CN104386731A - Preparation method of pineapple-shaped nano cerium oxide by nano-bulk self-assembly - Google Patents
Preparation method of pineapple-shaped nano cerium oxide by nano-bulk self-assembly Download PDFInfo
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- CN104386731A CN104386731A CN201410634144.2A CN201410634144A CN104386731A CN 104386731 A CN104386731 A CN 104386731A CN 201410634144 A CN201410634144 A CN 201410634144A CN 104386731 A CN104386731 A CN 104386731A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The invention relates to a preparation method of a nano material, particularly a preparation method of pineapple-shaped nano cerium oxide by nano-bulk self-assembly, which comprises the following steps: (1) dissolving 2-2.5g of cerium nitrate in 70-75ml of water, sufficiently dissolving, and adding 2.5-2.6g of cetyl trimethylammonium bromide; stirring for 30-40 minutes, adding 4-4.5g of urea, continuing stirring for sufficient mixing; (2) transferring the mixed solution into a reaction kettle, and carrying out thermostatic reaction at 120 DEG C for 10-12 hours; and (3) after the reaction kettle is cooled, taking out the sample, centrifuging, washing, drying, and keeping the temperature at 400-450 DEG C for 2 hours to obtain the product. The method is simple in preparation process, convenient to operate and controllable in technological parameters. The synthesized nano cerium oxide is the special-pineapple-shaped nano cerium oxide prepared by nano-bulk self-assembly.
Description
Technical field
The present invention relates to the preparation method of nano material cerium oxide, be specially a kind of preparation method having nanometer blocks to be self-assembled into pineapple shape nano-cerium oxide.
Background technology
Cerium dioxide is the light rare earths oxide compound that a kind of cheapness, purposes are extremely wide, has been used to the chemical decolorization agent, radioresistive glass, electronic ceramics etc. of luminescent material, rumbling compound, uv-absorbing agent, cleaning catalyst for tail gases of automobiles, glass.The physicochemical property of cerium dioxide directly may affect the performance of material, and as adding of ultra-fine cerium dioxide not only can reduce ceramic sintering temperature, can also increase the density of pottery, bigger serface can improve the catalytic activity of catalyzer; And there is appraising at the current rate property due to cerium, also significant to luminescent material.
In recent years, along with developing rapidly and widespread use of rare earth new material, it is found that ultrafine powder cerium dioxide has the performance of new excellence.Phase early 1990s, prepare about ultra-fine cerium dioxide, two sections of patents that Jin You Rhone-Poulene company applies for, its content utilizes cerous nitrate ammonium hydrolysis method and basic sulfate cerium salt pyrolysis method to prepare specific surface area to be greater than 100m
2the cerium dioxide of/g.Since the mid-90 in 20th century, increasing to the research in this field, the preparation method and application's research about nano ceric oxide achieves larger progress.The method preparing nano ceric oxide has solid sintering technology, liquid phase method and vapor phase process.
Summary of the invention
The object of the present invention is to provide a kind of method preparing nano-cerium oxide that process is simple, easy to operate, form pineapple shape nano-cerium oxide.
The present invention adopts following technical scheme to realize:
Be self-assembled into a preparation method for roller shape nano-cerium oxide by nanometer blocks, comprise the steps:
(1), by 2-2.5g cerous nitrate be dissolved in 70-75ml water, after fully dissolving, add 2.5-2.6g cetyl trimethylammonium bromide; After stirring 30-40min, add the urea of 4-4.5g, continue to be stirred to abundant mixing;
(2), by mixing solutions reactor is transferred to, at 120 DEG C of isothermal reaction 10-12h;
(3), reactor cooling after, take out sample, through centrifugal, washing and drying treatment after, at 400-450 DEG C, namely constant temperature 2h obtains product-pineapple shape nano-cerium oxide, and its microtexture is as shown in Figure 2.
Under these conditions, adopt the raw material type of regulation, rational proportioning raw materials, formulate the temperature of reaction and time optimized.Wherein, urea provides the alkaline environment strengthened gradually, is conducive to reacting with cerous nitrate generating nanometer blocks cerium oxide particle, simultaneously the structural promoter effect of collaborative cetyl trimethylammonium bromide (CTAB), and orientation is self-assembled into target product.The parameters such as the proportioning raw materials in aforesaid method, experimental temperature and time be all applicant through long-felt and great many of experiments, obtain the required special parameter of special pineapple shape nano-cerium oxide, last thermal treatment temp ensure that the purity of this product.
The nano material that aforesaid method obtains-pineapple shape cerium oxide carried noble metal palladium catalyst can be used for low concentration methane oxidation, Be very effective.Catalyst loadings 0.5%, air speed 130000/h, 250 degree start reaction, and 300 degree of methane conversions reach 14%, have light-off temperature low, the advantage that low temperature active is high.
The present invention is reasonable in design, and the nano-cerium oxide of synthesis is self-assembled into the nano-cerium oxide with roller shape special appearance by nanometer blocks, and preparation process is simple, and easy to operate, processing parameter is easy to control, and cost is low, has good application prospect.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram that nanometer blocks is self-assembled into pineapple shape nano-cerium oxide.
Fig. 2 is the scanning electron microscope (SEM) photograph that nanometer blocks is self-assembled into pineapple shape nano-cerium oxide.
Embodiment
Below specific embodiments of the invention are described in detail.
embodiment 1
Be self-assembled into a preparation method for pineapple shape nano-cerium oxide by nanometer blocks, comprise the steps:
(1), by 2g cerous nitrate be dissolved in 75ml water, after fully dissolving, add 2.55g cetyl trimethylammonium bromide; After stirring 40min, add the urea of 4.5g, continue to stir 30min to fully mixing;
(2), by mixing solutions reactor is transferred to, at 120 DEG C of isothermal reaction 10h;
(3), reactor cooling after, take out sample, through centrifugal, washing and drying treatment after, at 400 DEG C, namely constant temperature 2h obtains product-pineapple shape nano-cerium oxide.
embodiment 2
Be self-assembled into a preparation method for pineapple shape nano-cerium oxide by nanometer blocks, comprise the steps:
(1), by 2.3g cerous nitrate be dissolved in 70ml water, after fully dissolving, add 2.6g cetyl trimethylammonium bromide; After stirring 35min, add the urea of 4g, continue to stir 30min to fully mixing;
(2), by mixing solutions reactor is transferred to, at 120 DEG C of isothermal reaction 11h;
(3), reactor cooling after, take out sample, through centrifugal, washing and drying treatment after, at 450 DEG C, namely constant temperature 2h obtains product-pineapple shape nano-cerium oxide.
embodiment 3
Be self-assembled into a preparation method for pineapple shape nano-cerium oxide by nanometer blocks, comprise the steps:
(1), by 2.5g cerous nitrate be dissolved in 72ml water, after fully dissolving, add 2.5g cetyl trimethylammonium bromide; After stirring 30min, add the urea of 4.2g, continue to stir 30min to fully mixing;
(2), by mixing solutions reactor is transferred to, at 120 DEG C of isothermal reaction 12h;
(3), reactor cooling after, take out sample, through centrifugal, washing and drying treatment after, at 430 DEG C, namely constant temperature 2h obtains product-pineapple shape nano-cerium oxide.
Claims (1)
1. be self-assembled into a preparation method for pineapple shape nano-cerium oxide by nanometer blocks, it is characterized in that: comprise the steps:
(1), by 2-2.5g cerous nitrate be dissolved in 70-75ml water, after fully dissolving, add 2.5-2.6g cetyl trimethylammonium bromide; After stirring 30-40min, add the urea of 4-4.5g, continue to be stirred to abundant mixing;
(2), by mixing solutions reactor is transferred to, at 120 DEG C of isothermal reaction 10-12h;
(3), reactor cooling after, take out sample, through centrifugal, washing and drying treatment after, at 400-450 DEG C, namely constant temperature 2h obtains product.
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| CN201410634144.2A CN104386731B (en) | 2014-11-12 | 2014-11-12 | Be self-assembled into the preparation method of pineapple shape nano-cerium oxide by nanometer blocks |
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| CN201410634144.2A CN104386731B (en) | 2014-11-12 | 2014-11-12 | Be self-assembled into the preparation method of pineapple shape nano-cerium oxide by nanometer blocks |
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| Publication Number | Publication Date |
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| CN104386731A true CN104386731A (en) | 2015-03-04 |
| CN104386731B CN104386731B (en) | 2016-05-18 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101264922A (en) * | 2008-04-21 | 2008-09-17 | 上海大学 | Method for preparing cerium oxide rhombus nano sheet-shaped material |
| US20100264097A1 (en) * | 2007-07-18 | 2010-10-21 | Nanyang Technological University | Hollow porous microspheres |
| CN101891236A (en) * | 2010-07-16 | 2010-11-24 | 扬州大学 | Method for synthesizing monodisperse samarium-doped rare earth cerium oxide nanocrystal |
| CN102407127A (en) * | 2011-11-23 | 2012-04-11 | 中国科学院生态环境研究中心 | Cobalt cerium composite metal oxide, its preparation method and its application |
| CN103449496A (en) * | 2012-12-31 | 2013-12-18 | 深圳信息职业技术学院 | Nano cerium oxide and preparation method thereof |
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- 2014-11-12 CN CN201410634144.2A patent/CN104386731B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100264097A1 (en) * | 2007-07-18 | 2010-10-21 | Nanyang Technological University | Hollow porous microspheres |
| CN101264922A (en) * | 2008-04-21 | 2008-09-17 | 上海大学 | Method for preparing cerium oxide rhombus nano sheet-shaped material |
| CN101891236A (en) * | 2010-07-16 | 2010-11-24 | 扬州大学 | Method for synthesizing monodisperse samarium-doped rare earth cerium oxide nanocrystal |
| CN102407127A (en) * | 2011-11-23 | 2012-04-11 | 中国科学院生态环境研究中心 | Cobalt cerium composite metal oxide, its preparation method and its application |
| CN103449496A (en) * | 2012-12-31 | 2013-12-18 | 深圳信息职业技术学院 | Nano cerium oxide and preparation method thereof |
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Inventor after: Guo Tianyu Inventor after: Li Jinping Inventor after: Du Jianping Inventor after: Wu Jinting Inventor before: Li Jinping Inventor before: Guo Tianyu Inventor before: Du Jianping Inventor before: Wu Jinting |
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