CN114940509B - Method for preparing cerium oxide material with hierarchical pore structure by re-dissolving doped zinc - Google Patents
Method for preparing cerium oxide material with hierarchical pore structure by re-dissolving doped zinc Download PDFInfo
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- 229910000420 cerium oxide Inorganic materials 0.000 title claims abstract description 25
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 239000011701 zinc Substances 0.000 title claims abstract description 19
- 239000000463 material Substances 0.000 title claims abstract description 16
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 13
- 239000002149 hierarchical pore Substances 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 title claims description 17
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 239000011148 porous material Substances 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 8
- 239000004246 zinc acetate Substances 0.000 claims abstract description 8
- 230000032683 aging Effects 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract 2
- 239000011259 mixed solution Substances 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 10
- 239000002244 precipitate Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- 229910052684 Cerium Inorganic materials 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- -1 cerium ion Chemical class 0.000 claims description 3
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 abstract description 4
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 238000000975 co-precipitation Methods 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract 2
- 239000003513 alkali Substances 0.000 abstract 1
- 230000015556 catabolic process Effects 0.000 abstract 1
- QQZMWMKOWKGPQY-UHFFFAOYSA-N cerium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QQZMWMKOWKGPQY-UHFFFAOYSA-N 0.000 abstract 1
- 238000006731 degradation reaction Methods 0.000 abstract 1
- 230000002431 foraging effect Effects 0.000 abstract 1
- 230000002363 herbicidal effect Effects 0.000 abstract 1
- 239000012855 volatile organic compound Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 239000004793 Polystyrene Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 2
- 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 description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 241001247197 Cephalocarida Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 208000031513 cyst Diseases 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000000132 electrospray ionisation Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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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
-
- B01J35/56—
-
- 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
- C01F17/224—Oxides or hydroxides of lanthanides
- C01F17/235—Cerium oxides or hydroxides
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention relates to a methodA preparation method for preparing a porous cerium oxide material, which belongs to the technical field related to the preparation of inorganic nano materials. The preparation method comprises the steps of two steps, wherein in the first step, a certain amount of cerium nitrate hexahydrate, oxalic acid and zinc acetate are dissolved in deionized water at room temperature, the solutions are mixed and stirred for coprecipitation reaction, and then the mixture is placed in an oven for aging to obtain the composite oxalate. Filtering, washing and drying after aging, calcining to remove herbicidal acid radicals to obtain the Zn-CeO product of the first step 2 Doping the porous material. And secondly, removing zinc components in the doped product of the first step by using alkali liquor or acid liquor, filtering, washing, drying and calcining to obtain the cerium oxide material with the hierarchical pore structure. The invention prepares the disordered cerium oxide material with the hierarchical pore structure under a simpler condition, has higher specific surface and better performance, and can be applied to the aspects of VOCs catalytic degradation, automobile exhaust catalysis, ultraviolet light shielding and the like.
Description
Technical Field
The invention particularly relates to a method for preparing cerium dioxide with a hierarchical pore structure by zinc doping and then dissolving, belonging to the technical field of inorganic nano material preparation.
Background
Cerium oxide as one kind of functional RE material has unique property and wide application in catalysis, electrochemistry, optics and other fields. In recent years, nano-micro structures of cerium oxide, such as nanorods/wires, nanocubes, nanooctahedrons exposing specific crystal planes, have been synthesized by different methods, with two-dimensional ordered, three-dimensional ordered, randomly arranged porous structures, doped structures, and the like. The porous material has important application in the field of catalysis, has unique advantages, is favorable for fully utilizing active sites, and can increase the specific surface area and improve the flow and the evacuation of gas. At present, porous cerium oxide and cerium-based composite oxide are mainly prepared into three-dimensional ordered macroporous Au/CeO with controllable aperture by means of a template and a PS colloid template method by Zhang et al 2 The catalyst has better catalytic oxidation capability to formaldehyde. However, the method has complicated steps, and the monodisperse polystyrene colloid spheres are firstly utilized to assemble the three-dimensional ordered polystyrene colloid crystal template (J.Zhang, et al, appl. Catalyst. B, 2009.91 (1-2): p.11-20.). Chinese patent CN201710107622.8 uses surfactant as template, and prepares porous cerium-based composite oxide by sol-gel-foaming method. Chinese patent CN201410374724.2Polyvinylpyrrolidone (PVP) is used as a high molecular template agent, and an electrospray ionization technology is adopted to prepare the cerium dioxide porous microsphere. Chinese patent CN201310228257.8 mainly uses surfactant or block copolymer as soft template, artemia cysts shell as hard template, and adds metal salt and citric acid to prepare multi-stage porous cerium oxide material, but the method can obtain macroporous structure of 0.4-1.5 μm. In addition, porous cerium oxide can be produced under high temperature calcination conditions by using hard templates such as SBA-15 and KIT-6 mesoporous molecular sieves (H.F. Gong, et al, new J. Chem.,2015,39 (12). 9380-9388). However, both the soft template method and the hard template method require two steps of introducing the template and then removing the template, so that the preparation process becomes complicated, the pore canal collapse is easy to cause in the removing process, and the cost for using the template agent is high. In summary, the existing preparation method of porous cerium oxide is complicated to prepare or difficult to regulate and control, and is difficult to prepare a multi-level pore structure, especially an atomic-level pore structure, so that the preparation method for effectively synthesizing the porous cerium oxide material by adopting simpler steps and mild conditions still needs to be explored.
Disclosure of Invention
The invention overcomes the defects of the prior art and provides a method for preparing a cerium oxide material with a hierarchical pore structure by zinc doping and then dissolving.
The preparation method of the porous cerium oxide comprises the following steps:
(1) Accurately weigh a certain amount of Ce (NO) 3 )·6H 2 O, oxalic acid and zinc acetate are dissolved in deionized water at room temperature to obtain a mixed solution, the mixed solution is uniformly stirred at room temperature, and white precipitate is obtained after aging at 80 ℃;
(2) Filtering, washing, drying, calcining at 500 deg.C to obtain the product Zn/CeO of first step 2 A porous material, designated sample a;
(3) Dissolving the product of the first step in deionized water for ultrasonic dispersion, adding a solvent, stirring at a certain temperature for reaction, and removing zinc components;
(4) Filtering, washing and drying the turbid liquid after the reaction, and placing the dried solid sample in a muffle furnace for calcining for 2 hours at 350 ℃ to obtain a porous cerium oxide material;
wherein Ce (NO) as described in step (1) 3 )·6H 2 The concentration of O is 0.05-0.20mol/L, and the mol ratio of zinc ion to cerium ion is 0.02-0.60.
Preferably, n in step (1) Zn / n Ce =X (X=0.02-0.20)。
Preferably, the solution addition sequence in the step (1) is to add zinc acetate solid into cerium nitrate solution to dissolve and then add oxalic acid solution.
Preferably, the aging time of step (1) is 8-16 hours.
Preferably, the solvent in the step (3) is urea solution or concentrated ammonia water.
Preferably, the reaction time in step (4) is from 5 to 8 hours.
The invention uses Ce (NO) 3 )·6H 2 O, oxalic acid, zinc acetate and urea are used as raw materials to prepare the cerium oxide material with a hierarchical pore structure, and the method has the advantages that:
(1) The preparation method is simple: and preparing the porous composite oxide by adopting a coprecipitation method without using a template agent, and then carrying out in-situ pore-forming by adopting solvent etching to obtain the multistage porous cerium oxide material. (2) The prepared porous cerium oxide has better catalytic performance on toluene.
Drawings
Fig. 1 is a scanning electron microscope image of example 1 of the present invention.
FIG. 2 is a graph showing the catalytic oxidation performance of toluene in example 1 of the present invention.
Fig. 3 is an N2 adsorption/desorption isothermal curve according to example 2 of the present invention.
Fig. 4 is an XRD pattern of example 3 of the present invention.
Detailed Description
Specific embodiments of the invention will now be described below:
example 1
(1) Accurately weigh 8.682g Ce (NO) 3 )·6H 2 O, 4.538g oxalic acid and 0.220g zinc acetate (X=5%) are dissolved in 200ml deionized water at room temperature to obtain a mixed solution, and the mixed solution is uniformly stirred, aged at 80 ℃ to obtain white precipitate;
(2) Filtering to separate white precipitate, washing, drying, calcining at 500 deg.c to obtain the product 5% -Zn/CeO in the first step 2 Pore material (Sample a);
(3) Dissolving the product of the first step in deionized water for ultrasonic dispersion, adding 0.15mol/l urea solution, placing the solution in a water bath kettle at 80 ℃ for water bath stirring reaction for 4 hours, and removing zinc components;
(4) And filtering, washing and drying the turbid liquid after the reaction, and placing the dried solid Sample in a muffle furnace for calcining at 350 ℃ for 2 hours to obtain the disordered porous cerium oxide material (Sample B).
Example 2
(1) Accurately weigh 8.682g Ce (NO) 3 )·6H 2 O, 4.538g oxalic acid and 0.220g zinc acetate (X=5%) are dissolved in 200ml deionized water at room temperature to obtain a mixed solution, and the mixed solution is uniformly stirred, aged at 80 ℃ to obtain white precipitate;
(2) Filtering to separate white precipitate, washing, drying, calcining at 500 deg.c to obtain the product 5% -Zn/CeO in the first step 2 Pore material (Sample a);
(3) Dissolving the product of the first step in deionized water, performing ultrasonic dispersion, adding ammonia water, stirring at room temperature, reacting for 10 hours, and removing zinc components;
(4) And filtering, washing and drying the turbid liquid after the reaction, and placing the dried solid Sample in a muffle furnace for calcining at 350 ℃ for 2 hours to obtain the disordered porous cerium oxide material (Sample B).
Example 3
(1) Accurately weigh 8.682g Ce (NO) 3 )·6H 2 O, 4.538g oxalic acid and 0.439g zinc acetate (X=10%) are dissolved in 200ml deionized water at room temperature to obtain a mixed solution, and the mixed solution is uniformly stirred, aged at 80 ℃ to obtain white precipitate;
(2) Filtering to separate white precipitate, washing, drying, calcining at 500 deg.c to obtain 10% -Zn/CeO product 2 Pore material (Sample a);
(3) Dissolving the product of the first step in deionized water for ultrasonic dispersion, adding 0.15mol/l urea solution, placing the solution in a water bath kettle at 80 ℃ for water bath stirring reaction for 4 hours, and removing zinc components;
(4) And filtering, washing and drying the turbid liquid after the reaction, and placing the dried solid Sample in a muffle furnace for calcining at 350 ℃ for 2 hours to obtain the disordered porous cerium oxide material (Sample B).
Claims (3)
1. The method for preparing the cerium oxide with the hierarchical pore structure by re-dissolving after zinc doping is characterized by comprising the following preparation steps:
(1) Accurately weigh a certain amount of Ce (NO) 3 )·6H 2 O, oxalic acid and zinc acetate are dissolved in deionized water at room temperature to obtain a mixed solution, the mixed solution is stirred uniformly at room temperature, and white precipitate is obtained after aging at 80 DEG C
(2) Filtering, washing, drying, calcining at 500 deg.C to obtain the product Zn/CeO of first step 2 A porous material;
(3) Dissolving the product of the first step in deionized water for ultrasonic dispersion, adding a solvent, and placing the mixture in a water bath kettle at 80 ℃ for stirring reaction to remove zinc components;
(4) Filtering, washing and drying the turbid liquid after the reaction, and placing a dried solid sample in a muffle furnace for calcining for 2 hours at 350 ℃ to obtain a disordered porous cerium oxide material;
wherein Ce (NO) as described in step (1) 3 )·6H 2 The concentration of O is 0.05-0.20mol/L, and the mol ratio of zinc ion to cerium ion is 0.02-0.60.
2. The method for preparing cerium oxide with a hierarchical pore structure by re-dissolving doped zinc according to claim 1, wherein the solvent in the step (3) is any one of urea, ammonia water, sodium hydroxide and dilute hydrochloric acid.
3. The method for preparing cerium oxide having a hierarchical pore structure by re-dissolving after doping zinc according to claim 1, wherein the reaction time in the step (3) is 4 to 12 hours.
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| CN101920984A (en) * | 2010-08-11 | 2010-12-22 | 中国科学院合肥物质科学研究院 | Method for preparing mesoporous CeO2 nano-tubes having large specific surface area and high catalytic activity |
| CN102417201B (en) * | 2011-08-31 | 2014-06-11 | 北京大学 | Method for preparing one-dimensional self-assembly material with ZnO nanorod array as template |
| GB201502813D0 (en) * | 2015-02-19 | 2015-04-08 | Univ St Andrews | Mesoporous materials |
| CN108927139A (en) * | 2018-06-22 | 2018-12-04 | 上海纳米技术及应用国家工程研究中心有限公司 | Nano bar-shape Nb-CeO2Material preparation method and products thereof and application |
| CN111362295A (en) * | 2020-02-21 | 2020-07-03 | 宁夏大学 | Ordered large-mesoporous cerium oxide material with high specific surface area and preparation method thereof |
| CN112007650B (en) * | 2020-08-13 | 2023-02-03 | 石家庄铁道大学 | Method for preparing porous cerium oxide-copper oxide composite material by chemical corrosion method |
| CN112295515B (en) * | 2020-11-30 | 2022-03-25 | 江南大学 | Preparation method of zinc oxide/cerium oxide hollow microspheres with inverted blueberry-shaped structures |
| CN112844444A (en) * | 2021-01-25 | 2021-05-28 | 清华大学 | Method for preparing cerium dioxide catalytic material by utilizing carrier pore channel self-adsorption principle |
| CN113713797A (en) * | 2021-09-03 | 2021-11-30 | 巢湖学院 | Preparation method and application of sandwich-shaped zinc oxide-cerium oxide composite nanoparticles |
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