瓷及塑料股份有限公司 | Ceria material and method of forming same |
| CN101584981B (en) * | 2009-06-12 | 2010-12-01 | 华中师范大学 | Low-temperature preparation method of ceria nano-crystalline microsphere of graduation structure |
| CN102600790A (en) * | 2011-01-20 | 2012-07-25 | 中国科学院金属研究所 | Nanometer cerium oxide hydrate-based arsenic removing material, preparation method thereof and application in arsenic removing |
| CN102923753B (en) * | 2012-11-05 | 2015-06-03 | 昆明理工大学 | Method for preparing cerium dioxide material with high specific surface area |
| CN102923753A (en) * | 2012-11-05 | 2013-02-13 | 昆明理工大学 | Method for preparing cerium dioxide material with high specific surface area |
| CN103787399A (en) * | 2013-12-10 | 2014-05-14 | 天津大学 | Preparation method of hollow-structure cerium dioxide photocatalyst |
| CN103983777A (en) * | 2014-05-07 | 2014-08-13 | 大连理工大学 | Nanometer cerium dioxide bionic oxidase-based microcystic toxin colorimetric detection method |
| CN115084543A (en) * | 2022-05-26 | 2022-09-20 | 深圳航天科技创新研究院 | Composite catalyst for alkaline fuel cell, preparation method of composite catalyst and alkaline fuel cell |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1215981C (en) | 2005-08-24 |
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