CN103395819A - Preparation method of butterfly-tie-shaped cerium dioxide - Google Patents
Preparation method of butterfly-tie-shaped cerium dioxide Download PDFInfo
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- CN103395819A CN103395819A CN2013103396472A CN201310339647A CN103395819A CN 103395819 A CN103395819 A CN 103395819A CN 2013103396472 A CN2013103396472 A CN 2013103396472A CN 201310339647 A CN201310339647 A CN 201310339647A CN 103395819 A CN103395819 A CN 103395819A
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Abstract
The invention discloses a preparation method of butterfly-tie-shaped cerium dioxide, and relates to the preparation method of the cerium dioxide. The preparation method aims to solve the technical problems that the morphology of the cerium dioxide prepared by preparation methods in the prior art is mainly rod-shaped, line-shaped, tube-shaped and spherical. The preparation method comprises the following steps: first, mixing Ce(NO3)3.6H2O and L-cysteine, adding into distilled water and stirring until the Ce(NO3)3.6H2O and the L-cysteine are completely dissolved, then adding NaOH, and continuing to stir for 30 min to obtain a mixed liquid; and second, transferring the mixed liquid into a reaction kettle for reaction, naturally cooling to the room temperature, washing a sample with the distilled water until the sample being free of impurity, filtering, drying, and then calcining, thus obtaining the butterfly-tie-shaped cerium dioxide. The butterfly-tie-shaped cerium dioxide prepared by the preparation method is butterfly-tie-shaped, and both ends of the butterfly-tie-shaped cerium dioxide are bound-branch-shaped, the sample has complete morphology, the size is about 18 [mu]m, the size distribution is uniform, both ends of the sample are multilevel structures, and have pore structures. The preparation method belongs to the field of preparation of oxides.
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 to the Economic development of China many benefits.CeO
2As a kind of important rare earth oxide, make it show excellent the oxygen ability of storing and charge-exchange ability owing to having unique 4f electronic structure, at three-way catalyst, fuel cell, all have application in the fields such as photochemical catalysis and pollutant treatment.
Development along with science and technology, 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 the material pattern can produce considerable influence to material property, how to realize that material that controlled preparation has a suitable pattern 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.At present the pattern of common cerium dioxide is mainly: bar-shaped, wire, tubulose and the shape such as spherical are still more rare for the report of the cerium dioxide of other special appearances.This shows to have higher scientific research and learning value for the preparation research of special appearance cerium dioxide.And,, if the special appearance cerium dioxide that makes has comparatively unique performance, also can bring wide application prospect for it.
Summary of the invention
The objective of the invention is provides a kind of preparation method of bow tie cerium dioxide for the cerium dioxide pattern that solves the preparation of existing method is mainly bar-shaped, wire, tubulose and spherical technical problem.
The preparation method of bow tie cerium dioxide carries out according to following steps:
One, with the Ce (NO of 0.01mol～0.03mol
3)
36H
2The Cys of O and 0.01mol～0.03mol is mixed to join in 30ml distilled water to be stirred to fully and dissolves, then adds 0.04mol～0.08mol NaOH, continues to stir 30min, obtains mixed solution;
Two, mixed solution is changed in reactor and react 12h～36h under the condition of 140 ℃～180 ℃, reactor is taken out and naturally cools to room temperature, with the distilled water wash sample to inclusion-free, filter, dry 12h under 80 ℃～100 ℃, and then, at 400 ℃ of calcining 1h, obtain the bow tie cerium dioxide.
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 bow tie in conjunction with hydrothermal method.The cerium dioxide of the present invention preparation is bow tie, and two ends are Shu Zhizhuan, and sample has complete pattern, and size is about 18 μ m, and the size substep is comparatively even, and the sample two ends are multilevel hierarchy, and the tool pore texture.This bow tie cerium dioxide has higher degree of crystallization, larger specific surface area, than the gap structure of horn of plenty and stronger oxygen ability and the electron transport ability stored, more be conducive to adhering to of reactant, intensified response efficiency greatly.
The present invention adopts amino acid to prepare cerium dioxide as tensio-active agent, and the cerium dioxide pattern that obtains is novel, and cost simple to operate is low, and the product purity that obtains is high.
Description of drawings
Fig. 1 is the XRD figure of the bow tie of experiment one preparation;
Fig. 2 is the SEM figure of the bow tie cerium dioxide of experiment one preparation;
Fig. 3 is the high power SEM figure of the bow tie cerium dioxide of experiment one preparation;
Fig. 4 is the SEM figure of the bow tie cerium dioxide of experiment two preparations;
Fig. 5 tests the SEM figure of the bow tie cerium dioxide of three preparations;
Fig. 6 tests the SEM figure of the bow tie cerium dioxide of four preparations.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: in present embodiment, the preparation method of bow tie cerium dioxide carries out according to following steps:
One, with the Ce (NO of 0.01mol～0.03mol
3)
36H
2The Cys of O and 0.01mol～0.03mol is mixed to join in 30ml distilled water to be stirred to fully and dissolves, then adds 0.04mol～0.08mol NaOH, continues to stir 30min, obtains mixed solution;
Two, mixed solution is changed in reactor and react 12h～36h under the condition of 140 ℃～180 ℃, reactor is taken out and naturally cools to room temperature, with the distilled water wash sample to inclusion-free, filter, dry 12h under 80 ℃～100 ℃, and then, at 400 ℃ of calcining 1h, obtain the bow tie cerium dioxide.
Embodiment two: that present embodiment is different from embodiment one is the Ce (NO 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 one of embodiment one or two is the Ce (NO described in step 1
3)
36H
2The mol ratio of O and Cys is 2:1.Other is not identical with one of embodiment one or two.
Embodiment four: that present embodiment is different from one of embodiment one to three is the Ce (NO described in step 1
3)
36H
2The mol ratio of O and Cys is 1:1.Other is identical with one of embodiment one to three.
Embodiment five: that present embodiment is different from one of embodiment one to four is the Ce (NO described in step 1
3)
36H
2The mol ratio of O and Cys is 1:2.Other is identical with one of embodiment one to four.
Embodiment six: that present embodiment is different from one of embodiment one to five is the Ce (NO described in step 1
3)
36H
2The mol ratio of O and Cys is 1:3.Other is identical with one of embodiment one to five.
Embodiment seven: present embodiment is different from one of embodiment one to six is that the add-on of NaOH in step 1 is 0.06mol.Other is identical with one of embodiment one to six.
Embodiment eight: what present embodiment was different from one of embodiment one to seven is in step 2, mixed solution to be changed in reactor and react 24h under the condition of 160 ℃.Other is identical with one of embodiment one to seven.
Embodiment nine: present embodiment is different from one of embodiment one to eight be in step 2 under 90 ℃ dry 12h.Other is identical with one of embodiment one to eight.
Adopt following experimental verification effect of the present invention:
Experiment one:
The preparation method of bow tie cerium dioxide carries out according to following steps:
One, with the Ce (NO of 0.01mol
3)
36H
2The Cys of O and 0.03mol is mixed to join in 30ml distilled water to be stirred to fully and dissolves, then adds 0.06molNaOH, continues to stir 30min, obtains mixed solution;
Two, mixed solution is changed in reactor and react 24h under the condition of 180 ℃, reactor is taken out and naturally cools to room temperature, use the distilled water wash sample to inclusion-free, filter, dry 12h under 80 ℃, and then, at 400 ℃ of calcining 1h, obtain the bow tie cerium dioxide.
As can be seen from Figure 1 in 2 θ=28.6 °, 33.1 °, 47.4 °, 56.3 ° strong characteristic diffraction peak occurred, have 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
As can be seen from Figure 2 the prepared sample of this experiment is bow tie, and two ends are Shu Zhizhuan, and sample has complete pattern, and size is about 18 μ m, and the size substep is comparatively even, and the sample two ends are multilevel hierarchy, and have certain pore texture.
Experiment two:
The preparation method of bow tie cerium dioxide carries out according to following steps:
One, with the Ce (NO of 0.03mol
3)
36H
2The Cys of O and 0.01mol is mixed to join in 30ml distilled water to be stirred to fully and dissolves, then adds 0.06molNaOH, continues to stir 30min, obtains mixed solution;
Two, mixed solution is changed in reactor and react 24h under the condition of 180 ℃, reactor is taken out and naturally cools to room temperature, use the distilled water wash sample to inclusion-free, filter, dry 12h under 80 ℃, and then, at 400 ℃ of calcining 1h, obtain the bow tie cerium dioxide.
The cerium dioxide of this experiment preparation is bow tie, and two ends are Shu Zhizhuan, and sample has complete pattern, and size is about 18 μ m, and the size substep is comparatively even, and the sample two ends are multilevel hierarchy, and have certain pore texture.
Experiment three:
The preparation method of bow tie cerium dioxide carries out according to following steps:
One, with the Ce (NO of 0.01mol
3)
36H
2The Cys of O and 0.01mol is mixed to join in 30ml distilled water to be stirred to fully and dissolves, then adds 0.08mol NaOH, continues to stir 30min, obtains mixed solution;
Two, mixed solution is changed in reactor and react 36h under the condition of 180 ℃, reactor is taken out and naturally cools to room temperature, use the distilled water wash sample to inclusion-free, filter, dry 12h under 100 ℃, and then, at 400 ℃ of calcining 1h, obtain the bow tie cerium dioxide.
The cerium dioxide of this experiment preparation is bow tie, and two ends are Shu Zhizhuan, and sample has complete pattern, and size is about 20 μ m, and the size substep is comparatively even, and the sample two ends are multilevel hierarchy, and have certain pore texture.
Experiment four:
The preparation method of bow tie cerium dioxide carries out according to following steps:
One, with the Ce (NO of 0.01mol
3)
36H
2The Cys of O and 0.03mol is mixed to join in 30ml distilled water to be stirred to fully and dissolves, then adds 0.08mol NaOH, continues to stir 30min, obtains mixed solution;
Two, mixed solution is changed in reactor and react 12h under the condition of 140 ℃, reactor is taken out and naturally cools to room temperature, use the distilled water wash sample to inclusion-free, filter, dry 12h under 80 ℃, and then, at 400 ℃ of calcining 1h, obtain the bow tie cerium dioxide.
The cerium dioxide of this experiment preparation is bow tie, and two ends are Shu Zhizhuan, and sample has complete pattern, and size is about 18 μ m, and the size substep is comparatively even, and the sample two ends are multilevel hierarchy, and have certain pore texture.
Experiment five:
The preparation method of bow tie cerium dioxide carries out according to following steps:
One, with the Ce (NO of 0.02mol
3)
36H
2The Cys of O and 0.01mol is mixed to join in 30ml distilled water to be stirred to fully and dissolves, then adds 0.04molNaOH, continues to stir 30min, obtains mixed solution;
Two, mixed solution is changed in reactor and react 24h under the condition of 140 ℃, reactor is taken out and naturally cools to room temperature, use the distilled water wash sample to inclusion-free, filter, dry 12h under 90 ℃, and then, at 400 ℃ of calcining 1h, obtain the bow tie cerium dioxide.
The cerium dioxide of this experiment preparation is bow tie, and two ends are Shu Zhizhuan, and sample has complete pattern, and size is about 18 μ m, and the size substep is comparatively even, and the sample two ends are multilevel hierarchy, and have certain pore texture.
Experiment six:
The preparation method of bow tie cerium dioxide carries out according to following steps:
One, with the Ce (NO of 0.03mol
3)
36H
2The Cys of O and 0.01mol is mixed to join in 30ml distilled water to be stirred to fully and dissolves, then adds 0.06mol NaOH, continues to stir 30min, obtains mixed solution;
Two, mixed solution is changed in reactor and react 36h under the condition of 140 ℃, reactor is taken out and naturally cools to room temperature, use the distilled water wash sample to inclusion-free, filter, dry 12h under 90 ℃, and then, at 400 ℃ of calcining 1h, obtain the bow tie cerium dioxide.
The cerium dioxide of this experiment preparation is bow tie, and two ends are Shu Zhizhuan, and sample has complete pattern, and size is about 18 μ m, and the size substep is comparatively even, and the sample two ends are multilevel hierarchy, and have certain pore texture.
Claims (9)
1. the preparation method of bow tie cerium dioxide is characterized in that the preparation method of bow tie cerium dioxide carries out according to following steps:
One, with the Ce (NO of 0.01mol～0.03mol
3)
36H
2The Cys of O and 0.01mol～0.03mol is mixed to join in 30ml distilled water to be stirred to fully and dissolves, then adds 0.04mol～0.08mol NaOH, continues to stir 30min, obtains mixed solution;
Two, mixed solution is changed in reactor and react 12h～36h under the condition of 140 ℃～180 ℃, reactor is taken out and naturally cools to room temperature, with the distilled water wash sample to inclusion-free, filter, dry 12h under 80 ℃～100 ℃, and then, at 400 ℃ of calcining 1h, obtain the bow tie cerium dioxide.
2. the preparation method of bow tie cerium dioxide according to claim 1, is characterized in that the Ce (NO described in step 1
3)
36H
2The mol ratio of O and Cys is 3:1.
3. the preparation method of bow tie cerium dioxide according to claim 1, is characterized in that the Ce (NO described in step 1
3)
36H
2The mol ratio of O and Cys is 2:1.
4. the preparation method of bow tie cerium dioxide according to claim 1, is characterized in that the Ce (NO described in step 1
3)
36H
2The mol ratio of O and Cys is 1:1.
5. the preparation method of bow tie cerium dioxide according to claim 1, is characterized in that the Ce (NO described in step 1
3)
36H
2The mol ratio of O and Cys is 1:2.
6. the preparation method of bow tie cerium dioxide according to claim 1, is characterized in that the Ce (NO described in step 1
3)
36H
2The mol ratio of O and Cys is 1:3.
7. the preparation method of bow tie cerium dioxide according to claim 1, the add-on that it is characterized in that NaOH in step 1 is 0.06mol.
8. the preparation method of bow tie cerium dioxide according to claim 1, is characterized in that in step 2, mixed solution being changed in reactor and react 24h under the condition of 160 ℃.
9. the preparation method of bow tie cerium dioxide according to claim 1, is characterized in that in step 2 dry 12h under 90 ℃.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103816924A (en) * | 2014-03-11 | 2014-05-28 | 黑龙江大学 | Preparation method of sulfur-doped cerium dioxide mesoporous hollow sphere photocatalysts |
| CN106384679A (en) * | 2016-10-13 | 2017-02-08 | 福州大学 | Method for preparing dumbbell type CeO2 super capacitor electrode material |
| CN107555464A (en) * | 2017-08-23 | 2018-01-09 | 电子科技大学 | A kind of CeO of bow tie2Nano material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030215378A1 (en) * | 2002-05-15 | 2003-11-20 | Xiao-Dong Zhou | Method for preparation of nanometer cerium-based oxide particles |
| CN102992384A (en) * | 2012-12-12 | 2013-03-27 | 黑龙江大学 | Preparation method of triangular prism-shape ceric oxide |
| CN103183371A (en) * | 2013-04-01 | 2013-07-03 | 黑龙江大学 | Preparation method of persimmon cake-shaped cerium dioxide |
-
2013
- 2013-08-06 CN CN201310339647.2A patent/CN103395819B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030215378A1 (en) * | 2002-05-15 | 2003-11-20 | Xiao-Dong Zhou | Method for preparation of nanometer cerium-based oxide particles |
| CN102992384A (en) * | 2012-12-12 | 2013-03-27 | 黑龙江大学 | Preparation method of triangular prism-shape ceric oxide |
| CN103183371A (en) * | 2013-04-01 | 2013-07-03 | 黑龙江大学 | Preparation method of persimmon cake-shaped cerium dioxide |
Non-Patent Citations (1)
| Title |
|---|
| 周艳慧: "CeO2@Au核壳结构纳米粒子的制备与表征", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103816924A (en) * | 2014-03-11 | 2014-05-28 | 黑龙江大学 | Preparation method of sulfur-doped cerium dioxide mesoporous hollow sphere photocatalysts |
| CN106384679A (en) * | 2016-10-13 | 2017-02-08 | 福州大学 | Method for preparing dumbbell type CeO2 super capacitor electrode material |
| CN107555464A (en) * | 2017-08-23 | 2018-01-09 | 电子科技大学 | A kind of CeO of bow tie2Nano material and preparation method thereof |
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| CN103395819B (en) | 2015-02-04 |
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