CN109133144A - A kind of preparation method of monodisperse ultra-small grain size ceria nano-crystalline - Google Patents
A kind of preparation method of monodisperse ultra-small grain size ceria nano-crystalline Download PDFInfo
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- CN109133144A CN109133144A CN201811228727.XA CN201811228727A CN109133144A CN 109133144 A CN109133144 A CN 109133144A CN 201811228727 A CN201811228727 A CN 201811228727A CN 109133144 A CN109133144 A CN 109133144A
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- crystalline
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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
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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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
Abstract
A kind of preparation method of monodisperse ultra-small grain size ceria nano-crystalline, method includes the following steps: cerium nitrate hexahydrate, which is first dissolved in deionized water, is made into cerous nitrate solution, then n,N-Dimethylformamide, triethanolamine mixing is added, magnetic agitation obtains uniform mixed solution；Mixed solution is transferred in the reaction kettle of polytetrafluoroethyllining lining again, is sealed, is placed in baking oven and heats, product is cooled to room temperature by heating and thermal insulation after reaction, to sediment centrifuge separation, is washed to get ceria nano-crystalline material.Gained ceria nano-crystalline partial size is about 4 ~ 8 nm, pattern almost spherical, good dispersion.The method of the present invention simple process, preparation cost is low, and reaction condition is mild, and yield is high, with short production cycle, is conducive to industrialized production.
Description
Technical field
The present invention relates to a kind of preparation methods of monodisperse ultra-small grain size ceria nano-crystalline.
Background technique
Ceria is a kind of important rare-earth oxide, due to extraordinary oxygen storage capacity and release oxygen
Ability and good redox ability, are widely used in the fields such as catalyst, UV absorbing material, fuel cell.
Pattern, particle size, surface texture, dispersibility of nanometer titanium dioxide cerium material etc. have significant shadow to its performance
It rings, by improving preparation process and method, obtains the high cerium dioxide nano of monodisperse, ultra-small grain size, large specific surface area, activity
Crystalline substance is the research hotspot having been a concern in the world.In recent years, the technology of preparing of nano ceric oxide has obtained rapid progression,
As the methods of the precipitation method, sol-gel method, hydro-thermal method, peptisation, microemulsion method, Hydrolyze method, solvent thermal decomposition method are obtained into
Function application, the granular size of prepared nano ceric oxide, pattern, aggregating state are also different.But due to titanium dioxide
Cerium is face-centred cubic structure, and crystallization trend is not easy to control in preparation process, obtains monodisperse, ultra-small grain size ceria nano-crystalline
Difficulty it is very big.From current research status, the ceria nano-crystalline or particle size of preparation larger (about 20 ~ 100
Nm) or dispersibility is poor or using expensive oil-based solvent, higher cost.Therefore, a kind of simple and feasible, production is researched and developed
Amount is high, at low cost, and the new preparation method for obtaining the small ceria nano-crystalline material of good dispersion, partial size is very necessary
's.
Summary of the invention
This, which is sent out its purpose and is that, provides a kind of preparation method of monodisperse ultra-small grain size ceria nano-crystalline, solves
Art methods are larger or dispersed poor in the presence of the ceria nano-crystalline or particle size of preparation or use
The problem of expensive oil-based solvent, higher cost.
It adopts the technical scheme that achieve the above object, a kind of system of monodisperse ultra-small grain size ceria nano-crystalline
Preparation Method, method includes the following steps:
(1) cerium nitrate hexahydrate is dissolved in deionized water and is made into cerous nitrate solution, n,N-Dimethylformamide, three ethyl alcohol is then added
Amine mixing, magnetic agitation obtain uniform mixed solution；
(2) mixed solution obtained by step (1) is transferred in the hydrothermal reaction kettle of polytetrafluoroethyllining lining, seals, is placed in baking oven
In, product is cooled to room temperature by heating and thermal insulation after reaction, to sediment centrifuge separation, is washed and is received to get ceria
The brilliant material of rice.
The concentration of cerous nitrate solution in the step (1) is 0.02 ~ 0.08 mol/L；The triethanolamine and cerous nitrate
Solution, N,N-dimethylformamide volume ratio be 1:6 ~ 16:54 ~ 64.
Baking oven heating temperature in the step (2) is 150 ~ 170 DEG C, and soaking time is 5 ~ 10 h.
Beneficial effect
The present invention has the following advantages that compared with prior art.
It is an advantage of the invention that being water and N using cerium nitrate hexahydrate and triethanolamine as raw material, N- dimethyl in this method
Formamide is solvent, and first cerium nitrate hexahydrate is dissolved in deionized water and obtains cerous nitrate solution, and N, N- dimethyl methyl is then added
Amide, magnetic agitation are a kind of high boiling pole since n,N-Dimethylformamide energy and water and most of organic solvent dissolve each other
Property (hydrophily) non-protonic solvent, acts on very crucial in the methods of the invention；In addition triethanolamine, triethanolamine are added
Water-soluble and n,N-Dimethylformamide, and there is alkalinity, triethanolamine adds in a kettle again after mixing with above-mentioned solution
Heat can release alkali radical ion, and the cerium ion that alkali radical ion and cerous nitrate ionize out, which reacts, generates cerium hydroxide, reheating point
Solution obtains ceria nano-crystalline, and the ceria nano-crystalline partial size that the method for the present invention obtains is extra small, about 4 ~ 8 nm, closely
Like spherical shape, good dispersion, large specific surface area, preparation process is simple, at low cost, and reaction condition is mild, and yield is high, the production cycle
It is short, be conducive to industrialized production.
Detailed description of the invention
Below in conjunction with attached drawing, the invention will be further described.
Fig. 1 is the TEM figure of ceria nano-crystalline made from the embodiment of the present invention 1；
Fig. 2 is the TEM figure of ceria nano-crystalline made from the embodiment of the present invention 2.
Specific embodiment
With reference to the accompanying drawing, the present invention is further illustrated.
A kind of preparation method of monodisperse ultra-small grain size ceria nano-crystalline, method includes the following steps:
(1) cerium nitrate hexahydrate is dissolved in deionized water and is made into cerous nitrate solution, n,N-Dimethylformamide, three ethyl alcohol is then added
Amine mixing, magnetic agitation obtain uniform mixed solution；
(2) mixed solution obtained by step (1) is transferred in the hydrothermal reaction kettle of polytetrafluoroethyllining lining, seals, is placed in baking oven
In, product is cooled to room temperature by heating and thermal insulation after reaction, to sediment centrifuge separation, is washed and is received to get ceria
The brilliant material of rice.
The concentration of cerous nitrate solution in the step (1) is 0.02 ~ 0.08 mol/L；The triethanolamine and cerous nitrate
Solution, N,N-dimethylformamide volume ratio be 1:6 ~ 16:54 ~ 64.
Baking oven heating temperature in the step (2) is 150 ~ 170 DEG C, and soaking time is 5 ~ 10 h.
Embodiment 1
(1) 0.40 g cerium nitrate hexahydrate is dissolved in 20 mL deionized waters, magnetic agitation obtains cerous nitrate solution；Then 120 are added
ML n,N-Dimethylformamide, 15 min of magnetic agitation；2 mL triethanolamines are added, 30 min of magnetic agitation is obtained uniformly
Mixed solution；
(2) 35mL step (1) resulting mixed solution is taken, is transferred in the reaction kettle of polytetrafluoroethyllining lining, seals, is placed in
It is heated in 150 DEG C of baking ovens, product is cooled to room temperature by 7 h of heat preservation after reaction, is centrifugated to sediment, is used deionization
Water and dehydrated alcohol wash 3 times to get ceria nano-crystalline material, as shown in Figure 1.
Embodiment 2
(1) 0.40 g cerium nitrate hexahydrate is dissolved in 20 mL deionized waters, magnetic agitation obtains cerous nitrate solution；Then 120 are added
ML n,N-Dimethylformamide, 15 min of magnetic agitation；2 mL triethanolamines are added, 30 min of magnetic agitation is obtained uniformly
Mixed solution；
(2) 35mL step (1) resulting mixed solution is taken, is transferred in the reaction kettle of polytetrafluoroethyllining lining, seals, is placed in
It is heated in 160 DEG C of baking ovens, product is cooled to room temperature by 6 h of heat preservation after reaction, is centrifugated to sediment, is used deionization
Water and dehydrated alcohol wash 3 times to get ceria nano-crystalline material, as shown in Figure 2.
Claims (3)
1. a kind of preparation method of monodisperse ultra-small grain size ceria nano-crystalline, which is characterized in that this method includes following step
It is rapid:
Cerium nitrate hexahydrate is dissolved in deionized water and is made into cerous nitrate solution, n,N-Dimethylformamide, triethanolamine is then added
Mixing, magnetic agitation obtain uniform mixed solution；
Mixed solution obtained by step (1) is transferred in the hydrothermal reaction kettle of polytetrafluoroethyllining lining, seals, is placed in baking oven,
Product is cooled to room temperature by heating and thermal insulation after reaction, to sediment centrifuge separation, is washed to get ceria nano-crystalline
Material.
2. a kind of preparation method of monodisperse ultra-small grain size ceria nano-crystalline according to claim 1, feature exist
In the concentration of the cerous nitrate solution in the step (1) is 0.02 ~ 0.08 mol/L；The triethanolamine and cerous nitrate solution,
The volume ratio of N,N-dimethylformamide is 1:6 ~ 16:54 ~ 64.
3. a kind of preparation method of monodisperse ultra-small grain size ceria nano-crystalline according to claim 1, feature exist
In the baking oven heating temperature in the step (2) is 150 ~ 170 DEG C, and soaking time is 5 ~ 10 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811228727.XA CN109133144B (en) | 2018-10-22 | 2018-10-22 | Preparation method of monodisperse ultra-small particle size cerium dioxide nanocrystal |
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| CN201811228727.XA CN109133144B (en) | 2018-10-22 | 2018-10-22 | Preparation method of monodisperse ultra-small particle size cerium dioxide nanocrystal |
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| CN109133144A true CN109133144A (en) | 2019-01-04 |
| CN109133144B CN109133144B (en) | 2021-04-02 |
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| CN201811228727.XA Expired - Fee Related CN109133144B (en) | 2018-10-22 | 2018-10-22 | Preparation method of monodisperse ultra-small particle size cerium dioxide nanocrystal |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111434612A (en) * | 2020-02-28 | 2020-07-21 | 东南大学 | Oxygen vacancy content adjustable CeO2Preparation method of nano material |
| CN112794357A (en) * | 2021-03-29 | 2021-05-14 | 安徽景成新材料有限公司 | Method for synthesizing nano cerium oxide by hydrothermal method |
| CN116004122A (en) * | 2022-12-27 | 2023-04-25 | 嘉庚创新实验室 | Cerium dioxide polishing solution and preparation method thereof |
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| CN101117233A (en) * | 2007-07-23 | 2008-02-06 | 北京科技大学 | Method for preparing high specific surface area meso-porous cerium dioxide micro-balloon |
| CN101264922A (en) * | 2008-04-21 | 2008-09-17 | 上海大学 | Method for preparing cerium oxide rhombus nano sheet-shaped material |
| CN104925845A (en) * | 2015-07-08 | 2015-09-23 | 江西师范大学 | Multi-layer core shell structure CeO2 nanometer hollow sphere template-free composite method |
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2018
- 2018-10-22 CN CN201811228727.XA patent/CN109133144B/en not_active Expired - Fee Related
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| CN101264922A (en) * | 2008-04-21 | 2008-09-17 | 上海大学 | Method for preparing cerium oxide rhombus nano sheet-shaped material |
| CN106794448A (en) * | 2014-10-07 | 2017-05-31 | 巴斯夫公司 | The synthesis of the colloid noble metal nano particles with controlled size and form |
| CN106277049A (en) * | 2015-06-08 | 2017-01-04 | 北京化工大学 | A kind of transparent nano zirconium oxide liquid dispersion and preparation method and application |
| CN104925845A (en) * | 2015-07-08 | 2015-09-23 | 江西师范大学 | Multi-layer core shell structure CeO2 nanometer hollow sphere template-free composite method |
| CN107482229A (en) * | 2017-06-27 | 2017-12-15 | 广西大学 | A kind of surfactant-free prepares CeO2The method of/C nano net |
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| ANRAN XIE ET AL.: ""Template-free hydrothermal synthesis and CO oxidation properties of flower-like CeO2 nanostructures"", 《MATERIALS RESEARCH BULLETIN》 * |
| DONGFENG SUN ET AL.: ""Effects of nitrogen content in monocrystalline nano-CeO2 on the degradation of dye in indoor lighting"", 《APPLIED SURFACE SCIENCE》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111434612A (en) * | 2020-02-28 | 2020-07-21 | 东南大学 | Oxygen vacancy content adjustable CeO2Preparation method of nano material |
| CN111434612B (en) * | 2020-02-28 | 2023-07-18 | 东南大学 | CeO with adjustable oxygen vacancy content 2 Method for preparing nano material |
| CN112794357A (en) * | 2021-03-29 | 2021-05-14 | 安徽景成新材料有限公司 | Method for synthesizing nano cerium oxide by hydrothermal method |
| CN116004122A (en) * | 2022-12-27 | 2023-04-25 | 嘉庚创新实验室 | Cerium dioxide polishing solution and preparation method thereof |
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