CN109665554A - A method of it adjusting solvent burden ratio and obtains the micro-nano ceria of morphology controllable - Google Patents
A method of it adjusting solvent burden ratio and obtains the micro-nano ceria of morphology controllable Download PDFInfo
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- CN109665554A CN109665554A CN201910042312.1A CN201910042312A CN109665554A CN 109665554 A CN109665554 A CN 109665554A CN 201910042312 A CN201910042312 A CN 201910042312A CN 109665554 A CN109665554 A CN 109665554A
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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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- 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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- 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
Abstract
The invention discloses a kind of methods that adjusting solvent burden ratio obtains the micro-nano ceria of morphology controllable.With CeCl3·7H2O is cerium source, and using ammonium hydroxide or sodium hydroxide as alkali, using ethylene glycol and water as solvent, presoma is calcined the micro-nano ceria for original pattern that is maintained by the presoma of the proportion solvent structure morphology controllable by adjusting ethylene glycol and water.This method is easy to operate, obtained open column shape ceria structure novel.
Description
Technical field
The invention belongs to technical field of micro nano material preparation, are related to a kind of adjusting solvent burden ratio acquisition morphology controllable micro-nano
The method of rice ceria.
Background technique
CeO2It is a kind of important Rare Earth Functional Materials, there is excellent oxygen ion transport ability, in catalysis, shines, purple
The numerous areas extensive applications such as outer absorption, solid oxide fuel cell, polishing.CeO under nanoscale2Relative to body phase
Material, electronic structure change, and specific surface area increases, and often show some new physical properties and higher chemistry is living
Property.The performance of nano material, other than depending on the chemical composition of material, crystallographic structure, also with the size of nanocrystal, shape
The correlations such as shape, surface texture and the direction of growth, coherent condition.Therefore, develop the controllable CeO of size and shape2Nano material
Preparation method become research hotspot.
Water (solvent) thermal synthesis is under high-temperature and high-pressure conditions, and solvent is in the synthesis carried out under critical or supercriticality
Reaction；Have many advantages, such as to generate product good dispersion, purity is high, morphology controllable.In recent years, around the water of cerium based nano-material
Numerous studies have been carried out in (solvent) thermal synthesis, and the adjusting to Product size and shape may be implemented by controlling synthetic parameters.Example
Such as, Haoxin Mai etc. (J.Phys.Chem.B, 2005,109,24380-24385) is using cerous nitrate and sodium hydroxide as raw water
Thermally synthesizing nano CeO2, CeO is prepared for by controlling naoh concentration2Polyhedron, nanometer rods and nano cubic.Fu Zhou etc.
(J.Phys.Chem.C, 2007,111,1651-1657) using cerous nitrate as cerium source, polyvinylpyrrolidone (PVP) is living for surface
Property agent, pass through control nitric acid cerium concentration and PVP sized spherical nano Ce O different from cerous nitrate molar ratio hydrothermal synthesis2.China
For patent CN105565360A using cerium chloride or cerous nitrate as cerium source, urea is precipitating reagent, passes through control cerium source and urea concentration ratio
Hydro-thermal is prepared for CeO2Nanosphere, hollow nano-sphere, nanometer octahedron, nanometer rods, micron fish-bone and micron silk ball.Currently,
In the reaction system of glycol/water, with CeCl3·7H2O is cerium source, using solvent structure cerium based nano-material, and is passed through
Solvent burden ratio in change system, which regulates and controls its pattern and even controls, to be generated the research of the special appearances such as open column shape and has not been reported.
Summary of the invention
That there are product morphologies is single for the existing technical solution for preparing micro-nano ceria, not easy-regulating the shortcomings that,
The present invention provides it is a kind of adjusting solvent burden ratio obtain the micro-nano ceria of morphology controllable method, by adjust ethylene glycol/
The volume ratio of water realizes the controllable of micro-nano ceria pattern, simultaneously, moreover it is possible to generate the micro-nano of special appearance open column shape
Rice ceria.
The present invention is achieved through the following technical solutions above-mentioned purpose:
It is a kind of adjust solvent burden ratio obtain the micro-nano ceria of morphology controllable method include the following steps:
(1) solvent-thermal process presoma: by CeCl3·7H2O is dissolved in ethylene glycol or glycol/water mixed solution, then exists
Certain density aqueous slkali is added dropwise under stirring condition, obtains reaction solution, the volume ratio of ethylene glycol and water is (9 in control reaction solution
~0.15): in 1 range, within the scope of 0.06~0.12mol/L, reaction solution is transferred in reaction kettle for Ce (III) concentration,
140~220 DEG C of isothermal reactions 12~for 24 hours, after completion of the reaction, solid product obtained is centrifuged, washs drying, is obtained
To presoma；
(2) presoma is calcined: presoma calcines 1~4h at 600 DEG C to get the micro-nano ceria of morphology controllable.
Further, the aqueous slkali is ammonia or sodium hydrate aqueous solution.
Further, in the reaction solution Ce (III)/alkali molar ratio 1: in (0.9~1.2).
Further, a certain amount of polyvinylpyrrolidone (PVP K30) can be added in the reaction solution, wherein
CeCl3·7H2The mass ratio of O and polyvinylpyrrolidone is 1: (0.6~1).
The principle of the present invention is:
The OH- and Ce that initial reaction stage alkali carries supply3+In conjunction with generation Ce (OH)3, Ce (OH)3It is oxidized and generates CeO2, due to CeO2
With oxidisability, solvent ethylene glycol has reproducibility, and the two occurs a series of redox reactions, obtains the cerium base of complicated component
Mix precursor, except containing Ce (OH) in presoma3、CeO2Outside, also contain other cerium based compounds, after presoma calcining
To the CeO of single object phase2。
The beneficial effects of the present invention are:
1, the present invention controls presoma pattern by adjusting the volume ratio of glycol/water in reaction solution, thus realization pair
The regulation of micro-nano ceria pattern, when the process that glycol/water volume ratio changes from 9~0.15: 1, gained micro-nano two
Cerium oxide shows apparent pattern transition.
2, the present invention surprisingly has found, in the change procedure for adjusting glycol/water volume ratio when glycol/water volume
When than being 2: 1, the micro-nano ceria of open column shape pattern is obtained for the first time.Open column shape ceria is aoxidized as CO
Catalysts, air speed 36000mLg-1·h-1, gaseous mixture composition: 1%CO, 21%O2, 78%N2, catalytic effect is good.
Detailed description of the invention
The X-ray diffraction spectrogram of 1 solvent-thermal process difference presoma of Fig. 1 embodiment, analysis shows, presoma ingredient is multiple
It is miscellaneous, except containing CeO2(standard diagram JCPDS 34-0394), Ce (OH)3(standard diagram JCPDS19-0284) outside, also contains it
It waits for earnest phase, and with the variation of glycol/water volume ratio in reaction solution, and the relative amount of each ingredient becomes in presoma
Change.
The stereoscan photograph of 1 solvent-thermal process difference presoma of Fig. 2 embodiment, with glycol/water in reaction solution
Volume ratio changes to 0.2: 1 from 5: 1, and the pattern of presoma is converted into open column shape, rodlike, strip and sheet by gear-like.
The X-ray diffraction spectrogram of 1 presoma of Fig. 3 embodiment calcining gained micro-nano ceria of morphology controllable, with standard
Unanimously, product is pure ceria to map (JCPDS 34-0394) after illustrating calcining.
The stereoscan photograph of 1 presoma of Fig. 4 embodiment calcining gained micro-nano ceria of morphology controllable, You Tuke
See, product maintains original pattern after calcining.
The transmission electron microscope of open column shape ceria (volume ratio of glycol/water is 2: 1) prepared by Fig. 5 embodiment 1 shines
Piece.
The CO catalysis oxidation of open column shape ceria (volume ratio of glycol/water is 2: 1) prepared by Fig. 6 embodiment 1
Performance.
The stereoscan photograph of the micro-nano ceria of morphology controllable prepared by Fig. 7 embodiment 6 is reacting as seen from the figure
A certain amount of polyvinylpyrrolidone (PVP K30) is added in liquid, the volume ratio for controlling glycol/water changes to 0.2: 1 by 5: 1,
Obtained micro-nano ceria pattern variation tendency is similar with PVP is not added.
Specific embodiment
With reference to the accompanying drawing, the present invention is further described.
Embodiment 1
Solvent-thermal process presoma: respectively by 1.1177g CeCl3·7H2O is dissolved in 25ml ethylene glycol, 25ml glycol/water
Mixed solution (volume of glycol/water is respectively 20ml/5ml, 15ml/10ml, 10ml/15ml, 5ml/20ml), is then being stirred
0.6M ammonium hydroxide 5ml is added dropwise under the conditions of mixing, obtaining reaction solution, (volume ratio of glycol/water is respectively 5: 1,2: 1,1 in reaction solution
: 1,0.5: 1,0.2: 1), reaction solution be transferred to reaction kettle in, 180 DEG C of isothermal reactions for 24 hours, end of reaction, to obtained solid
(revolving speed 8000rpm, time 8min) is centrifuged in body product, is washed solid product 2 times with dehydrated alcohol, then dry through 60 DEG C
Dry 12h obtains different presomas.
Presoma calcining: presoma respectively obtains the micro-nano ceria of morphology controllable in 600 DEG C of calcining 2h.
X-ray diffraction and Electronic Speculum characterization are carried out to presoma obtained above and micro-nano ceria, characterization result is shown in
Fig. 1 to Fig. 5.
Embodiment 2
Solvent-thermal process presoma: respectively by 0.8904g CeCl3·7H2O is dissolved in 23ml ethylene glycol, 23ml glycol/water
Mixed solution (volume of glycol/water is respectively 18ml/5ml, 13ml/10ml, 8ml/15ml, 4ml/19ml), is then being stirred
0.32M sodium hydrate aqueous solution 7ml is added dropwise under the conditions of mixing, obtaining reaction solution, (volume ratio of glycol/water is respectively in reaction solution
3.286: 1,1.5: 1,0.765: 1,0.364: 1,0.154: 1), reaction solution being transferred in reaction kettle, in 160 DEG C of isothermal reactions
20h, end of reaction are centrifuged (revolving speed 8000rpm, time 8min) to solid product obtained, are washed with dehydrated alcohol
It washs solid product 2 times, then through 60 DEG C of dry 12h, obtains different presomas.
Presoma calcining: presoma respectively obtains the micro-nano ceria of morphology controllable in 600 DEG C of calcining 3h.
Embodiment 3
Solvent-thermal process presoma: respectively by 1.3413g CeCl3·7H2O is dissolved in 24ml ethylene glycol, 24ml glycol/water
Mixed solution (volume of glycol/water is respectively 19ml/5ml, 14ml/10ml, 9ml/15ml, 4ml/20ml), is then being stirred
Under the conditions of mixing be added dropwise 0.6M ammonium hydroxide 6ml, obtain reaction solution (volume ratio of glycol/water is respectively 4: 1,1.727 in reaction solution:
1,0.875: 1,0.429: 1,0.154: 1), reaction solution being transferred in reaction kettle, in 200 DEG C of isothermal reaction 16h, reacted
Finish, (revolving speed 8000rpm, time 8min) is centrifuged to solid product obtained, washs solid product 2 with dehydrated alcohol
It is secondary, then through 60 DEG C of dry 12h, obtain different presomas.
Presoma calcining: presoma respectively obtains the micro-nano ceria of morphology controllable in 600 DEG C of calcining 4h.
Embodiment 4
Solvent-thermal process presoma: respectively by 0.6678g CeCl3·7H2O is dissolved in 24ml ethylene glycol, 24ml glycol/water
Mixed solution (volume of glycol/water is respectively 20ml/4ml, 17ml/7ml, 12ml/12ml, 5ml/19ml), is then being stirred
0.36M sodium hydrate aqueous solution 6ml is added dropwise under the conditions of mixing, obtaining reaction solution, (volume ratio of glycol/water is respectively in reaction solution
4: 1,1.727: 1,0.875: 1,0.429: 1,0.154: 1), reaction solution being transferred in reaction kettle, in 220 DEG C of isothermal reactions
12h, end of reaction are centrifuged (revolving speed 8000rpm, time 8min) to solid product obtained, are washed with dehydrated alcohol
It washs solid product 2 times, then through 60 DEG C of dry 12h, obtains different presomas.
Presoma calcining: presoma respectively obtains the micro-nano ceria of morphology controllable in 600 DEG C of calcining 1h.
Embodiment 5
Solvent-thermal process presoma: respectively by 1.1177g CeCl3·7H2O is dissolved in 27ml ethylene glycol, 27ml glycol/water
Mixed solution (volume of glycol/water is respectively 19ml/8ml, 14ml/13ml, 9ml/18ml, 4ml/23ml), is then being stirred
Under the conditions of mixing be added dropwise 1.1M ammonium hydroxide 3ml, obtain reaction solution (volume ratio of glycol/water is respectively 9: 1,1.727 in reaction solution:
1,0.875: 1,0.429: 1,0.154: 1), reaction solution be transferred to reaction kettle in, 140 DEG C of isothermal reactions for 24 hours, reacted
Finish, (revolving speed 8000rpm, time 8min) is centrifuged to solid product obtained, washs solid product 2 with dehydrated alcohol
It is secondary, then through 60 DEG C of dry 12h, obtain different presomas.
Presoma calcining: presoma respectively obtains the micro-nano ceria of morphology controllable in 600 DEG C of calcining 3h.
Embodiment 6
Solvent-thermal process presoma: respectively by 1.1177g CeCl3·7H2O and 0.75g polyvinylpyrrolidone (PVP
K30) it is dissolved in 25ml ethylene glycol, (volume of glycol/water is respectively 20ml/5ml, 15ml/ to 25ml glycol/water mixed solution
10ml, 10ml/15ml, 5ml/20ml), 0.6M sodium hydrate aqueous solution 5ml is then added dropwise under agitation, is reacted
(volume ratio of glycol/water is respectively 5: 1,2: 1,1: 1,0.5: 1,0.2 to liquid in reaction solution: 1), reaction solution being transferred to reaction
In kettle, 180 DEG C of isothermal reactions for 24 hours, end of reaction, solid product obtained is centrifuged (revolving speed 8000rpm, when
Between 8min), washed solid product 2 times with dehydrated alcohol, then through 60 DEG C of dry 12h, obtain different presomas.
Presoma calcining: presoma respectively obtains the micro-nano ceria of morphology controllable in 600 DEG C of calcining 2h.
Electronic Speculum characterization is scanned to micro-nano ceria obtained above, characterization result is shown in Fig. 7.
Claims (5)
1. it is a kind of adjust solvent burden ratio obtain the micro-nano ceria of morphology controllable method, which is characterized in that specifically include as
Lower step:
(1) by CeCl3·7H2O is dissolved in ethylene glycol or glycol/water mixed solution, and certain density alkali soluble is added dropwise under stirring condition
Liquid obtains reaction solution, and reaction solution is transferred in reaction kettle, right after completion of the reaction in 140~220 DEG C of isothermal reactions 12~for 24 hours
Solid product is centrifuged, washs drying, obtains presoma；
(2) presoma is obtained into micro-nano ceria in 600 DEG C of 1~4h of calcining.
2. a kind of method for adjusting solvent burden ratio and obtaining the micro-nano ceria of morphology controllable as described in claim 1, special
Sign is that aqueous slkali described in step (1) is ammonia or sodium hydrate aqueous solution.
3. a kind of method for adjusting solvent burden ratio and obtaining the micro-nano ceria of morphology controllable as described in claim 1, special
Sign is that the volume ratio of ethylene glycol and water is in 9~0.15: 1 range in reaction solution described in step (1).
4. a kind of method for adjusting solvent burden ratio and obtaining the micro-nano ceria of morphology controllable as described in claim 1, special
Sign is that Ce (III) concentration is 0.06~0.12mol/L in reaction solution described in step (1).
5. a kind of method for adjusting solvent burden ratio and obtaining the micro-nano ceria of morphology controllable as described in claim 1, special
Sign is that Ce (III)/alkali molar ratio is in 1: 0.9~1.2 ranges in reaction solution described in step (1).
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Cited By (8)
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| CN111804303A (en) * | 2020-06-30 | 2020-10-23 | 浙江工业大学 | Preparation method of cerium dioxide/cobalt aluminum hydrotalcite material with core-shell structure |
| CN112777623A (en) * | 2021-01-14 | 2021-05-11 | 江西省科学院能源研究所 | Preparation method of cerium dioxide with triangular-like nanosheet structure |
| CN112919523A (en) * | 2021-03-16 | 2021-06-08 | 厦门稀土材料研究所 | Preparation method of hexagonal flaky rare earth cerium oxide |
| CN113769752A (en) * | 2021-09-23 | 2021-12-10 | 淮阴师范学院 | Preparation method of dodecahedron doped cerium dioxide composite photocatalyst |
| CN115124064A (en) * | 2022-06-15 | 2022-09-30 | 厦门稀土材料研究所 | Cerium dioxide nano material and preparation method and application thereof |
| CN115231604A (en) * | 2022-08-31 | 2022-10-25 | 华中科技大学 | Microstructure-controllable nano cerium dioxide catalyst based on photothermal hydrolysis hydrogen production |
| CN115259211A (en) * | 2022-07-18 | 2022-11-01 | 吉林大学 | Superfine BaTiO3Controllable preparation method of nano crystal |
| CN115472445A (en) * | 2022-09-29 | 2022-12-13 | 贵州民族大学 | Method for preparing super-capacitor electrode material by using cerium dioxide |
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| CN111804303B (en) * | 2020-06-30 | 2023-03-28 | 浙江工业大学 | Preparation method of cerium dioxide/cobalt aluminum hydrotalcite material with core-shell structure |
| CN111804303A (en) * | 2020-06-30 | 2020-10-23 | 浙江工业大学 | Preparation method of cerium dioxide/cobalt aluminum hydrotalcite material with core-shell structure |
| CN112777623A (en) * | 2021-01-14 | 2021-05-11 | 江西省科学院能源研究所 | Preparation method of cerium dioxide with triangular-like nanosheet structure |
| CN112919523A (en) * | 2021-03-16 | 2021-06-08 | 厦门稀土材料研究所 | Preparation method of hexagonal flaky rare earth cerium oxide |
| CN112919523B (en) * | 2021-03-16 | 2022-01-28 | 厦门稀土材料研究所 | Preparation method of hexagonal flaky rare earth cerium oxide |
| CN113769752A (en) * | 2021-09-23 | 2021-12-10 | 淮阴师范学院 | Preparation method of dodecahedron doped cerium dioxide composite photocatalyst |
| CN113769752B (en) * | 2021-09-23 | 2023-08-22 | 淮阴师范学院 | Preparation method of dodecahedron iron doped cerium dioxide composite photocatalyst |
| CN115124064A (en) * | 2022-06-15 | 2022-09-30 | 厦门稀土材料研究所 | Cerium dioxide nano material and preparation method and application thereof |
| CN115124064B (en) * | 2022-06-15 | 2023-08-29 | 厦门稀土材料研究所 | Cerium dioxide nano material and preparation method and application thereof |
| CN115259211A (en) * | 2022-07-18 | 2022-11-01 | 吉林大学 | Superfine BaTiO3Controllable preparation method of nano crystal |
| CN115259211B (en) * | 2022-07-18 | 2023-11-24 | 吉林大学 | Superfine BaTiO 3 Controllable preparation method of nanocrystals |
| CN115231604A (en) * | 2022-08-31 | 2022-10-25 | 华中科技大学 | Microstructure-controllable nano cerium dioxide catalyst based on photothermal hydrolysis hydrogen production |
| CN115472445A (en) * | 2022-09-29 | 2022-12-13 | 贵州民族大学 | Method for preparing super-capacitor electrode material by using cerium dioxide |
| CN115472445B (en) * | 2022-09-29 | 2024-03-29 | 贵州民族大学 | Method for preparing super capacitor electrode material by utilizing cerium dioxide |
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