CN101407331A - Method of preparing cerium oxide nano-plate - Google Patents
Method of preparing cerium oxide nano-plate Download PDFInfo
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- CN101407331A CN101407331A CNA2008102019990A CN200810201999A CN101407331A CN 101407331 A CN101407331 A CN 101407331A CN A2008102019990 A CNA2008102019990 A CN A2008102019990A CN 200810201999 A CN200810201999 A CN 200810201999A CN 101407331 A CN101407331 A CN 101407331A
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Abstract
The invention relates to a method for preparing a cerium oxide nanometer slice, which belongs to the technical field of the preparation of inorganic nanometer materials, and comprises the main steps as follows: (1) the preparation of a cerium salt mixture liquor: chemometry cerium salt of 0.3-1.0mmol and hexadecyl trimethyl ammonium bromide are dissolved by using an appropriate amount of deionized water and made into a mixture liquor; (2) hydro-thermal reaction: the obtained mixture liquor is added with an appropriate amount of ammonia and subjected to ultrasonic dispersion, and then hydro-thermal reaction is carried out for 1-3 days at the temperature of 100-180 DEG C; afterwards, centrifuge separation is carried out, the obtained precipitate is washed by using deionized water so as to lead the pH value to be 7 and neutral, and then drying is carried out at 60 DEG C so as to obtain the cerium oxide nanometer slice. The shape of the cerium oxide nanometer slice obtained by the method is square, or rhombus, or hexagon, with the size of 20-80nm and the thickness of 3-5nm.
Description
Technical field
The present invention relates to a kind of preparation method of cerium oxide nano-plate, belong to the inorganic nano material preparation process technology field.
Background technology
The rare earth resources of China is very abundant, and industrial reserves is the first in the world.Among this, cerium oxide is as a kind of rare earth compound, account for rare earth proven reserve about 50%.It has important use at aspects such as purifying vehicle exhaust, solid fuel cell, fluidic catalytic pyrolysis, chemically machinery polished abrasives.Cerium oxide nanostructure is because its specific surface area is big, and the special nature such as surfactivity height of the little and particular nanostructure of grain-size become one of present cerium oxide synthetic focus.
Japanese Patent JP2004107186 has proposed the method that a kind of thermal decomposition method prepares the cerium oxide nanoballs of diameter about 50nm, though the output of this method is bigger, solid nanometer ball has but reduced the specific surface area of cerium oxide, reduces its catalytic performance.US2008051283 has proposed a kind of with the Hydrothermal Preparation size method at the cerium oxide nano particle of 50-1000nm because it does not use other template, so its granular size homogeneity relatively poor.Chinese patent CN1683248 has proposed a kind of method with coordination precipitation legal system preparing cerium oxide nanoparticle, though this nano particle size is very easily reunited together at 5-10nm, has influenced their specific surface area, thereby has reduced the performance of cerium oxide.Simultaneously, nano-cerium oxide in reported in literature, its microscopic appearance mainly is nanoparticle (Marta Maria Natile et al.Chem.Mater.2005,17:3403-3414, Ali Bumajdad et al.Langmuir 2004,20,11223-11233, Yadong Li et al.Journal of Catalysis, 2005,229:206-212.).And easily reunion also is their total defectives.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of polymorphic cerium oxide nano-plate.
The preparation method of a kind of cerium oxide nano-plate of the present invention is characterized in that having following preparation process and step:
A. the preparation of cerium mixed salt solution: under continuous agitation condition, stoichiometric 0.3～1.0mmol cerium salt and 0.6～5.0mmol cetyl trimethylammonium bromide are dissolved with an amount of deionization; The quality mol ratio of cerium salt and cetyl trimethylammonium bromide is 1: 2～1: 5; Described cerium salt is any in Cerium II Chloride, cerous nitrate or the ceric ammonium nitrate;
B. hydro-thermal reaction and aftertreatment:, add proper ammonia, and carried out ultra-sonic dispersion 10 minutes with the cerium mixed salt solution of above-mentioned gained; Then 100-180 ℃ of hydro-thermal reaction 1～3 day; Carry out centrifugation then,, make its pH value reach 7 and be neutral the precipitated product deionized water wash after separating; 60 ℃ of oven dry down, promptly get cerium oxide nano-plate then.
The form of described cerium oxide nano-plate is square or rhombus or hexagon; It is of a size of 20～80nm, and thickness is 3～5nm.
In the inventive method, the formation mechanism of cerium oxide nano-plate is as described below:
In reaction, cetyltrimethyl ammonium ion (CTA
+) at first be adsorbed on CeO
2Nanocrystal surface, and this absorption is selectively, compares (100) crystal face, CTA
+Easier being adsorbed in (111) crystal face, easier being bonded to each other of while non-stabilized (100) crystal face, and reduce surface energy; From than big scale, just formed square nanometer sheet within a certain period of time.But after temperature raises, CeO
2Nanometer sheet shows as six sides and diamond structure.This is because the temperature rising can reduce CTA
+To (111) crystal face adsorptive power, the template direction effect is weakened; And to the CeO of cube fluorite structure that do not have the template direction effect
2, combining by (111) crystal face and to reduce surface energy, this has just formed hexagon and rhombus nanometer sheet.
The inventive method is to be soft template with the cetyl trimethylammonium bromide, makes cerium oxide nanocrystal be grown to cerium oxide nano-plate by hydro-thermal.
The cerium oxide nano-plate that the inventive method makes has the following advantages: because cerium oxide nano-plate thickness of the present invention is very little, therefore have bigger specific surface area, so its catalytic performance strengthens obviously.Nano-cerium oxide specific surface area of the present invention is 60～90m
2/ g, and commodity ceria oxide powder specific surface area is 5～10m
2/ g, the nano-cerium oxide of reporting in the document is generally 30～50m
2/ g.Nano-cerium oxide of the present invention reduces by 20～40 ℃ to the catalytic temperature of CO than other nano-cerium oxides, and the catalytic efficiency under the equal conditions improves 1～2 times.
The inventive method has characteristics such as technology is simple, easy to operate, easy control of structure.
Description of drawings
Fig. 1 is transmission electron microscope (TEM) photo of the embodiment of the invention 1 gained sample.(wire frame among the figure indicates square)
Embodiment
After now specific embodiments of the invention being described in.
Embodiment one: under condition of stirring, cerous nitrate and the 3mmol cetyl trimethylammonium bromide of 1mmol are dissolved in the 35mL water, add 5ml ammoniacal liquor, ultrasonic 10min is transferred in the 50mL water heating kettle, at 100 ℃ of hydro-thermal 24h, product is centrifugal, to neutral (pH is 7),, promptly obtain cerium oxide nano-plate with deionized water wash 60 ℃ of oven dry.(product is a square, is of a size of 20-40nm, and thickness is 3-5nm).
Embodiment two: Cerium II Chloride and the 0.9mmol cetyl trimethylammonium bromide of 0.3mmol are dissolved in the 35mL water, add 5ml ammoniacal liquor, ultrasonic 10min, be transferred in the 50mL water heating kettle, at 180 ℃ of hydro-thermal 24h, product is centrifugal, with deionized water wash extremely neutral (pH is 7), 60 ℃ of oven dry, promptly obtain cerium oxide nano-plate.(product is rhombus and hexagon, is of a size of 10-20nm, and thickness is 3-5nm).
Embodiment three: ceric ammonium nitrate and the 0.9mmol cetyl trimethylammonium bromide of 0.3mmol are dissolved in the 35mL water, add 5ml ammoniacal liquor, ultrasonic 10min, be transferred in the 50mL water heating kettle, at 120 ℃ of hydro-thermal 72h, product is centrifugal, with deionized water wash extremely neutral (pH is 7), 60 ℃ of oven dry, promptly obtain cerium oxide nano-plate.(product is a square, and rhombus and hexagon are of a size of 40-80nm, and thickness is 3-5nm).
Claims (2)
1, a kind of preparation method of cerium oxide nano-plate is characterized in that having following preparation process and step:
A. the preparation of cerium mixed salt solution: under continuous agitation condition, stoichiometric 0.3～1.0mmol cerium salt and 0.6～5.0mmol cetyl trimethylammonium bromide are dissolved with an amount of deionization; The quality mol ratio of cerium salt and cetyl trimethylammonium bromide is 1: 2～1: 5; Described cerium salt is any in Cerium II Chloride, cerous nitrate or the ceric ammonium nitrate;
B. hydro-thermal reaction and aftertreatment:, add proper ammonia, and carried out ultra-sonic dispersion 10 minutes with the cerium mixed salt solution of above-mentioned gained; Then 100-180 ℃ of hydro-thermal reaction 1～3 day; Carry out centrifugation then,, make its pH value reach 7 and be neutral the precipitated product deionized water wash after separating; 60 ℃ of oven dry down, promptly get cerium oxide nano-plate then.
2, the preparation method of a kind of cerium oxide nano-plate as claimed in claim 1 is characterized in that the form of described cerium oxide nano-plate is square or rhombus or hexagon; It is of a size of 20～80nm, and thickness is 3～5nm.
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| CNA2008102019990A CN101407331A (en) | 2008-10-30 | 2008-10-30 | Method of preparing cerium oxide nano-plate |
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| CNA2008102019990A CN101407331A (en) | 2008-10-30 | 2008-10-30 | Method of preparing cerium oxide nano-plate |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103224215A (en) * | 2013-04-09 | 2013-07-31 | 中国科学院合肥物质科学研究院 | Hexagonal nanosheet array and preparation method thereof |
| CN103274441A (en) * | 2013-05-23 | 2013-09-04 | 浙江理工大学 | Method for preparing nanoscale sheet cerium oxide by hydrothermal method |
| CN103747874A (en) * | 2011-08-24 | 2014-04-23 | 蓝氧科技有限股份公司 | Plate-shaped catalyst product and method for manufacturing same |
| CN103922385A (en) * | 2014-05-08 | 2014-07-16 | 宿州学院 | Preparation method of cerium oxide hexagonal nanometer sheet structure |
| CN106495202A (en) * | 2016-11-10 | 2017-03-15 | 中国科学院上海高等研究院 | Rare earth metal hydroxide and oxide porous tunnel nanotube and preparation method |
| CN106904649A (en) * | 2017-03-08 | 2017-06-30 | 江西理工大学 | A kind of in-situ control method of nano-cerium oxide form and crystal face |
| CN112547099A (en) * | 2020-12-23 | 2021-03-26 | 天津水泥工业设计研究院有限公司 | Low-temperature cerium-based sulfur-resistant water-resistant denitration catalyst and preparation method thereof |
| CN116251562A (en) * | 2023-02-10 | 2023-06-13 | 广州市汉宵科研技术有限公司 | Nanoscale cerium oxide particle material and preparation method thereof |
-
2008
- 2008-10-30 CN CNA2008102019990A patent/CN101407331A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103747874A (en) * | 2011-08-24 | 2014-04-23 | 蓝氧科技有限股份公司 | Plate-shaped catalyst product and method for manufacturing same |
| CN103224215A (en) * | 2013-04-09 | 2013-07-31 | 中国科学院合肥物质科学研究院 | Hexagonal nanosheet array and preparation method thereof |
| CN103224215B (en) * | 2013-04-09 | 2015-09-02 | 中国科学院合肥物质科学研究院 | Hexagonal nanosheet array and preparation method thereof |
| 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 |
| CN106495202A (en) * | 2016-11-10 | 2017-03-15 | 中国科学院上海高等研究院 | Rare earth metal hydroxide and oxide porous tunnel nanotube and preparation method |
| CN106495202B (en) * | 2016-11-10 | 2018-03-02 | 中国科学院上海高等研究院 | Rare earth metal hydroxide and oxide porous tunnel nanotube and preparation method |
| CN106904649A (en) * | 2017-03-08 | 2017-06-30 | 江西理工大学 | A kind of in-situ control method of nano-cerium oxide form and crystal face |
| CN106904649B (en) * | 2017-03-08 | 2021-01-05 | 江西理工大学 | In-situ control method for form and crystal face of nano cerium oxide |
| CN112547099A (en) * | 2020-12-23 | 2021-03-26 | 天津水泥工业设计研究院有限公司 | Low-temperature cerium-based sulfur-resistant water-resistant denitration catalyst and preparation method thereof |
| CN112547099B (en) * | 2020-12-23 | 2023-03-21 | 天津水泥工业设计研究院有限公司 | Low-temperature cerium-based sulfur-resistant water-resistant denitration catalyst and preparation method thereof |
| CN116251562A (en) * | 2023-02-10 | 2023-06-13 | 广州市汉宵科研技术有限公司 | Nanoscale cerium oxide particle material and preparation method thereof |
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Open date: 20090415 |