CN109574061A - A kind of method for preparing solid phase with different-shape nano ceria - Google Patents
A kind of method for preparing solid phase with different-shape nano ceria Download PDFInfo
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- CN109574061A CN109574061A CN201811414564.4A CN201811414564A CN109574061A CN 109574061 A CN109574061 A CN 109574061A CN 201811414564 A CN201811414564 A CN 201811414564A CN 109574061 A CN109574061 A CN 109574061A
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- Prior art keywords
- ceria
- different
- solid phase
- preparing solid
- stratiform
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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
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
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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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The present invention provides a kind of stratiform, sheet, graininess nano ceric oxide method for preparing solid phase.In the inventive method, solid state reaction is occurred by cerium system metal salt and differential responses object at room temperature, stratiform, sheet, graininess nano ceric oxide are made respectively, is used as Oxidation of Carbon Monoxide catalysts, it is shown that preferable catalytic effect.Raw material used in the method for the present invention is cheap and easy to get, and operation is simple, and time-consuming is few, is easy to be produced in enormous quantities, have broad application prospects.
Description
Technical field
The present invention relates to a kind of method for preparing solid phase of nano ceric oxide, belongs to materials synthesis and catalyst preparation is led
Domain.
Background technique
The unique 4f electronic structure of rare earth element makes its compound in terms of light, electricity, magnetic field, material conversion and storage
It is widely used.In addition to this, these special natures, institute can be possessed by rare earth element or its compound modified material
The a variety of materials of exploitation can be used for being catalyzed, electronics, the energy, environmental protection, the multiple fields such as biological medicine.Wherein, cerium is rare earth
The most abundant element of reserves in element, the abundance in the earth's crust is 68ppm, accounts for the 28% of rare earth total content.Ceria conduct
The a kind of of transition metal oxide is extensively studied with characteristics such as its nontoxicity, high oxygen storage power, chemical property stabilizations.Synthesis
The method of cerium dioxide nano material is mainly vapor phase method, liquid phase method, solid phase method.Vapor phase method is needed using special equipment, and
Liquid phase method has the characteristics that equipment is simple, easy to operate, at low cost, but complex steps, needs largely to use solvent.Solid phase method has
Feature easy to operate, yield is high, at low cost, environmentally protective, but generally use the pattern of solid phase method products therefrom, size is not easy
Control.
It is well known that the pattern of nano material, size are huge on the influence of its performance.(111) may be present in ceria,
(110) the exposure crystal face different with (100) three, when for being catalyzed reaction, it is living that different crystal faces shows different reactions
Property.Therefore, how the system with different-shape, sized nanostructures ceria is realized by the solid state reaction of method simplicity
It is standby, become current urgent problem to be solved.
Summary of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the present invention provides a kind of with different-shape nano ceria
Method for preparing solid phase.It can be prepared using easy operating method through solid state reaction by using raw material cheap and easy to get
Stratiform, sheet, graininess nano ceric oxide out, are used for catalytic CO oxidation reaction, show preferable catalysis
Effect.
Technical scheme is as follows:
At room temperature, the cerium system metal salt that molar ratio is 1:0.5 ~ 6 is mixed from different acid, alkali, salt, carries out grinding or ball milling
Solid state reaction, product obtain stratiform, sheet or graininess nano ceric oxide after water-bath, washing, drying, calcining.Institute
Cerium salt be cerous sulfate, cerous acetate, cerium chloride, cerous nitrate, ammonium ceric nitrate, cerous acetate it is one or more, it is used anti-
Answering object is oxalic acid, sodium oxalate, ammonium oxalate, tartaric acid, sodium carbonate, sodium bicarbonate, ammonium carbonate, ammonium acetate, potassium hydroxide, hydroxide
Sodium it is one or more.Sheet ceria with a thickness of 50-100nm, stratiform ceria is 50-100nm, graininess dioxy
The partial size for changing cerium is 20-100nm.Different-shape nano ceria shows different catalytics to Oxidation of Carbon Monoxide reaction
Energy.
Compared with prior art, the invention has the following advantages that based on solid state reaction, using cheap and easy to get
Stratiform, sheet, graininess nanometer titanium dioxide cerium catalyst can be made by simply grinding or ball milling operation in raw material.Preparation side
Method is simple, and catalyst production is high, it is easy to accomplish the features such as mass production all makes the present invention have extremely wide application prospect.
Detailed description of the invention
Fig. 1 is the X ray diffracting spectrum of the product of the 1st embodiment preparation of the invention.
Fig. 2 is the electron scanning micrograph of the product of the 1st embodiment preparation of the invention.
Fig. 3 is the catalyzing carbon monoxide performance of the product of the 1st embodiment preparation of the invention.
Fig. 4 is the X ray diffracting spectrum of the product of the 2nd embodiment preparation of the invention.
Fig. 5 is the electron scanning micrograph of the product of the 2nd embodiment preparation of the invention.
Fig. 6 is the catalyzing carbon monoxide performance of the product of the 2nd embodiment preparation of the invention.
Fig. 7 is the X ray diffracting spectrum of the product of the 3rd embodiment preparation of the invention.
Fig. 8 is the electron scanning micrograph of the product of the 3rd embodiment preparation of the invention.
Fig. 9 is the catalyzing carbon monoxide performance of the product of the 3rd embodiment preparation of the invention.
Specific embodiment
Below with reference to specific embodiment, the present invention is further elaborated.These embodiments are interpreted as being merely to illustrate
The present invention rather than limit the scope of the invention.After having read the content of the invention recorded, based on of the invention
Principle equally falls into claims of the present invention limited range to the various changes of the invention made or modification.
Embodiment 1
By 2.02 g cerous sulfate (Ce (SO4)2·H2O 1.42 g oxalic acid (H are added after) grinding in mortar2C2O4·2H2O it) grinds
It mixes them thoroughly, continuing grinding makes them that solid state reaction occur for about 1 hour, later by sample in 60 degrees Celsius of lower water-baths
24 hours, product water and ethanol washing simultaneously calcined sample after being dried at room temperature for 24 hours under 400 degrees Celsius of air
To laminar nano ceria.It is used for catalytic CO oxidation reaction, it can make carbon monoxide complete at 380 degrees Celsius
It is oxidized to carbon dioxide.
Embodiment 2
By 2.17 g cerous nitrate (Ce (NO3)3·6H2O 1.68 g sodium bicarbonate (NaHCO are added after) grinding in mortar3) grinding
It mixes them thoroughly, continuing grinding makes them that solid state reaction occur for about 1 hour, later by sample in 60 degrees Celsius of lower water-baths
For 24 hours, product water and ethanol washing and sample is calcined after being dried at room temperature for 24 hours under 400 degrees Celsius of air and obtains piece
Shape nano ceric oxide.It is used for catalytic CO oxidation reaction, it can make carbon monoxide in 380 degrees Celsius of complete oxidations
Carbon dioxide.
Embodiment 3
By 2.17 g cerous nitrate (Ce (NO3)3·6H2O 3.14 g ammonium carbonate ((NH are added after) grinding in mortar4)2CO3) grinding
It mixes them thoroughly, continuing grinding makes them that solid state reaction occur for about 1 hour, later by sample in 60 degrees Celsius of lower water-baths
24 hours, product water and ethanol washing simultaneously calcined sample after being dried at room temperature for 24 hours under 400 degrees Celsius of air
To graininess nano ceric oxide.It is used for catalytic CO oxidation reaction, it can make carbon monoxide complete at 320 degrees Celsius
Oxidized carbon dioxide.
From Fig. 1,4,7, X ray diffracting spectrum result can be seen that we are successfully prepared the ceria of pure phase.From figure
2,5,8, electron scanning micrograph can be seen that product is stratiform, sheet, graininess pattern.It can be seen that from Fig. 3,6,9
The ceria of the different-shape of preparation shows different catalyzing carbon monoxide oxidation susceptibilities.The present invention provides one kind to have
The method for preparing solid phase of different-shape nano ceria.This method does not use solvent, easy to operate, mild condition, and product produces
Rate is high, is easy to industrial mass production.
Claims (4)
1. a kind of method for preparing solid phase with different-shape nano ceria comprising following steps: at room temperature, will rub
You carry out grinding or ball milling solid state reaction than the cerium salt and differential responses object for being 1:0.5 ~ 6, product is washed, it is dry, forge
Stratiform, sheet, graininess nano ceric oxide are obtained after burning.
2. a kind of method for preparing solid phase with different-shape nano ceria according to claim 1, feature exist
In: cerium salt used be cerous sulfate, cerous acetate, cerium chloride, cerous nitrate, ammonium ceric nitrate, cerous acetate it is one or more, used
Reactant be oxalic acid, sodium oxalate, ammonium oxalate, tartaric acid, sodium carbonate, sodium bicarbonate, ammonium carbonate, ammonium acetate, potassium hydroxide, hydrogen
Sodium oxide molybdena it is one or more.
3. a kind of method for preparing solid phase with different-shape nano ceria according to claim 1, feature exist
In: by changing the available sheet of reactant type, stratiform, particulate ceria, wherein the thickness of sheet ceria
For 50-100nm, stratiform ceria is 50-100nm, and the partial size of particulate ceria is 20-100nm.
4. a kind of method for preparing solid phase with different-shape nano ceria according to claim 1, feature exist
In: obtained different-shape nano ceria shows different catalytic performances to Oxidation of Carbon Monoxide reaction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811414564.4A CN109574061A (en) | 2018-11-26 | 2018-11-26 | A kind of method for preparing solid phase with different-shape nano ceria |
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| CN201811414564.4A CN109574061A (en) | 2018-11-26 | 2018-11-26 | A kind of method for preparing solid phase with different-shape nano ceria |
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| CN201811414564.4A Pending CN109574061A (en) | 2018-11-26 | 2018-11-26 | A kind of method for preparing solid phase with different-shape nano ceria |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111389360A (en) * | 2020-03-30 | 2020-07-10 | 中国农业大学 | Bio-carbon-loaded Ce-rich material3+Cerium dioxide material, preparation method and application thereof |
| CN113845858A (en) * | 2021-10-25 | 2021-12-28 | 池州市君浦新材料科技有限公司 | Antistatic touch screen protection film |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1386706A (en) * | 2002-04-29 | 2002-12-25 | 四川大学 | Process for preparing rare-earth nano oxide by ball grinding and solid-phase chemical reaction |
| CN104877573A (en) * | 2015-06-08 | 2015-09-02 | 四川大学 | Preparation method of spherical nano fluorine-doped CeO2 polishing powder |
| CN105733445A (en) * | 2016-03-21 | 2016-07-06 | 四川大学 | Preparation method of nano CeO2 polishing powder |
| CN108262051A (en) * | 2018-01-18 | 2018-07-10 | 蚌埠学院 | A kind of method of mechanical ball mill heat treatment two-step method synthesis ceria-bismuthyl carbonate nano-complex |
-
2018
- 2018-11-26 CN CN201811414564.4A patent/CN109574061A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1386706A (en) * | 2002-04-29 | 2002-12-25 | 四川大学 | Process for preparing rare-earth nano oxide by ball grinding and solid-phase chemical reaction |
| CN104877573A (en) * | 2015-06-08 | 2015-09-02 | 四川大学 | Preparation method of spherical nano fluorine-doped CeO2 polishing powder |
| CN105733445A (en) * | 2016-03-21 | 2016-07-06 | 四川大学 | Preparation method of nano CeO2 polishing powder |
| CN108262051A (en) * | 2018-01-18 | 2018-07-10 | 蚌埠学院 | A kind of method of mechanical ball mill heat treatment two-step method synthesis ceria-bismuthyl carbonate nano-complex |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111389360A (en) * | 2020-03-30 | 2020-07-10 | 中国农业大学 | Bio-carbon-loaded Ce-rich material3+Cerium dioxide material, preparation method and application thereof |
| CN111389360B (en) * | 2020-03-30 | 2021-04-02 | 中国农业大学 | Bio-carbon-loaded Ce-rich material3+Cerium dioxide material, preparation method and application thereof |
| CN113845858A (en) * | 2021-10-25 | 2021-12-28 | 池州市君浦新材料科技有限公司 | Antistatic touch screen protection film |
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Application publication date: 20190405 |