CN102992376A - Preparation method of sheet-shaped nano-grade cerium oxide - Google Patents
Preparation method of sheet-shaped nano-grade cerium oxide Download PDFInfo
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- CN102992376A CN102992376A CN2011102725488A CN201110272548A CN102992376A CN 102992376 A CN102992376 A CN 102992376A CN 2011102725488 A CN2011102725488 A CN 2011102725488A CN 201110272548 A CN201110272548 A CN 201110272548A CN 102992376 A CN102992376 A CN 102992376A
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Abstract
The invention discloses a preparation method of sheet-shaped nano-grade cerium oxide. According to the invention, cerium acetate or cerium formate is dispersed into anhydrous methanol, wherein a molar concentration is 0.1-0.5mol/L; benzyl alcohol or benzylamine with a same molar amount of that of cerium salt is uniformly dispersed in the solution; the mixture is delivered into an autoclave; crystallization is carried out for 24-72h under a temperature of 180 DEG C; cooling, filtering, and roasting are carried out, such that sheet-shaped nano-grade cerium oxide is obtained. The preparation method and post-treatment method are simple, and a yield is high. With the method, industrialized large-scale production is easy to realize.
Description
Technical field
The present invention relates to a kind of preparation method of rare earth material, particularly pass through the method for solvent-thermal method synthesizing flaky nano cerium oxide.
Background technology
Cerium oxide is owing to have flexibly redox couple (Ce
3+/ Ce
4+), store the oxygen ability with and to ultraviolet strong receptivity, be widely used in the wide spectrums such as gas sensor, optical material, three-way catalyst; Research cerium oxide nano materials is compared deep research, the method for preparing nano-cerium oxide also has a lot, such as high-temperature calcination, hydrothermal synthesis method, solution deposit, sol-gel method, microemulsion method, organic cerium salt thermal decomposition method etc.; In recent years, investigators find that the cerium oxide of different-shape has different physico-chemical properties.
Although the many (J.Am.Chem.Soc.2005 of bibliographical information of relevant preparation specific morphology nano-cerium oxide, 127,12814-12815.Chem.Commun., 2005,3565-3567.Chem.Mater.2007,19,1215-12171215.J.Alloy.Compd.509 (2011) 67206724. etc.), but the report of preparation two-dimensional sheet nano-cerium oxide output fewer and other preparation specific morphology nano-cerium oxides are lower, therefore are not easy to industry's enlarging production.
Summary of the invention
The purpose of this invention is to provide the method that a kind of solvent thermal (methyl alcohol heat) prepares the flake nano cerium oxide, utilize the method not only can obtain the flake nano cerium oxide, and output is larger, realize easily suitability for industrialized production.
The preparation method of a kind of flake nano cerium oxide of the present invention is to be distributed in the methanol solution, and to obtain the flake nano cerium oxide after the phenylcarbinol of adding and cerium same molar or the benzene methanamine crystallization take cerous acetate or formate as raw material.
Of the present invention a kind ofly comprise the steps: for the cerium oxide preparation method
(1) gets the cerium salt of certain mass, evenly spread to anhydrous methanol;
(2) phenylcarbinol or the benzene methanamine that take by weighing with cerium salt equimolar amount join in the above-mentioned methanol solution;
(3) mentioned solution is changed in the crystallizing kettle, put into air dry oven, after reaction under the reaction conditions of regulation, take out;
(4) after the cooling, filtration, washing, drying obtain the cerium oxide nano thin slice.
Temperature of reaction is 180 ℃, and the reaction times is 24～72 hours.
Characteristics of the present invention are: adopt the method for a kind of solvent thermal (methyl alcohol heat), can not only obtain the flake nano cerium oxide, and output is high, the aftertreatment simple and reaction of whole preparation process is also simple, realizes easily the production of technique.
Description of drawings:
Fig. 1: the scanning electron microscope (SEM) photograph of intermediate before the roasting
Fig. 2: the scanning electron microscope (SEM) photograph of sheet nano-cerium oxide after the roasting
Embodiment
The present invention will be further described below in conjunction with embodiment, but protection scope of the present invention is not limited to this.
Embodiment 1
Take by weighing the 0.01mol cerous acetate, join in the methyl alcohol of 100ml, add while stirring the 0.01mol phenylcarbinol, behind Uniform Dispersion, change mentioned solution over to reactor that volume is 200ml, put into air dry oven, 180 ℃ of lower reactions were taken out after 24 hours, after cooling, filtered, and with the anhydrous methanol washing, both got the flake nano cerium oxide behind the drying and roasting.
Embodiment 2
Take by weighing the 0.01mol cerous acetate, join in the methyl alcohol of 100ml, add while stirring the 0.01mol benzene methanamine, behind Uniform Dispersion, change mentioned solution over to reactor that volume is 200ml, put into air dry oven, 180 ℃ of lower reactions were taken out after 24 hours, after cooling, filtered, and with the anhydrous methanol washing, both got the flake nano cerium oxide behind the drying and roasting.
Embodiment 3
Take by weighing the 0.01mol cesium formate, join in the methyl alcohol of 100ml, add while stirring the 0.01mol phenylcarbinol, behind Uniform Dispersion, change mentioned solution over to reactor that volume is 200ml, put into air dry oven, 180 ℃ of lower reactions were taken out after 24 hours, after cooling, filtered, and with the anhydrous methanol washing, both got the flake nano cerium oxide behind the drying and roasting.
Claims (4)
1. the preparation method of a flake nano cerium oxide is characterized in that comprising the steps:
(1) gets the cerium salt of certain mass, evenly spread to anhydrous methanol;
(2) phenylcarbinol or the benzene methanamine that take by weighing with cerium salt equimolar amount join in the above-mentioned methanol solution;
(3) mentioned solution is changed in the crystallizing kettle, put into air dry oven, after reaction under the reaction conditions of regulation, take out;
(4) after the cooling, obtain the flake nano cerium oxide after filtration, washing, drying, the roasting.
2. method according to claim 1 is characterized in that, cerium salt is cerous acetate or cesium formate.
3. method according to claim 1 is characterized in that, the concentration of cerium salt is 0.1～0.5mol/L.
4. method according to claim 1 is characterized in that, the temperature of reaction is 180 ℃, and the reaction times is 24～72 hours.
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| CN2011102725488A CN102992376A (en) | 2011-09-15 | 2011-09-15 | Preparation method of sheet-shaped nano-grade cerium oxide |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274441A (en) * | 2013-05-23 | 2013-09-04 | 浙江理工大学 | Method for preparing nanoscale sheet cerium oxide by hydrothermal method |
| CN103922385A (en) * | 2014-05-08 | 2014-07-16 | 宿州学院 | Preparation method of cerium oxide hexagonal nanometer sheet structure |
| CN103991891B (en) * | 2014-05-08 | 2015-12-09 | 华东理工大学 | The preparation method of flake nano cerium oxide |
| CN106006703A (en) * | 2016-05-25 | 2016-10-12 | 中国科学院大学 | Method for preparing nano flaky cerium oxide and lanthanum-cerium hydroxysulfate by hydrothermal process |
| CN106145955A (en) * | 2016-08-08 | 2016-11-23 | 屠秀芬 | The nano oxidized terbium of a kind of ALON is combined the preparation method of magneto-optic crystalline ceramics |
| CN108226227A (en) * | 2017-12-31 | 2018-06-29 | 苏州南尔材料科技有限公司 | A kind of preparation method of nano-cellulose cerium oxide sensor material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004149389A (en) * | 2002-10-31 | 2004-05-27 | Nippon Shokubai Co Ltd | Process for manufacturing metal oxide particle |
| CN1948157A (en) * | 2006-11-09 | 2007-04-18 | 上海大学 | Hollow bead shaped nano-cerium oxide and its preparation method |
| CN101584981A (en) * | 2009-06-12 | 2009-11-25 | 华中师范大学 | Low-temperature preparation method of ceria nano-crystalline microsphere of graduation structure |
| CN101792171A (en) * | 2010-03-04 | 2010-08-04 | 上海大学 | Preparation method of cerium oxide nanoballs |
| CN101982414A (en) * | 2010-10-19 | 2011-03-02 | 北京航空航天大学 | Method for preparing doped nano ceria powder by utilizing solvent-thermal method |
-
2011
- 2011-09-15 CN CN2011102725488A patent/CN102992376A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004149389A (en) * | 2002-10-31 | 2004-05-27 | Nippon Shokubai Co Ltd | Process for manufacturing metal oxide particle |
| CN1948157A (en) * | 2006-11-09 | 2007-04-18 | 上海大学 | Hollow bead shaped nano-cerium oxide and its preparation method |
| CN101584981A (en) * | 2009-06-12 | 2009-11-25 | 华中师范大学 | Low-temperature preparation method of ceria nano-crystalline microsphere of graduation structure |
| CN101792171A (en) * | 2010-03-04 | 2010-08-04 | 上海大学 | Preparation method of cerium oxide nanoballs |
| CN101982414A (en) * | 2010-10-19 | 2011-03-02 | 北京航空航天大学 | Method for preparing doped nano ceria powder by utilizing solvent-thermal method |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274441A (en) * | 2013-05-23 | 2013-09-04 | 浙江理工大学 | Method for preparing nanoscale sheet cerium oxide by hydrothermal method |
| CN103922385A (en) * | 2014-05-08 | 2014-07-16 | 宿州学院 | Preparation method of cerium oxide hexagonal nanometer sheet structure |
| CN103922385B (en) * | 2014-05-08 | 2015-09-30 | 宿州学院 | A kind of preparation method of cerium oxide hexagonal nanosheet shape structure |
| CN103991891B (en) * | 2014-05-08 | 2015-12-09 | 华东理工大学 | The preparation method of flake nano cerium oxide |
| CN106006703A (en) * | 2016-05-25 | 2016-10-12 | 中国科学院大学 | Method for preparing nano flaky cerium oxide and lanthanum-cerium hydroxysulfate by hydrothermal process |
| CN106145955A (en) * | 2016-08-08 | 2016-11-23 | 屠秀芬 | The nano oxidized terbium of a kind of ALON is combined the preparation method of magneto-optic crystalline ceramics |
| CN108226227A (en) * | 2017-12-31 | 2018-06-29 | 苏州南尔材料科技有限公司 | A kind of preparation method of nano-cellulose cerium oxide sensor material |
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Application publication date: 20130327 |