CN112811457A - Preparation method of loose porous nano cerium oxide - Google Patents

Preparation method of loose porous nano cerium oxide Download PDF

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CN112811457A
CN112811457A CN202110235665.0A CN202110235665A CN112811457A CN 112811457 A CN112811457 A CN 112811457A CN 202110235665 A CN202110235665 A CN 202110235665A CN 112811457 A CN112811457 A CN 112811457A
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cerium oxide
nano cerium
crucible
porous nano
prepared
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路军
李雨轩
王燕燕
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Gansu Agricultural University
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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
    • C01F17/10—Preparation or treatment, e.g. separation or purification
    • 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
    • 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
    • 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
    • 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
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • 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)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
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  • Manufacturing & Machinery (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention discloses a preparation method of loose porous nano cerium oxide, which is prepared by adopting microwave-induced rheological phase self-propagating reaction and comprises the following steps: s1, respectively weighing a certain amount of cerous nitrate hexahydrate (Ce (NO)3)2·6H2O) and ascorbic acid (C)6H8O6) Adding a small amount of deionized water into a mortar to adjust into a rheological phase, and fully grinding for 10min to obtain a precursor; s2, transferring the obtained precursor into a crucible, and then putting the crucible into a microwave oven to treat for 1min-2min to obtain a powdery solid substance (white or light yellow) with very light texture; s3, roasting the powdery solid obtained in the S2 at the high temperature of 400-1200 ℃ for a certain time to obtainTo nano cerium oxide powder. The invention can synthesize a large amount of nano cerium oxide with stable yield and uniform particle size distribution in a limited time, and provides a new method for rapid and large-scale preparation of the nano cerium oxide.

Description

Preparation method of loose porous nano cerium oxide
Technical Field
The invention relates to the field of chemical raw material preparation, in particular to a preparation method of loose porous nano cerium oxide.
Background
The rare earth element has unique 4f electrons, so that the rare earth compound has unique optical, electric and magnetic properties. Among them, cerium oxide is an oxide catalyst with the highest activity in the rare earth oxide series, and is a cheap and widely-used material. With the continuous development of science and technology, the application of cerium oxide is wider and wider, and the dosage is larger and larger. Nano CeO2Due to its unique structural characteristics, it has special properties and is widely used in functional ceramics, catalysis, polishing, luminescence, gas sensors, fuel cells, and ultraviolet absorption. For example, cerium oxide is often used as a catalyst for removing nitrogen oxides and nitric oxide from automobile exhaust.
At present, a plurality of methods for preparing nano oxides are available, and a sol-gel method, a precipitation method, a micro-emulsion method and a self-propagating combustion method are common. Among these conventional methods, the self-propagating combustion method has significant advantages, especially for preparing nano-oxides by using low-temperature self-propagating combustion synthesis technology. The metal nitrate and the complexing agent are used for reaction, in-situ oxidation can be realized at low temperature, the spontaneous combustion can quickly synthesize the primary powder of the product, and the preparation period is greatly shortened. The method has simple and easy experimental operation and short experimental period, thereby saving time and energy. More importantly, the reactants are in a highly uniform dispersion state in the synthesis process, atoms can enter lattice sites only through short-range diffusion or rearrangement during reaction, the reaction speed is high, the decomposition temperature of the precursor and the formation temperature of the compound are low, and the particle size of the product is small and the distribution is uniform.
The common operation steps for preparing cerium oxide by the self-propagating combustion method are as follows: weighing quantitative oxidant (cerium nitrate hexahydrate) and fuel (mainly organic reducing agents such as glycine, urea, ascorbic acid and the like) according to a certain molar ratio, mixing, and adding deionized water for dissolving to obtain a solution, namely the precursor solution. The precursor solution was transferred to a crucible and stirred on a magnetic stirrer to dissolve the reactants in water sufficiently. The crucible is placed into a muffle furnace for heating, when the temperature is high enough, the solvent in the precursor liquid is gradually evaporated, and when the ignition temperature is reached, the self-propagating combustion reaction occurs in the muffle furnace, which is violent and is accompanied with a large amount of smoke generation. And obtaining a product cerium oxide in the crucible after full reaction. However, the above steps have some disadvantages, such as: heating the solution to evaporate the solvent for a longer time; when the reaction is carried out in a muffle furnace, the process is not easy to control; the reaction product pollutes the muffle furnace.
As a new inorganic synthesis method, the microwave heating method has the advantages of other methods, especially the advantages of the traditional synthesis method, and on one hand, the microwave heating method has the advantages of convenience, rapidness and high efficiency: microwave heating is bulk heating of a material caused by dielectric losses in an electromagnetic field. When microwave is applied to a sample, the microwave energy is converted into heat energy under the action of an electromagnetic field, so that the nano material is prepared. On the other hand, the microwave technology has the characteristics of cleanness, high efficiency, low consumption and the like, so that the nano material with stable yield and uniform particle size distribution can be synthesized in a large amount in a limited time.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of nano cerium oxide.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for preparing loose porous nano cerium oxide adopts microwave-induced rheological phase self-propagating reaction to prepare the nano cerium oxide.
Preferably, the method comprises the following steps:
s1, respectively weighing a certain amount of cerous nitrate hexahydrate (Ce (NO)3)2·6H2O) and ascorbic acid (C)6H8O6) Adding a small amount of deionized water into a mortar to adjust into a rheological phase, and fully grinding for 10min to obtain a precursor;
s2, transferring the obtained precursor into a crucible, and then putting the crucible into a microwave oven to treat for 1min-2min to obtain a powdery solid substance (white or light yellow) with very light texture;
s3, roasting the powdery solid obtained in the step S2 at the high temperature of 400-1200 ℃ for a certain time to obtain the nano cerium oxide powder.
Preferably, in the step S2, the ratio of the amounts of the substances of cerium nitrate hexahydrate and ascorbic acid is 2: 1; the time for the treatment in the microwave oven was 2 min.
In step S2, the high-temperature roasting temperature is 400 ℃ and the high-temperature roasting time is 2 h.
It is noted that the organic substance used for the combustion reaction may be a reducing organic compound such as glycine, urea, glycerin, mannitol, or the like, in addition to ascorbic acid.
The invention can synthesize a large amount of nano cerium oxide with stable yield, uniform particle size and distribution in a limited time, and provides a new method for preparing the nano cerium oxide.
Drawings
Fig. 1 is an X-ray diffraction spectrum of nano cerium oxide powder in an example of the present invention.
Fig. 2 is a scanning electron microscope image of the nano cerium oxide powder in the example of the present invention.
FIG. 3 is a transmission electron microscope spectrum of nano cerium oxide powder in the example of the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Examples
Synthetic preparation of cerium oxide
S1, respectively weighing a certain amount of cerium nitrate hexahydrate and ascorbic acid, wherein the ratio of the amounts of the cerium nitrate hexahydrate and the ascorbic acid is 2: 1; placing the two reactants in a mortar, adding a small amount of deionized water to adjust into a rheological phase, and fully grinding for 10min to obtain a precursor;
s2, transferring the obtained precursor into a crucible, and then putting the crucible into a microwave oven to treat for 1min-2min to obtain a powdery solid substance (white or light yellow) with very light texture;
and S3, roasting the powdery solid obtained in the step S2 at the high temperature of 400 ℃ for two hours to obtain the nano cerium oxide powder.
Results and analysis
X-ray diffraction analysis:
fig. 1 is an XRD spectrum of the product obtained in S3. The position and the relative intensity of the diffraction characteristic peak of the product are both equal to those of CeO2Corresponds to the standard card of (1), wherein the four most intense peaks are respectively at 2 θ =28.54 °, 33.06 °, 47.52 ° and 56.42 °, corresponding to CeO respectively2And (111), (200), (220) and (311) of (A), and no other hetero-phase peak. The products prepared above are all single-phase crystalline CeO2Belonging to the fluorite cubic system.
FIG. 2 is a Scanning Electron Microscope (SEM) image of the product obtained in S3 according to the present invention; it can be clearly seen that the product nano-ceria aggregates to have a loose porous structure.
FIG. 3 is a transmission electron microscope spectrum of nano cerium oxide powder in the example of the present invention. It can be seen from the figure that the product is relatively serious in aggregation, but the degree of crystallization is good, the particle sizes are different, but the particle sizes are all very small, not more than 10nm, and most of the particles are concentrated in 2-5 nm.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention. The embodiments and features of the embodiments of the present application may be combined with each other arbitrarily without conflict.

Claims (4)

1. A method for preparing loose porous nano cerium oxide is characterized in that: the nano cerium oxide is prepared by adopting microwave to initiate rheological phase self-propagating reaction.
2. The method of claim 1, wherein the porous nano cerium oxide is prepared by the following steps: the method comprises the following steps:
s1, respectively weighing a certain amount of cerous nitrate hexahydrate (Ce (NO)3)2·6H2O) and ascorbic acid (C)6H8O6) Adding a small amount of deionized water into a mortar to adjust into a rheological phase, and fully grinding for 10min to obtain a precursor;
s2, transferring the obtained precursor into a crucible, and then placing the crucible into a microwave oven for treatment for 1-2 min to obtain a powdery solid matter with very light texture;
s3, roasting the powdery solid obtained in the step S2 at the high temperature of 400-1200 ℃ for a certain time to obtain the nano cerium oxide powder.
3. The method of claim 1, wherein the porous nano cerium oxide is prepared by the following steps: in the step S2, cerium nitrate hexahydrate (Ce (NO)3)2·6H2O) and ascorbic acid (C)6H8O6) The amount ratio of the substances of (a) to (b) is 2: 1; the time for the treatment in the microwave oven was 2 min.
4. The method of claim 1, wherein the porous nano cerium oxide is prepared by the following steps: in step S2, the high-temperature roasting temperature is 400 ℃ and the high-temperature roasting time is 2 h.
CN202110235665.0A 2021-03-03 2021-03-03 Preparation method of loose porous nano cerium oxide Pending CN112811457A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1443811A (en) * 2003-04-04 2003-09-24 中国科学院上海硅酸盐研究所 Synthesizing nano crystal cobalt aluminium spinelle pigment by using solution combustion method
JP2005126253A (en) * 2003-10-21 2005-05-19 Mitsui Mining & Smelting Co Ltd Cerium oxide, cerium oxide for abrasive material, and their production method
CN101891216A (en) * 2010-07-22 2010-11-24 东北大学 Preparation method of high purity CeB6 nano powder
US20190300384A1 (en) * 2018-03-27 2019-10-03 Savannah River Nuclear Solutions, Llc Single step solution combustion synthesis of crystalline transuranic-doped rare earth zirconate pyrochlores
CN110385121A (en) * 2019-07-26 2019-10-29 江西离子型稀土工程技术研究有限公司 A kind of microwave burning preparation method of cerium-based composite oxides
CN110817927A (en) * 2019-12-26 2020-02-21 江西师范大学 Method for preparing light porous nano cerium oxide by combustion method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1443811A (en) * 2003-04-04 2003-09-24 中国科学院上海硅酸盐研究所 Synthesizing nano crystal cobalt aluminium spinelle pigment by using solution combustion method
JP2005126253A (en) * 2003-10-21 2005-05-19 Mitsui Mining & Smelting Co Ltd Cerium oxide, cerium oxide for abrasive material, and their production method
CN101891216A (en) * 2010-07-22 2010-11-24 东北大学 Preparation method of high purity CeB6 nano powder
US20190300384A1 (en) * 2018-03-27 2019-10-03 Savannah River Nuclear Solutions, Llc Single step solution combustion synthesis of crystalline transuranic-doped rare earth zirconate pyrochlores
CN110385121A (en) * 2019-07-26 2019-10-29 江西离子型稀土工程技术研究有限公司 A kind of microwave burning preparation method of cerium-based composite oxides
CN110817927A (en) * 2019-12-26 2020-02-21 江西师范大学 Method for preparing light porous nano cerium oxide by combustion method

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