CN103193257B - Flower-shaped ceria preparation method - Google Patents
Flower-shaped ceria preparation method Download PDFInfo
- Publication number
- CN103193257B CN103193257B CN201310111041.3A CN201310111041A CN103193257B CN 103193257 B CN103193257 B CN 103193257B CN 201310111041 A CN201310111041 A CN 201310111041A CN 103193257 B CN103193257 B CN 103193257B
- Authority
- CN
- China
- Prior art keywords
- preparation
- ceria
- cerium dioxide
- flower
- shaped
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
The invention relates to a ceria preparing method, and particularly relates to a flower-shaped ceria preparation method. The flower-shaped ceria preparation method solves the technical problem that as the shape of the conventional ceria is not easy to adjust and control, most of the products are rod-shaped, linear, tubular or spherical. The flower-shaped ceria preparation method comprises the following steps: step 1, mixing and putting Ce(NO3)3.6H2O and L-cysteine into distilled water, adding an ammonia solution for adjusting the pH, and transferring the mixed solution into a reaction kettle for heating after further stirring; and step 2, cooling the reaction kettle to obtain a reaction product, and washing, filtering and drying to obtain the pale yellow flower-shaped ceria. The flower-shaped ceria is synthesized by a simple method; and unlike the commonly used raw material for preparing ceria, the L-cysteine is introduced in the shape preparation of ceria to serve as the surfactant, and the flower-shaped ceria is prepared by being combined with a hydrothermal method. The flower-shaped ceria preparation method has the characteristics that amino acid is used as a surfactant for preparing ceria; the prepared ceria is novel in shape; the operation is simple; and the cost is low, and the obtained product is high in purity.
Description
Technical field
The present invention relates to a kind of preparation method of cerium dioxide.
Background technology
At present, rare earth material all has irreplaceable effect at aspects such as military affairs, chemical industry, glass-ceramic, agriculturals, China has abundant rare earth Mineral resources, minerogentic condition is superior, can be rated as richly endowed by nature, explored reserves occupy first of the world, if can reasonably utilize rare earth resources, will inevitably bring many benefits to the Economic development of China.CeO
2as a kind of important rare earth oxide, owing to thering is unique 4f electronic structure, make it show excellent the oxygen ability of storing and charge-exchange ability, at three-way catalyst, fuel cell, all has application in the fields such as photochemical catalysis and pollutant treatment.
Along with scientific and technical development, many high-new pointed collars territory is more and more higher to the requirement of rare earth material performance, and large quantity research shows, therefore material pattern can produce considerable influence to material property, how to realize material that controlled preparation has suitable pattern and is undoubtedly in field of material preparation one and has far-reaching problem.In view of the impact of material pattern on material property, if can prepare the cerium dioxide with Unique pattern, make possibly it show special performance.The pattern that current existing method is prepared cerium dioxide is easy-regulating not, and the pattern of common cerium dioxide is mainly: bar-shaped, wire, tubulose and the shape such as spherical, be still more rare for the report of the cerium dioxide of other special appearances.As can be seen here, the preparation research for special appearance cerium dioxide has higher scientific research and learning value.And, if the special appearance cerium dioxide making has comparatively unique performance, also can bring wide application prospect for it.
Summary of the invention
The present invention seeks in order to solve not easy-regulating of pattern that existing method prepares cerium dioxide, make product shape and mostly be bar-shaped, wire, tubulose and spherical technical problem, and a kind of preparation method who spends shape cerium dioxide is provided.
The preparation method of flower shape cerium dioxide realizes according to the following steps:
One, by Ce (NO
3)
36H
2o and Cys are with (1-3): mixed in molar ratio (1-3) is put in 30ml distilled water and is stirred to completely and dissolves, the ammonia soln that is 25% to above-mentioned mixed solution and dripping mass concentration under agitation condition is to pH=9～12 of mixing solutions, after continuing to stir 30min, above-mentioned solution is proceeded in reactor and at 140～180 ℃, carries out airtight heating, the reaction times is 12～48h;
Two, after completion of the reaction reactor is taken out and naturally cools to room temperature, obtain reaction product, then use distilled water repetitive scrubbing remaining to inclusion-free, filter, dry 12h at 80～100 ℃, obtains lurid colored shape cerium dioxide again, completes the preparation of colored shape cerium dioxide.
The present invention adopts a kind of simple preparation method to synthesize the cerium dioxide of colored shape, be different from and prepare the raw material that cerium dioxide material is conventional, the present invention serves as tensio-active agent in the middle of Cys being incorporated into the pattern preparation of cerium dioxide, has prepared the cerium dioxide of colored shape in conjunction with hydrothermal method.Outstanding feature of the present invention is: (1) adopts amino acid to prepare cerium dioxide as tensio-active agent; (2) the cerium dioxide pattern obtaining is novel; (3) simple to operate; (4) cost is low, and the product pattern obtaining is homogeneous comparatively.
Accompanying drawing explanation
Fig. 1 is the XRD figure of preparing gained flower shape cerium dioxide in embodiment 1;
Fig. 2 is the scanning electron microscope (SEM) photograph of preparing gained flower shape cerium dioxide in embodiment 1;
Fig. 3 is the scanning electron microscope (SEM) photograph of preparing gained flower shape cerium dioxide in embodiment 2;
Fig. 4 is the scanning electron microscope (SEM) photograph of preparing gained flower shape cerium dioxide in embodiment 3.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method of present embodiment flower shape cerium dioxide realizes according to the following steps:
One, by Ce (NO
3)
36H
2o and Cys are with (1-3): mixed in molar ratio (1-3) is put in 30ml distilled water and is stirred to completely and dissolves, the ammonia soln that is 25% to above-mentioned mixed solution and dripping mass concentration under agitation condition is to pH=9～12 of mixing solutions, after continuing to stir 30min, above-mentioned solution is proceeded in reactor and at 140～180 ℃, carries out airtight heating, the reaction times is 12～48h;
Two, after completion of the reaction reactor is taken out and naturally cools to room temperature, obtain reaction product, then use distilled water repetitive scrubbing remaining to inclusion-free, filter, dry 12h at 80～100 ℃, obtains lurid colored shape cerium dioxide again, completes the preparation of colored shape cerium dioxide.
Embodiment two: that present embodiment is different from embodiment one is (the NO of Ce described in step 1
3)
36H
2the mol ratio of O and Cys is 3: 1.Other is identical with embodiment one.
Embodiment three: that present embodiment is different from embodiment one is (the NO of Ce described in step 1
3)
36H
2the mol ratio of O and Cys is 1: 1.Other is identical with embodiment one.
Embodiment four: that present embodiment is different from embodiment one is (the NO of Ce described in step 1
3)
36H
2the mol ratio of O and Cys is 1: 3.Other is identical with embodiment one.
Embodiment five: present embodiment is different from one of embodiment one to four is that to drip mass concentration in step 1 be that 25% ammonia soln is to the pH=9 of mixing solutions.Other is identical with one of embodiment one to four.
Embodiment six: present embodiment is different from one of embodiment one to four is that to drip mass concentration in step 1 be that 25% ammonia soln is to the pH=10 of mixing solutions.Other is identical with one of embodiment one to four.
Embodiment seven: present embodiment is different from one of embodiment one to four is that to drip mass concentration in step 1 be that 25% ammonia soln is to the pH=12 of mixing solutions.Other is identical with one of embodiment one to four.
Embodiment eight: what present embodiment was different from one of embodiment one to seven is to carry out airtight heating in step 2 at 160 ℃, and the reaction times is 24h.Other is identical with one of embodiment one to seven.
Embodiment nine: what present embodiment was different from one of embodiment one to eight is to be dried 12h in step 3 at 90 ℃.Other is identical with one of embodiment one to eight.
Embodiment 1:
The preparation method of flower shape cerium dioxide realizes according to the following steps:
One, by Ce (NO
3)
36H
2o and Cys are put in 30ml distilled water and are stirred to completely and dissolve with the mixed in molar ratio of 1: 3, the ammonia soln that is 25% to above-mentioned mixed solution and dripping mass concentration under agitation condition is to the pH=10 of mixing solutions, after continuing to stir 30min, above-mentioned solution is proceeded in reactor and at 180 ℃, carries out airtight heating, the reaction times is 24h;
Two, after completion of the reaction reactor is taken out and naturally cools to room temperature, obtain reaction product, then use distilled water repetitive scrubbing remaining to inclusion-free, filter, dry 12h at 100 ℃, obtains lurid colored shape cerium dioxide again, completes the preparation of colored shape cerium dioxide.
In the present embodiment, prepare gained flower shape cerium dioxide, its XRD result (seeing Fig. 1) shows: in 2 θ=28.6 °, 33.1 °, 47.4 °, 56.3 ° have occurred strong characteristic diffraction peak, corresponded respectively to CeO
2(111), (200), (220) and (311) crystal face, these strong characteristic diffraction peaks are all pointed out CeO
2the crystalline phase that exists be Emission in Cubic CeO
2.
In the present embodiment, prepare gained flower shape cerium dioxide, its SEM result (Fig. 2) shows: the cerium dioxide preparing is colored shape, and flower shape structure is assembled by numerous laminar cerium dioxides, and the material making has larger specific surface area.Size is: be about 20 μ m.
Embodiment 2:
The preparation method of flower shape cerium dioxide realizes according to the following steps:
One, by Ce (NO
3)
36H
2o and Cys are put in 30ml distilled water and are stirred to completely and dissolve with the mixed in molar ratio of 3: 1, the ammonia soln that is 25% to above-mentioned mixed solution and dripping mass concentration under agitation condition is to the pH=10 of mixing solutions, after continuing to stir 30min, above-mentioned solution is proceeded in reactor and at 140 ℃, carries out airtight heating, the reaction times is 48h;
Two, after completion of the reaction reactor is taken out and naturally cools to room temperature, obtain reaction product, then use distilled water repetitive scrubbing remaining to inclusion-free, filter, dry 12h at 100 ℃, obtains lurid colored shape cerium dioxide again, completes the preparation of colored shape cerium dioxide.
In the present embodiment, prepare gained flower shape cerium dioxide, its SEM result (Fig. 3) shows: the cerium dioxide preparing also presents colored shape state, but imperfect.
Embodiment 3:
The preparation method of flower shape cerium dioxide realizes according to the following steps:
One, by Ce (NO
3)
36H
2o and Cys are put in 30ml distilled water and are stirred to completely and dissolve with the mixed in molar ratio of 1: 1, the ammonia soln that is 25% to above-mentioned mixed solution and dripping mass concentration under agitation condition is to the pH=10 of mixing solutions, after continuing to stir 30min, above-mentioned solution is proceeded in reactor and at 140 ℃, carries out airtight heating, the reaction times is 48h;
Two, after completion of the reaction reactor is taken out and naturally cools to room temperature, obtain reaction product, then use distilled water repetitive scrubbing remaining to inclusion-free, filter, dry 12h at 100 ℃, obtains lurid colored shape cerium dioxide again, completes the preparation of colored shape cerium dioxide.
In the present embodiment, prepare gained flower shape cerium dioxide, its SEM result (Fig. 4) shows: the cerium dioxide preparing also presents colored shape state, but imperfect.
Through embodiment 1,2 and 3, Ce (NO in visible embodiment 1
3)
36H
2o: Cys=1: reaction at 3,180 ℃, gained cerium dioxide is the in the best state of colored shape, and flower shape structure is assembled by numerous laminar cerium dioxides, and the material making has larger specific surface area.
Claims (4)
1. spend the preparation method of shape cerium dioxide, it is characterized in that it realizes according to the following steps:
One, by Ce (NO
3)
36H
2o and Cys are with (1-3): mixed in molar ratio (1-3) is put in 30mL distilled water and is stirred to completely and dissolves, the ammonia soln that is 25% to above-mentioned mixed solution and dripping mass concentration under agitation condition is to the pH=12 of mixing solutions, after continuing to stir 30min, above-mentioned solution is proceeded in reactor and at 140～180 ℃, carries out airtight heating, the reaction times is 12～48h;
Two, after completion of the reaction reactor is taken out and naturally cools to room temperature, obtain reaction product, then use distilled water repetitive scrubbing remaining to inclusion-free, filter, dry 12h at 80～100 ℃, obtains lurid colored shape cerium dioxide again, completes the preparation of colored shape cerium dioxide.
2. the preparation method of colored shape cerium dioxide according to claim 1, is characterized in that Ce (NO described in step 1
3)
36H
2the mol ratio of O and Cys is 1:3.
3. the preparation method of colored shape cerium dioxide according to claim 2, is characterized in that at 160 ℃, carrying out airtight heating in step 1, and the reaction times is 24h.
4. the preparation method of colored shape cerium dioxide according to claim 3, is characterized in that in step 2 dry 12h at 90 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310111041.3A CN103193257B (en) | 2013-04-01 | 2013-04-01 | Flower-shaped ceria preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310111041.3A CN103193257B (en) | 2013-04-01 | 2013-04-01 | Flower-shaped ceria preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103193257A CN103193257A (en) | 2013-07-10 |
| CN103193257B true CN103193257B (en) | 2014-08-20 |
Family
ID=48716103
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310111041.3A Expired - Fee Related CN103193257B (en) | 2013-04-01 | 2013-04-01 | Flower-shaped ceria preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103193257B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103713036A (en) * | 2014-01-22 | 2014-04-09 | 黑龙江大学 | Method of modifying electrode by virtue of ceria and method of determining content of heavy metals in water by virtue of electrode modified by ceria |
| CN106745175A (en) * | 2017-03-13 | 2017-05-31 | 南京工程学院 | A kind of simple preparation method of hollow nanospheres cerium oxide |
| CN113318792B (en) * | 2021-06-22 | 2022-06-21 | 哈尔滨理工大学 | Flaky CeO2/UIO-66-NH2Composite photocatalytic material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992384A (en) * | 2012-12-12 | 2013-03-27 | 黑龙江大学 | Preparation method of triangular prism-shape ceric oxide |
-
2013
- 2013-04-01 CN CN201310111041.3A patent/CN103193257B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992384A (en) * | 2012-12-12 | 2013-03-27 | 黑龙江大学 | Preparation method of triangular prism-shape ceric oxide |
Non-Patent Citations (10)
| Title |
|---|
| Chunwen Sun et al..Mesoscale organization of nearly monodisperse flowerlike ceria microspheres.《J. Phys. Chem. B》.2006,第110卷第13445-13452页. |
| Controlled synthesis of Ce(OH)CO3 flowers by a hydrothermal method and theirthermal conversion to CeO2 flowers;Dongen Zhang et al.;《Particuology》;20121231;第10卷;第771-776页 * |
| Controlled Synthesis of CeO2 Flower-Like and Well-Aligned Nanorod Hierarchical Architectures by a Phosphate-Assisted Hydrothermal Route;Ranbo Yu et al.;《J. Phys. Chem. C》;20081121;第112卷;第19896–19900页 * |
| Dongen Zhang et al..Controlled synthesis of Ce(OH)CO3 flowers by a hydrothermal method and theirthermal conversion to CeO2 flowers.《Particuology》.2012,第10卷第771-776页. |
| Mesoscale organization of nearly monodisperse flowerlike ceria microspheres;Chunwen Sun et al.;《J. Phys. Chem. B》;20060616;第110卷;第13445-13452页 * |
| Ranbo Yu et al..Controlled Synthesis of CeO2 Flower-Like and Well-Aligned Nanorod Hierarchical Architectures by a Phosphate-Assisted Hydrothermal Route.《J. Phys. Chem. C》.2008,第112卷第19896–19900页. |
| Template-Free Synthesis of Sphere, Rod and Prism Morphologies of CeO2 Oxidation Catalysts;Yejun Guan et al.;《Catal Lett》;20100422;第137卷;第28-34页 * |
| YejunGuanetal..Template-FreeSynthesisofSphere Rod and Prism Morphologies of CeO2 Oxidation Catalysts.《Catal Lett》.2010 |
| 不同形貌的CeO2的水热法制备及表征;栾宝平等;《上海师范大学学报(自然科学版)》;20110430;第40卷(第2期);第157-162页 * |
| 栾宝平等.不同形貌的CeO2的水热法制备及表征.《上海师范大学学报(自然科学版)》.2011,第40卷(第2期),第157-162页. |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103193257A (en) | 2013-07-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103746112B (en) | A kind of multistage nanometer micrometer structure material, its preparation method and comprise the battery of this material | |
| CN101584981B (en) | Low-temperature preparation method of ceria nano-crystalline microsphere of graduation structure | |
| CN102824884B (en) | A kind of TiO 2/ Fe 2o 3compound hollow microballoon and preparation method thereof | |
| CN109999836A (en) | A kind of preparation of indium oxide/indium sulfide heterojunction semiconductor material and photochemical catalyst purposes and solar energy fixed nitrogen application | |
| CN102992384B (en) | Preparation method of triangular prism-shape ceric oxide | |
| CN103193257B (en) | Flower-shaped ceria preparation method | |
| CN109433238A (en) | Iron-nitrogen doped oxygen reduction carbon catalyst with ordered hierarchical pores and preparation method thereof | |
| CN103537237A (en) | Preparation method of Fe3O4@C@PAM core-shell magnetic nano material | |
| CN101318708B (en) | Method for synthesizing high-specific surface area nano-lanthanum ferrous acid with mesoporous silicon dioxide as mould plate | |
| CN102942206A (en) | Method for preparing cerium dioxide nanometer hollow spheres | |
| CN103979597A (en) | Preparation method of rod-like copper-cerium composite oxide | |
| CN108080000A (en) | A kind of hollow porous micro sphere catalysis material and preparation method thereof and degradation NO applications | |
| CN103638923A (en) | Rare earth element Nd-doped Bi2WO6 composite photocatalyst, preparation method therefor and applications thereof | |
| CN102951669A (en) | Method for preparing CeO2 nano solid spheres by microwave-assisted urea hydrolysis | |
| CN105536791A (en) | Preparation method of octahedral cuprous oxide catalyst for synthesizing methyl chlorosilane monomers | |
| CN103395819B (en) | Preparation method of butterfly-tie-shaped cerium dioxide | |
| CN107626319A (en) | A kind of preparation method of flower-shaped cadmium ferrite photochemical catalyst | |
| CN101508462A (en) | Process for producing flower shaped indium hydroxide powder having high specific surface area | |
| CN102698735B (en) | Method of preparing flower-ball shaped Bi4V2O11 visible-light catalyst | |
| CN101850247A (en) | Preparation method of composite oxide of cerium oxide and tin oxide | |
| CN102134089B (en) | Fusiform large-scale cerium based composite oxide powder and preparation method thereof | |
| CN103611527A (en) | Visible-light response Ce doped Bi2WO6 microcrystal, preparation method and application thereof | |
| CN103601213A (en) | Preparation method for low silicon-aluminum ratio nanosheet flower cluster-like mordenite molecular sieve | |
| CN103657662B (en) | Nickel doping zinc-oxide hierarchical structure photocatalytic nano material and preparation method thereof | |
| CN103183371B (en) | preparation method of persimmon cake-shaped cerium dioxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140820 Termination date: 20180401 |