CN101508456A - Method for auxiliary preparation of different-shape nano-cerium oxide with microwave - Google Patents
Method for auxiliary preparation of different-shape nano-cerium oxide with microwave Download PDFInfo
- Publication number
- CN101508456A CN101508456A CNA200910026021XA CN200910026021A CN101508456A CN 101508456 A CN101508456 A CN 101508456A CN A200910026021X A CNA200910026021X A CN A200910026021XA CN 200910026021 A CN200910026021 A CN 200910026021A CN 101508456 A CN101508456 A CN 101508456A
- Authority
- CN
- China
- Prior art keywords
- microwave
- cerium oxide
- mixture
- different
- preparation
- 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.)
- Pending
Links
Images
Abstract
The invention belongs to the technical field of nanometer material preparation, in particular to a method for preparing nanometer cerium oxide with different appearances by microwave assistance. The method comprises the following steps: 1) preparing 0.01 to 0.1 mol/L aqueous solution of Ce(NO3)3 at room temperature; adding the Ce(NO3)3 aqueous solution, glycol, oleic acid and tert-butylamine into a high-temperature reaction kettle according to volume ratio of 100: (80-120) : (5-10) : (0.6-1.2) without any stirring; 2) sealing and placing the high-temperature reaction kettle in a microwave environment to be heated for 5 to 10 minutes with microwave power of between 100 and 1,000 watt; and 3) after reaction of step (2) is finished, cooling the obtained mixture till room temperature, adding acetone accounting for 3 to 5 times of the mixture by volume into the mixture to wash the glycol and the oleic acid, centrifugalizing the mixture after ultrasonic treatment, washing the centrifugalized solid by absolute ethyl alcohol, carrying out ultrasonic treatment and centrifugalization on the solid for 5 to 6 times, and drying the obtained solid powder to obtain the cerium oxide nanometer material. The method has the advantages of low cost, simple process and good controllability.
Description
Technical field
The invention belongs to the nano material preparation technical field, particularly a kind of method of auxiliary preparation of different-shape nano-cerium oxide with microwave.
Background technology
Because the special construction of nanoparticle, make nano material and traditional material some in nature (as optics, electricity etc.) bigger difference is arranged, and obtained widespread use in electronics, optics, chemical stoneware, biology and medicine and other fields.Nano-oxide is an integral part in the nano material, so its preparation, structure, performance and application have become one of focus of various countries researchist concern.Cerium oxide is the extremely wide light rare earths oxide compound of a kind of purposes, has N-type semiconductor character, is widely used in fields such as fuel cell, luminescent material, glass decolouring finings, catalyzer, electronic ceramics, uv-absorbing material and photochemical catalysis.The photocatalytic oxidation degradation pollutent is nearly 20 years a kind of energy-conservation, the environmental protection new technologies efficiently that grow up, and semiconductor material is applied to photocatalysis field curbs environmental pollution and become the research focus.Photocatalyst can be used in the degradation water and airborne organic pollutant, and with traditional pollution treatment measures comparison, the advantage of photocatalytic method is the pollutent exhaustive oxidation to be decomposed into CO and H
2Non-toxic substances such as O.In numerous semiconductor materials, cerium oxide with its catalytic activity height, stability is strong, universality is good, harmless, the improvement that can work, be applicable to low concentration pollutant at normal temperatures and pressures and cheap and easy to get and enjoy attention.
The method for preparing nano-cerium oxide is a lot, and at present the most frequently used is liquid phase method.Liquid phase method mainly comprises: the precipitator method, sol-gel method, hydrothermal method, microemulsion method, spray reaction method etc.For example Chinese patent CN1186262, CN1724380A, CN1760132A, CN1785815A, CN1792456A etc.The common complex process of these preparation methods, the preparation cost height, the nano material particle diameter of preparation, the controllability of pattern are relatively poor.
For this reason, the method for seeking a kind of low cost, efficient controllable preparation cerium oxide nano materials is badly in need of very much.Microwave is a kind of hertzian wave, hertzian wave comprises electric field and magnetic field, electric field makes the charged particle setting in motion and has a kind of power, thereby because the motion of charged particle further polarizes polarized particle, the electricity of microwave changes fast with the relevant force direction of magnetic part, makes himself temperature rising thereby produce friction.The ultimate principle of microwave heating that Here it is.The complexity that can simplify reaction in the chemical reaction is greatly introduced in microwave heating, simultaneously because microwave heating can make reaction soln reach a high temperature at short notice, so can reduce the time of reaction greatly.
Summary of the invention
The method that the purpose of this invention is to provide a kind of auxiliary preparation of different-shape nano-cerium oxide with microwave.
The step of the technical solution used in the present invention is as follows:
1) compound concentration is 0.01～0.1mol/LCe (NO under the room temperature
3)
3The aqueous solution, with Ce (NO3)
3The aqueous solution, ethylene glycol, oleic acid and tertiary butyl ammonium be 100:(80～120 by volume): (5～10): (0.6～1.2) joins in the pyroreaction still, without any need for stirring;
2) pyroreaction still sealing postposition is gone into heating 5～10min under the microwave environment, microwave power is 100～1000w.
3) treat that step (2) reaction finishes after, the mixture that obtains is cooled to room temperature, the acetone that adds volume and be 3～5 times of volume of mixture in mixture is in order to flush away ethylene glycol and oleic acid, after the supersound process solid after mixture centrifugation, the separation is added absolute ethanol washing again, carry out supersound process and centrifugation again, repeat 5～6 times, the pressed powder drying with obtaining promptly obtains cerium oxide nano materials.
Among the above-mentioned preparation method, the pyroreaction still has tightness system, and inner bag is coated with tetrafluoroethylene.
Among the above-mentioned preparation method, the time of supersound process is 5～10min.
Among the above-mentioned preparation method, the condition of centrifugation is: with mixture centrifugation 5～10min under 10000 rev/mins of speed.
Among the above-mentioned preparation method, preparation Ce (NO
3)
3The aqueous solution adopts is that mass percentage concentration is 99.9% six water cerous nitrate Ce (NO
3)
36H
2O,
Among the above-mentioned preparation method, ethylene glycol is that mass percentage concentration is 99.8% no water glycol;
Among the above-mentioned preparation method, oleic mass percentage concentration is 99% tertiary butyl ammonium C
12H
27N.
Among the above-mentioned preparation method, dehydrated alcohol is an analytical pure;
Among the above-mentioned preparation method, acetone is analytical pure.
Above reagent does not all pass through purification process;
The beneficial effect that the present invention has is:
1) this preparation method is simple, and cost is low, and condition is not harsh;
2) this preparation method can prepare the cerium oxide nano materials of different-shape, comprises cerium oxide nano square, cerium oxide nano particle, cerium oxide nano-rod, cerium oxide nano line etc.
3), reached artificial controllability for the microtexture and the size of synthetic cerium oxide nano materials by regulating experiment parameter.
This preparation method is significant for catalytic performance, optical characteristics and the pattern of research cerium oxide nano materials and the relation of size, has very high practical value and rosy prospect for the exploitation cerium oxide nano materials in the application of industrial application simultaneously.
Description of drawings
Fig. 1 is the CeO according to embodiment one preparation
2The transmission electron microscope photo of nanometer square;
Fig. 2 is the CeO according to embodiment two preparations
2The transmission electron microscope photo of nanometer rod;
Fig. 3 is the CeO according to embodiment three preparations
2The transmission electron microscope photo of nano wire;
Fig. 4 is the CeO according to embodiment four preparations
2The transmission electron microscope photo of nanoparticle.
Embodiment
Embodiment 1:
Carry out according to preparation process, under the room temperature with Ce (NO
3)
3Being mixed with concentration is the 0.01mol/l aqueous solution, in order with 0.01mol/l Ce (NO
3)
3Aqueous solution 100ml, ethylene glycol 100ml, oleic acid 8ml, tertiary butyl ammonium 1.2ml joins and has tightness system, in the pyroreaction still of inner bag plating one deck tetrafluoroethylene, without any need for stirring.Heat 10min with inserting in the 2.5GHz household microwave oven after the reactor sealing.The heating power of microwave oven is 900w.After question response finishes, the mixture that obtains is cooled to room temperature, the acetone that adds volume and be volume of mixture 700ml in mixture is in order to flush away ethylene glycol and oleic acid, and supersound process 5min then is with mixture centrifugation 5min under 10000 rev/mins of speed.Solid after the separation adds absolute ethanol washing again, and supersound process, centrifugation obtain the cerium oxide nano square after the pressed powder that repeats to obtain for 5 times places the dry 6h of vacuum drying oven.The test of transmission electron microscope observation (TEM) is that dried powder supersound process is dispersed in the toluene, then with drips of solution on the copper mesh that is coated with carbon film, drying at room temperature, TEM model are JEOL200CX.
Embodiment 2:
Carry out according to preparation process, under the room temperature with Ce (NO
3)
3Being mixed with concentration is the 0.05mol/l aqueous solution, in order with 0.05mol/l Ce (NO
3)
3Aqueous solution 100ml, ethylene glycol 120ml, oleic acid 10ml, tertiary butyl ammonium 0.8ml joins and has tightness system, in the pyroreaction still of inner bag plating one deck tetrafluoroethylene, without any need for stirring.Heat 10min with inserting in the 2.5GHz household microwave oven after the reactor sealing.The heating power of microwave oven is 1000w.After question response finishes, the mixture that obtains is cooled to room temperature, the acetone that adds volume and be volume of mixture 1000ml in mixture is in order to flush away ethylene glycol and oleic acid, and supersound process 5min then is with mixture centrifugation 7min under 10000 rev/mins of speed.Solid after the separation adds absolute ethanol washing again, and supersound process, centrifugation obtain cerium oxide nano-rod after the pressed powder that repeats to obtain for 5 times places the dry 6h of vacuum drying oven.The test of transmission electron microscope observation (TEM) is that dried powder supersound process is dispersed in the toluene, then with drips of solution on the copper mesh that is coated with carbon film, drying at room temperature, TEM model are JEOL200CX.
Embodiment 3:
Carry out according to preparation process, under the room temperature with Ce (NO
3)
3Being mixed with concentration is the 0.1mol/l aqueous solution, in order with 0.1mol/lCe (NO
3)
3Aqueous solution 100ml, ethylene glycol 80ml, oleic acid 8ml, tertiary butyl ammonium 0.6ml joins and has tightness system, in the pyroreaction still of inner bag plating one deck tetrafluoroethylene, without any need for stirring.Heat 10min with inserting in the 2.5GHz household microwave oven after the reactor sealing.The heating power of microwave oven is 600w.After question response finishes, the mixture that obtains is cooled to room temperature, the acetone that adds volume and be volume of mixture 1000ml in mixture is in order to flush away ethylene glycol and oleic acid, and supersound process 5min then is with mixture centrifugation 7min under 10000 rev/mins of speed.Solid after the separation adds absolute ethanol washing again, and supersound process, centrifugation obtain the cerium oxide nano line after the pressed powder that repeats to obtain for 6 times places the dry 10h of vacuum drying oven.The test of transmission electron microscope observation (TEM) is that dried powder supersound process is dispersed in the toluene, then with drips of solution on the copper mesh that is coated with carbon film, drying at room temperature, TEM model are JEOL200CX.
Embodiment 4:
Carry out according to preparation process, under the room temperature with Ce (NO
3)
3Being mixed with concentration is the 0.01mol/l aqueous solution, in order with 0.01mol/l Ce (NO
3)
3Aqueous solution 100ml, ethylene glycol 80ml, oleic acid 5ml, tertiary butyl ammonium 0.5ml joins and has tightness system, in the pyroreaction still of inner bag plating one deck tetrafluoroethylene, without any need for stirring.Heat 5min with inserting in the 2.5GHz household microwave oven after the reactor sealing.The heating power of microwave oven is 300w.After question response finishes, the mixture that obtains is cooled to room temperature, the acetone that adds volume and be volume of mixture 800ml in mixture is in order to flush away ethylene glycol and oleic acid, and supersound process 5min then is with mixture centrifugation 10min under 10000 rev/mins of speed.Solid after the separation adds absolute ethanol washing again, and supersound process, centrifugation obtain cerium oxide nano particle after the pressed powder that repeats to obtain for 5 times places the dry 6h of vacuum drying oven.The test of transmission electron microscope observation (TEM) is that dried powder supersound process is dispersed in the toluene, then with drips of solution on the copper mesh that is coated with carbon film, drying at room temperature, TEM model are JEOL200CX.
Claims (6)
1, a kind of method of auxiliary preparation of different-shape nano-cerium oxide with microwave, step is as follows:
1) compound concentration is 0.01～0.1mol/LCe (NO under the room temperature
3)
3The aqueous solution, with Ce (NO3)
3The aqueous solution, ethylene glycol, oleic acid and tertiary butyl ammonium be 100:(80～120 by volume): (5～10): (0.6～1.2) joins in the pyroreaction still, without any need for stirring;
2) pyroreaction still sealing postposition is gone into heating 5～10min under the microwave environment, microwave power is 100～1000w.
3) treat that step (2) reaction finishes after, the mixture that obtains is cooled to room temperature, the acetone that adds volume and be 3～5 times of volume of mixture in mixture is in order to flush away ethylene glycol and oleic acid, after the supersound process solid after mixture centrifugation, the separation is added absolute ethanol washing again, carry out supersound process and centrifugation again, repeat 5～6 times, the pressed powder drying with obtaining promptly obtains cerium oxide nano materials.
2, the method for the described a kind of auxiliary preparation of different-shape nano-cerium oxide with microwave of claim 1 is characterized in that: the pyroreaction still has tightness system, and inner bag is coated with tetrafluoroethylene.
3, the method for the described a kind of auxiliary preparation of different-shape nano-cerium oxide with microwave of claim 1 is characterized in that: the time of supersound process is 5～10min.
4, the method for the described a kind of auxiliary preparation of different-shape nano-cerium oxide with microwave of claim 1 is characterized in that: the condition of centrifugation is: with mixture centrifugation 5～10min under 10000 rev/mins of speed.
5, the method for the described a kind of auxiliary preparation of different-shape nano-cerium oxide with microwave of claim 1 is characterized in that: preparation Ce (NO
3)
3The aqueous solution adopts is that mass percentage concentration is 99.9% six water cerous nitrate Ce (NO
3)
36H
2O.
6, the method for the described a kind of auxiliary preparation of different-shape nano-cerium oxide with microwave of claim 1 is characterized in that: ethylene glycol is that mass percentage concentration is 99.8% no water glycol; Oleic mass percentage concentration is 99% tertiary butyl ammonium C
12H
27N; Dehydrated alcohol is an analytical pure; Acetone is analytical pure; Above reagent does not all pass through purification process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200910026021XA CN101508456A (en) | 2009-03-17 | 2009-03-17 | Method for auxiliary preparation of different-shape nano-cerium oxide with microwave |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200910026021XA CN101508456A (en) | 2009-03-17 | 2009-03-17 | Method for auxiliary preparation of different-shape nano-cerium oxide with microwave |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101508456A true CN101508456A (en) | 2009-08-19 |
Family
ID=41001017
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA200910026021XA Pending CN101508456A (en) | 2009-03-17 | 2009-03-17 | Method for auxiliary preparation of different-shape nano-cerium oxide with microwave |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101508456A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101962203A (en) * | 2010-09-30 | 2011-02-02 | 常州大学 | Method for synthesizing nano cerium oxide with different morphologies by hydrothermal method |
| CN103011235A (en) * | 2012-11-28 | 2013-04-03 | 江西师范大学 | Industrial microwave rapid synthesis method of ultra-large specific surface area nano cerium dioxide |
| CN103588175A (en) * | 2013-11-27 | 2014-02-19 | 昆明理工大学 | Method for making nano-powder through ultrasonic atomization-microwave pyrolysis |
| CN106186038A (en) * | 2016-07-19 | 2016-12-07 | 仇颖超 | The method that oleic acid prepares hollow cerium oxide gas sensitive is utilized under a kind of low temperature |
| CN109133140A (en) * | 2018-08-27 | 2019-01-04 | 江西师范大学 | A method of preparing cerium oxide nanoparticles |
-
2009
- 2009-03-17 CN CNA200910026021XA patent/CN101508456A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101962203A (en) * | 2010-09-30 | 2011-02-02 | 常州大学 | Method for synthesizing nano cerium oxide with different morphologies by hydrothermal method |
| CN101962203B (en) * | 2010-09-30 | 2013-05-08 | 常州大学 | Method for synthesizing nano cerium oxide with different morphologies by hydrothermal method |
| CN103011235A (en) * | 2012-11-28 | 2013-04-03 | 江西师范大学 | Industrial microwave rapid synthesis method of ultra-large specific surface area nano cerium dioxide |
| CN103588175A (en) * | 2013-11-27 | 2014-02-19 | 昆明理工大学 | Method for making nano-powder through ultrasonic atomization-microwave pyrolysis |
| CN106186038A (en) * | 2016-07-19 | 2016-12-07 | 仇颖超 | The method that oleic acid prepares hollow cerium oxide gas sensitive is utilized under a kind of low temperature |
| CN109133140A (en) * | 2018-08-27 | 2019-01-04 | 江西师范大学 | A method of preparing cerium oxide nanoparticles |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103934012B (en) | SnS 2/ g-C 3n 4composite nano plate photochemical catalyst and preparation method | |
| CN107469851B (en) | Ultrathin porous N-doped g-C3N4Photocatalyst and preparation method thereof | |
| CN104128184B (en) | A kind of float type CoFe2O4/TiO2/ float bead composite photochemical catalyst and preparation method thereof | |
| CN105854863B (en) | A kind of C/ZnO/TiO2The preparation method of composite Nano catalysis material | |
| CN103657623B (en) | Microballoon-type titanium dioxide photocatalyst and preparation method thereof | |
| CN102350354B (en) | Magnetically supported titanium dioxide photocatalyst and preparation method thereof | |
| CN104190445B (en) | BiOBr base heterojunction of a kind of visible light catalysis activity and preparation method thereof | |
| CN104998672A (en) | G-C3N4/{001}TiO2 composite visible-light-driven photocatalyst and preparation method and application thereof | |
| CN101966452B (en) | Method for preparing visible light-responded LaVO4 and TiO2 composite nanotube | |
| CN102407147A (en) | Preparation method and application of ZnIn2S4-graphene composited photochemical catalyst | |
| CN101508456A (en) | Method for auxiliary preparation of different-shape nano-cerium oxide with microwave | |
| CN110152711A (en) | A kind of CeO2@MoS2/g-C3N4Three-element composite photocatalyst and preparation method thereof | |
| CN103531365B (en) | The preparation method of electrode material for super capacitor cobalt-nickel oxide composite material | |
| CN103816912B (en) | Bi 2o 3/ Co 3o 4the preparation method of composite photo-catalyst and application | |
| CN105905940B (en) | A kind of preparation method of nickel titanate/titanium dioxide composite nano material | |
| CN109453792B (en) | Preparation method of sulfide heterojunction material resistant to photo-corrosion in photo-Fenton reaction | |
| CN103920518A (en) | High-visible-light-activity sulfur-modified carbon nitride photocatalyst as well as synthetic method and application of photocatalyst | |
| CN102795655A (en) | Method for preparing hierarchical floriform hollow-structure CuS | |
| CN102441395B (en) | Application of macroporous oxide oxygen carrier in circular hydrogen production of chemical chain and preparation method | |
| CN112023972B (en) | Composite photocatalytic material and preparation method and application thereof | |
| CN105597765A (en) | In2O3/ZnFe2O4 nanometer heterojunction composite photocatalytic material and preparation method thereof | |
| CN103990472A (en) | Stable and efficient hydrogen production co-catalyst and preparation method thereof | |
| CN105536765B (en) | A kind of shell base boron-doped titanium dioxide composite photo-catalyst and preparation method thereof | |
| CN111229205B (en) | WO3/Zn2GeO4Non-noble metal bimetal oxide photocatalyst and preparation method and application thereof | |
| CN106914266B (en) | g-C for fast degrading pollutant3N4Composite photocatalyst and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Open date: 20090819 |