CN106732625A - A kind of Copper-cladding Aluminum Bar cerium oxide nano materials of cyclic structure and its preparation and application - Google Patents
A kind of Copper-cladding Aluminum Bar cerium oxide nano materials of cyclic structure and its preparation and application Download PDFInfo
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- CN106732625A CN106732625A CN201611132099.6A CN201611132099A CN106732625A CN 106732625 A CN106732625 A CN 106732625A CN 201611132099 A CN201611132099 A CN 201611132099A CN 106732625 A CN106732625 A CN 106732625A
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- copper
- cerium oxide
- aluminum bar
- oxide nano
- cyclic structure
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- 229910000420 cerium oxide Inorganic materials 0.000 title claims abstract description 40
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 37
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 34
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000005253 cladding Methods 0.000 title claims abstract description 34
- 125000004122 cyclic group Chemical group 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004202 carbamide Substances 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 8
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 7
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 5
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 3
- 230000007062 hydrolysis Effects 0.000 claims abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 8
- 229910052684 Cerium Inorganic materials 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 3
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 3
- 206010013786 Dry skin Diseases 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 7
- 239000001301 oxygen Substances 0.000 abstract description 7
- 229910052760 oxygen Inorganic materials 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000005406 washing Methods 0.000 abstract description 4
- 238000004140 cleaning Methods 0.000 abstract description 2
- 239000003513 alkali Substances 0.000 abstract 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 abstract 1
- 229910052753 mercury Inorganic materials 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 5
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 5
- 238000003756 stirring Methods 0.000 description 4
- 239000012159 carrier gas Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 150000002823 nitrates Chemical class 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 150000004040 pyrrolidinones Chemical class 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/83—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8665—Removing heavy metals or compounds thereof, e.g. mercury
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Environmental & Geological Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Biomedical Technology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Catalysts (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of Copper-cladding Aluminum Bar cerium oxide nano materials of cyclic structure and its preparation and the application in terms of demercuration.Comprise the following steps:With a certain proportion of cerous nitrate and mantoquita as raw material, using urea as alkali source, using polyvinylpyrrolidone as surfactant, mixed hydrolysis react, the mixture for obtaining is after hydro-thermal constant temperature is preserved and washing is dried, again by calcining, pattern rule, size uniformity, the Copper-cladding Aluminum Bar cerium oxide of complete ring-type nanostructured are obtained.Copper-cladding Aluminum Bar cerium oxide nano materials structure prepared by the present invention is novel, and raw material is simple and easy to get, and operation is simple, course of reaction cleaning, non-secondary pollution.The removing of mercury in air is applied to, method is simple, and demercuration effect is good, concentration for the treatment of is 75 μ g/m3Hg0Steam, in the case where 4% Oxygen Condition is passed through, demercuration rate can reach more than 98%, good stability.
Description
Technical field
The present invention relates to the field of nano material preparation technology, and in particular to a kind of Copper-cladding Aluminum Bar cerium oxide of cyclic structure is received
Rice material and its preparation and its application in terms of demercuration.
Background technology
Cerium oxide is a kind of extremely wide rare earth oxide of purposes, with can rapid translating Ce3+/Ce4+, superior store
The quick Lacking oxygen diffusivity of oxygen function, high temperature, is widely used in catalytic field.Controlled in nano-scale when by scantling
When, the physical and chemical performance of uniqueness is showed, be conducive to lifting its catalysis activity.And the cerium oxide nano of different-shape structure
The catalytic performance of material there is also very big difference.
In recent years, research obtains the cerium oxide nano materials of portion of monocrystalline structure, bar-shaped, real compared to existing at present
The cerium oxide of the various patterns such as bulbus cordis shape, threadiness, the nano material of monocrystalline cyclic structure is in specific surface area and permeability
Etc. aspect have superior function, had a good application prospect in catalytic field.
And CeO2Adulterate after other exogenous metal ions, the twist distortion of the lattice structure that ion size difference causes,
Or ionic valence condition balance is broken in the change of Doped ions valence state, these can result in lattice occur more lattice defects and
Lacking oxygen, so as to further increase oxygen storage capacity and redox ability, and then improves catalysis activity.Therefore new list is researched and developed
The brilliant metal-doped cerium oxide nano materials of cyclic structure will have good application prospect.
The content of the invention
Copper-cladding Aluminum Bar cerium oxide nano materials it is an object of the invention to provide a kind of cyclic structure and preparation method thereof and
Using.Preparation method of the present invention is simple, short preparation period, cleaning, reproducible.The cerium oxide nano materials of preparation, structure is new
Grain husk, catalytic capability is stronger, and demercuration effect is good, easy to use using simple.
The purpose of the present invention is achieved in the following ways.
A kind of preparation method of the Copper-cladding Aluminum Bar cerium oxide nano materials of cyclic structure, comprises the following steps:By cerous nitrate, copper
After salt, polyvinylpyrrolidone, urea mixing are through hydro-thermal reaction, then by calcining, obtain the Copper-cladding Aluminum Bar cerium oxide of cyclic structure
Nano material.
The preparation method of the Copper-cladding Aluminum Bar cerium oxide nano materials of described cyclic structure, mantoquita includes copper chloride, copper nitrate
In one or two.
The mol ratio of the preparation method of the Copper-cladding Aluminum Bar cerium oxide nano materials of described cyclic structure, cerium and copper:1:0.01-
0.1。
The preparation method of the Copper-cladding Aluminum Bar cerium oxide nano materials of described cyclic structure, the cerous nitrate for being used, polyethylene
The mass ratio that pyrrolidones and urea are added is:1:(0.2~1):(2~6).
The preparation method of the Copper-cladding Aluminum Bar cerium oxide nano materials of described cyclic structure, 120 DEG C -180 of hydrothermal temperature
DEG C, time 10-12 hours.
The preparation method of the Copper-cladding Aluminum Bar cerium oxide nano materials of described cyclic structure, 300-600 DEG C of calcining heat, calcining
2-4h。
The preparation method of the Copper-cladding Aluminum Bar cerium oxide nano materials of described cyclic structure, by cerous nitrate and mantoquita and polyethylene
Pyrrolidones is added in deionized water, magnetic agitation 10-40 minutes, adds a certain amount of urea mixed hydrolysis reaction 15-60
Minute, the mixture for obtaining carries out hydro-thermal reaction again.
The preparation method of the Copper-cladding Aluminum Bar cerium oxide nano materials of described cyclic structure, the product washing three after hydro-thermal reaction
Secondary, ethanol is washed twice, after suction filtration, by its 60 DEG C of dryings more than 8 hours, then is calcined.
The Copper-cladding Aluminum Bar cerium oxide nano materials of above-mentioned cyclic structure are used to be catalyzed demercuration.Specifically method is:
Reaction temperature is 150 DEG C -250 DEG C, gaseous state Hg0Concentration be 50-100 μ g/m3, carrier gas is N2, air speed is
150000h-1, the material containing 4%O2Demercuration is carried out under the conditions of following carrier gas.
It is an advantage of the invention that:
(1) the invention provides a kind of cyclic structure Copper-cladding Aluminum Bar cerium oxide nano materials preparation method, preparation process
Easy clean is controllable, and raw material is simple and easy to get, meanwhile, your gold such as Au, Pd contained in current many preferable demercuration catalysts of effect
Category, it is relatively costly, and preparing raw material price of the invention is relatively low.
(2) same procedure is used, but does not mix the pure zirconia cerium that copper prepares and compared, the Copper-cladding Aluminum Bar oxidation that the present invention is provided
Cerium is presented the ring-type nanostructured of pattern rule, material is had more spaces, is conducive to increasing specific surface area, and lifting is lived
Property, and material C e3+/Ce4+Conversion capability lifted, while Surface Oxygen vacancy concentration increase, catalytic performance enhancing.
(3) nano material of the Copper-cladding Aluminum Bar cerium oxide of ring-type of the present invention, preferably, concentration for the treatment of is 75 μ g/m to demercuration effect3
Hg0Steam, after 4% oxygen is passed through, demercuration rate can reach 98.5%, and general catalyst often also needs to be passed through
HCl, and pure zirconia cerium is under the same conditions, demercuration rate is only 17%.
Brief description of the drawings
Fig. 1 is the TEM figures of the Copper-cladding Aluminum Bar cerium oxide nano materials of the cyclic structure prepared by the inventive method;
Fig. 2 be using same procedure but do not mix the pure zirconia cerium that copper is prepared TEM figure;
Fig. 3 is the XRD spectrum of the Copper-cladding Aluminum Bar cerium oxide nano materials of the cyclic structure prepared by the inventive method.
Specific embodiment
The present invention is illustrated with specific embodiment below to be described further, but it is necessary to note that following examples are only used
Further illustrated in the content of the invention, limitation of the present invention can't be formed.
Embodiment 1
By 0.143g cerous nitrates, in 0.068g copper chlorides and 0.5g polyvinylpyrrolidones addition 30mL deionized waters, magnetic
Power stirring 10min is completely dissolved until it, then 2.196g urea is added in reaction solution, stirring reaction 30min, will be mixed
Compound is added in hydrothermal reaction kettle.Reactor is put into baking oven, 150 DEG C of constant temperature 10h.Then gained mixed solution is spent
Ion water washing three times, ethanol is washed twice, and 10h is dried in 60 DEG C of baking ovens, finally 500 DEG C of calcining 4h in Muffle furnace, you can
Obtain the ring-type nano material of Copper-cladding Aluminum Bar cerium oxide.
Embodiment 2
By 0.143g cerous nitrates, in 0.097 copper nitrate and 0.5g polyvinylpyrrolidones addition 30mL deionized waters, magnetic force
Stirring 10min is completely dissolved until it, and then 2.196g urea is added in reaction solution, and stirring reaction 30min will mix
Thing is added in hydrothermal reaction kettle.Reactor is put into baking oven, 150 DEG C of constant temperature 10h.Then by gained mixed solution spend from
Sub- water washing three times, ethanol is washed twice, and 10h is dried in 60 DEG C of baking ovens, finally 500 DEG C of calcining 4h in Muffle furnace, you can
To the ring-type nano material of Copper-cladding Aluminum Bar cerium oxide.
Embodiment 3
Under conditions of 200 DEG C, respectively the material prepared by embodiment 1 as catalyst treatment concentration be 75 μ g/m3's
Hg0Steam, air speed is 150000h-1, in N2Under the conditions of as carrier gas, after 4% oxygen is passed through, demercuration effect can reach
More than 98.5%.
Claims (10)
1. the preparation method of the Copper-cladding Aluminum Bar cerium oxide nano materials of a kind of cyclic structure, it is characterised in that comprise the following steps:Will
After cerous nitrate, mantoquita, polyvinylpyrrolidone, urea mixing are through hydro-thermal reaction, then by calcining, the copper for obtaining cyclic structure is mixed
Miscellaneous cerium oxide nano materials.
2. the preparation method of the Copper-cladding Aluminum Bar cerium oxide nano materials of cyclic structure according to claim 1, it is characterised in that
Mantoquita include copper chloride, copper nitrate in one or two.
3. the preparation method of the Copper-cladding Aluminum Bar cerium oxide nano materials of cyclic structure according to claim 1, it is characterised in that
The mol ratio of cerium and copper:1:(0.01~0.1).
4. the preparation method of the Copper-cladding Aluminum Bar cerium oxide nano materials of cyclic structure according to claim 1, it is characterised in that
The mass ratio that cerous nitrate, polyvinylpyrrolidone and the urea for being used are added for:1:(0.2~1):(2~6).
5. the preparation method of the Copper-cladding Aluminum Bar cerium oxide nano materials of cyclic structure according to claim 1, it is characterised in that
120 DEG C -180 DEG C, time 10-12 hours of hydrothermal temperature.
6. the preparation method of the Copper-cladding Aluminum Bar cerium oxide nano materials of cyclic structure according to claim 1, it is characterised in that
300-600 DEG C of calcining heat, calcines 2-4h.
7. the preparation method of the Copper-cladding Aluminum Bar cerium oxide nano materials of cyclic structure according to claim 1, it is characterised in that
Cerous nitrate and mantoquita and polyvinylpyrrolidone are added in deionized water, magnetic agitation 10-40 minutes, added a certain amount of
Urea mixed hydrolysis react 15-60 minutes, and the mixture for obtaining carries out hydro-thermal reaction again.
8. the preparation method of the Copper-cladding Aluminum Bar cerium oxide nano materials of cyclic structure according to claim 1, it is characterised in that
Product after hydro-thermal reaction is washed three times, and ethanol is washed twice, after suction filtration, by its 60 DEG C of dryings more than 8 hours, then is calcined.
9. the Copper-cladding Aluminum Bar cerium oxide nano materials of the cyclic structure that the method described in any one of claim 1-8 is prepared from.
10. the Copper-cladding Aluminum Bar cerium oxide nano materials of the cyclic structure described in claim 9 are used to be catalyzed demercuration.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107754779A (en) * | 2017-10-24 | 2018-03-06 | 山东师范大学 | Transient metal doped cerium-based composite oxides multiaspect body catalyst and preparation method |
CN108948120A (en) * | 2018-07-07 | 2018-12-07 | 张正光 | A kind of preparation method of Abiraterone acetate intermediate |
CN110508288A (en) * | 2019-09-24 | 2019-11-29 | 福州大学 | A kind of preparation and its application of the rodlike Copper-cladding Aluminum Bar ceria with porous structure |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN107754779A (en) * | 2017-10-24 | 2018-03-06 | 山东师范大学 | Transient metal doped cerium-based composite oxides multiaspect body catalyst and preparation method |
CN108948120A (en) * | 2018-07-07 | 2018-12-07 | 张正光 | A kind of preparation method of Abiraterone acetate intermediate |
CN110508288A (en) * | 2019-09-24 | 2019-11-29 | 福州大学 | A kind of preparation and its application of the rodlike Copper-cladding Aluminum Bar ceria with porous structure |
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