CN114620755B - Cerium dioxide nanotube and preparation method thereof - Google Patents
Cerium dioxide nanotube and preparation method thereof Download PDFInfo
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- CN114620755B CN114620755B CN202111652065.0A CN202111652065A CN114620755B CN 114620755 B CN114620755 B CN 114620755B CN 202111652065 A CN202111652065 A CN 202111652065A CN 114620755 B CN114620755 B CN 114620755B
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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
- C01F17/224—Oxides or hydroxides of lanthanides
- C01F17/235—Cerium oxides or hydroxides
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- C01F17/00—Compounds of rare earth metals
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
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Abstract
The application discloses a cerium dioxide nanotube and a preparation method thereof, wherein the inner diameter of the cerium dioxide nanotube is between 4 and 10nm, the outer diameter of the cerium dioxide nanotube is between 20 and 60nm, and the length of the cerium dioxide nanotube is between 100 and 5 mu m. The magnesium hydroxide nanotube is used as a template, and the cerium oxide nanotube is efficiently prepared by adopting an ion exchange method without high-temperature calcination. The method is simple to operate, low in cost and has industrial application prospect.
Description
Technical Field
The application belongs to the field of inorganic nano materials, and particularly relates to a cerium dioxide nanotube and a preparation method thereof.
Background
With the high consumption of fossil fuels, a fuel including NO is produced x Harmful gases therein. Thus, how NO is controlled by denitration techniques x Reducing the environmental impact of human activity is a real problem to be solved. Selective Catalytic Reduction (SCR) is currently the most widely used denitration technique in industry, however, commercially available V 2 O 5 -WO 3 /TiO 2 Or V 2 O 5 -MoO 3 /TiO 2 The catalyst is easy to generate catalyst deactivation phenomenon under the severe reaction working condition. In addition, the vanadium-based catalyst has the defects of high volatility, high toxicity to human bodies and environment and the like, so that the application is greatly limited, and the development of a novel non-toxic or low-toxic transition metal oxide catalyst becomes a research hot spot. Wherein Ce has +3 valence and +4 valence, and the characteristic of valence change endows cerium oxide with unique oxidation and reductionThe original property makes it widely used as catalyst carrier material or active component of catalyst. For example, ceO 2 Can promote the dispersion of CuO, improve the electron and geometry structure of active components, and further improve the oxidation reaction performance of the catalyst in CO. The university of Kunming's wish to star teacher prepare a series of CeO with different morphology 2 The CuO catalyst supported by the carrier (nano particles, nano sheets, nano rods and octahedra) proves that the more oxygen defects on the surface of the catalyst are, the CeO is 2 The stronger the interaction with CuO, the better the catalytic effect, which verifies CeO 2 The morphology of the support has a significant effect on the activity of the catalyst.
The metal oxide with one-dimensional structure comprises nano rods, nano wires, nano tubes and the like, and has good chemical and thermal stability and high crystallinity. The nano tube is a hollow nano rod, has accurate and adjustable tube wall thickness and high specific surface area, and can be used as a mass transfer channel, so that the reactivity is greatly increased. In recent years, the synthesis method of the one-dimensional oxide is greatly expanded, and the method comprises a hydrothermal method, ultrasonic radiation, a sol-gel method, a molten salt method, molecular beam epitaxial growth and solid chemical reaction. For example, chinese patent CN110152658A adopts cerous nitrate hydrothermal method to prepare Pd@CeO 2 Nanotube catalysts. However, the method uses organic PVP and carbon nanotubes as a template agent, and the steps are complicated. Among the numerous methods, ion exchange methods are of great interest, being simple and easy to implement and having industrial prospects. We used Mg (OH) based on previous studies 2 The nano tube is used as a template, and the cerium oxide nano tube is prepared by adopting an ion exchange method. The method is simple, practical and low in cost, and has industrial application prospect.
Disclosure of Invention
The application aims at overcoming the defects of the prior art and provides a cerium oxide nanotube and a preparation method thereof.
In order to achieve the above purpose, the present application adopts the following technical scheme: a cerium oxide nanotube, wherein the inner diameter of the cerium oxide nanotube is between 4 and 10nm, the outer diameter of the cerium oxide nanotube is between 20 and 60nm, and the length of the cerium oxide nanotube is between 100 and 5 mu m.
Further, the cerium dioxide nanotube takes the magnesium hydroxide nanotube as a reaction template, cation exchange is carried out on the cerium salt solution and the magnesium hydroxide nanotube, and then the cerium dioxide nanotube is directly obtained after anion exchange is carried out on the cerium salt solution and the magnesium hydroxide nanotube.
The preparation method of the cerium oxide nano tube is characterized by comprising the following steps:
(1) Mg (OH) 2 Adding the nanotube into cerium salt aqueous solution, stirring for 1-60 h at room temperature, filtering and drying to obtain cation-exchanged nanotube;
(2) Adding the nano tube obtained in the step (1) into an alkali solution, stirring for 1-10 h at room temperature, filtering and drying to obtain the cerium dioxide nano tube.
Further, mg (OH) in step (1) 2 The nano tube is prepared by the following steps: adding a magnesium source into an alkali source solution, fully stirring, placing the mixture in a homogeneous reactor, carrying out hydrothermal reaction at 100-300 ℃ for 12-60 h, rotating at 5-200 rpm, and centrifugally drying the product to obtain Mg (OH) 2 Nanotube templates.
Further, the magnesium source is one or more of magnesium oxide, magnesium carbonate, basic magnesium carbonate, magnesium acetate, magnesium sulfate, magnesium nitrate or magnesium chloride water.
Further, the alkali source is one or a mixture of more than two of sodium hydroxide, potassium hydroxide or ammonia water, and the concentration is 0.1-10.0 mol/L.
Further, the cerium salt in the step (1) is Ce (Ac) 3 、Ce(NO 3 ) 3 、(NH 4 ) 2 Ce(SO 4 ) 2 Or CeCl 3 。
Further, the cerium salt and Mg (OH) in step (1) 2 In the nanotube, the molar ratio of Ce to Mg is 1-5:1.
Further, the alkali solution in the step (2) is sodium hydroxide or potassium hydroxide solution or a mixture of the two.
Further, the concentration of the alkali solution in the step (2) is 0.1 to 0.6mol/L.
The application discloses a cerium dioxide nanotube and a preparation method thereof. The preparation method starts from magnesium source and is simpleThe ceria nano tube can be prepared by a single hydrothermal and ion exchange process, and has the potential of industrialized amplification. Mg (OH) 2 The nano tube is easy to prepare in large quantity, and the ion exchange method is mild and simple, so that the large-scale preparation of the cerium dioxide nano tube can be realized.
Drawings
FIG. 1 shows CeO prepared in examples 1-3 2 Typical X-ray diffraction (XRD) patterns of nanotubes.
FIG. 2 shows CeO in example 1 2 Nanotube TEM transmission electron micrographs.
FIG. 3 is CeO in example 2 2 Nanotube TEM transmission electron micrographs.
FIG. 4 shows CeO in example 3 2 Nanotube TEM transmission electron micrographs.
FIG. 5 is CeO in example 4 2 Nanotube TEM transmission electron micrographs.
Detailed Description
In order that those skilled in the art will better understand the present application, a technical solution in the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in which it is apparent that the described embodiments are only some embodiments of the present application, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present application without making any inventive effort, shall fall within the scope of the present application.
It is noted that the terms "comprises" and "comprising," and any variations thereof, in the description and claims of the present application and in the foregoing figures, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed or inherent to such process, method, article, or apparatus.
The preparation method of the magnesium hydroxide nano tube comprises the following steps:
(1) Adding an alkali source and a magnesium source into a polytetrafluoroethylene hydrothermal kettle, uniformly stirring, and sealing the hydrothermal reaction kettle in a stainless steel autoclave;
(2) Fixing a stainless steel autoclave in a homogeneous phase reactor, and reacting for a certain period of time at a high temperature, wherein the reaction temperature is 100-300 ℃, the reaction time is 12-60 h, and the reaction rotating speed is 5-200 rpm;
(3) And (3) after naturally cooling to room temperature, centrifugally separating the product of the step (2), washing with water and ethanol for three times, and drying for a certain time to obtain the magnesium hydroxide nanotube, wherein the drying temperature is 40-100 ℃ and the drying time is 2-48 h.
The alkali source is one or more of sodium hydroxide, potassium hydroxide or ammonia water. The concentration is 0.1-10 mol/L.
The magnesium source is one or more of magnesium oxide, magnesium carbonate, basic magnesium carbonate, magnesium acetate, magnesium sulfate, magnesium nitrate or magnesium chloride water.
Example 1
The preparation method of the cerium oxide nano tube comprises the following steps:
A. 3.0g of magnesium carbonate was added to a mixed alkali aqueous solution of sodium hydroxide and potassium hydroxide at concentrations of 0.1mol/L and 1.5mol/L, respectively. The mixture was put in a homogeneous reactor at 300℃and 5rpm and was hydrothermally heated for 12 hours. And (5) centrifugally washing and drying to obtain the magnesium hydroxide nanotube template.
B. With Ce (NO) 3 ) 3 Ion exchange was performed at a molar ratio of Ce: mg=1:1 for Ce source. Take 3.0gCe (NO) 3 ) 3 Dissolved in deionized water, followed by the addition of 0.4g of Mg (OH) 2 And (3) stirring the template at room temperature for 1h, filtering and drying to obtain the cation-exchanged nanotube.
C. And B, placing the nano tube prepared in the step B into a 0.1mol/L NaOH solution, stirring for 1h at room temperature, filtering and drying to obtain the final cerium dioxide nano tube.
FIG. 1 is a typical XRD pattern for a nanotube product obtained in this example, with no Mg (OH) in the pattern 2 All diffraction peaks are attributed to ceria; fig. 2 is a typical TEM transmission electron micrograph of the obtained nanotube product showing a significant morphology of the nanotubes, and combining the analysis results of both, it was determined that ceria nanotubes were obtained. Prepared in this exampleThe proportion of the cerium dioxide nano-tube is about 93%, the inner diameter of the tube is 4-8nm, the outer diameter of the tube is 20-40nm, and the length of the tube is between 200nm and 3 mu m.
Example 2
The preparation method of the cerium oxide nano tube comprises the following steps:
A. 1.5g of magnesium oxide and 0.4g of magnesium sulfate were added to an aqueous ammonia solution having a concentration of 5.8mol/L, and the mixture was put in a homogeneous reactor at 240℃and hydrothermal conditions at 100rpm for 60 hours. And (5) centrifugally washing and drying to obtain the magnesium hydroxide nanotube template.
B. By CeCl 3 Ion exchange was performed as Ce salt in a molar ratio of Ce: mg=5:1. 13g CeCl was taken 3 Dissolved in deionized water, followed by the addition of 0.4g of Mg (OH) 2 And (5) stirring the template at room temperature for 6 hours, filtering and drying to obtain the cation-exchanged nanotube.
C. And B, placing the nano tube prepared in the step B into a KOH solution with the concentration of 0.6mol/L, stirring for 10 hours at room temperature, filtering and drying to obtain the final cerium dioxide nano tube.
FIG. 1 is a typical XRD pattern for a nanotube product obtained in this example, with no Mg (OH) in the pattern 2 All diffraction peaks are attributed to ceria; FIG. 3 is a typical TEM transmission electron micrograph of the obtained nanotube product showing a pronounced nanotube morphology, and combining the results of both analyses, it was determined that ceria nanotubes were obtained. The ratio of the cerium oxide nanotubes prepared in this example was about 95%, the inner diameter of the tubes was 5-10nm, the outer diameter was 30-60nm, and the tube length was from 100nm to 5. Mu.m.
Example 3
The preparation method of the cerium oxide nano tube comprises the following steps:
A. 6g of magnesium chloride was added to an aqueous potassium hydroxide solution at a concentration of 0.6mol/L. The mixture was put in a homogeneous reactor at 100℃and 200rpm and then hydrothermal-treated for 60 hours. And (5) centrifugally washing and drying to obtain the magnesium hydroxide nanotube template.
B. With Ce (Ac) 3 Ion exchange was performed as Ce salt in a molar ratio of Ce: mg=3:1. 6.6g Ce (Ac) 3 Dissolved in deionized water, followed by the addition of 0.4g of Mg (OH) 2 And (5) stirring the template at room temperature for 16h, filtering and drying to obtain the cation-exchanged nanotube.
C. And (3) placing the nano tube prepared in the step (B) into a mixed solution of 0.3mol/L NaOH and 0.1mol/L KOH, stirring for 8 hours at room temperature, filtering and drying to obtain the final cerium dioxide nano tube.
FIG. 1 is a typical XRD pattern for a nanotube product obtained in this example, with no Mg (OH) in the pattern 2 All diffraction peaks are attributed to ceria; fig. 4 is a typical TEM transmission electron micrograph of the obtained nanotube product showing a significant morphology of the nanotubes, and combining the analysis results of both, it was determined that ceria nanotubes were obtained. The ratio of the cerium oxide nanotubes prepared in this example was about 97%, the inner diameter of the tubes was 5-10nm, the outer diameter was 20-60nm, and the tube length was from 100nm to 4. Mu.m.
Example 4
The preparation method of the cerium oxide nano tube comprises the following steps:
A. 2g of magnesium acetate was added to a 10.0mol/L aqueous potassium hydroxide solution and the mixture was put into a homogeneous reactor at 200℃and 120rpm for 12 hours. And (5) centrifugally washing and drying to obtain the magnesium hydroxide nanotube template.
B. Ion exchange was performed with cerium ammonium sulphate as Ce salt in a molar ratio Ce: mg=5:1. 30g of ammonium cerium sulfate was dissolved in deionized water, followed by the addition of 0.4g of Mg (OH) 2 And (5) stirring the template at room temperature for 60 hours, filtering and drying to obtain the cation-exchanged nanotube.
C. And B, placing the nano tube prepared in the step B into a mixed solution of 0.1mol/L NaOH and 0.2mol/L KOH, stirring for 10 hours at room temperature, filtering and drying to obtain the final cerium dioxide nano tube.
FIG. 1 is a typical XRD pattern for a nanotube product obtained in this example, with no Mg (OH) in the pattern 2 All diffraction peaks are attributed to ceria; fig. 5 is a typical TEM transmission electron micrograph of the obtained nanotube product showing a significant morphology of the nanotubes, and combining the analysis results of both, it was determined that ceria nanotubes were obtained. The ratio of the cerium oxide nanotubes prepared in this example was about 96%, the inner diameter of the tubes was 5-10nm, the outer diameter was 30-60nm, and the tube length was from 100nm to 4. Mu.m.
The above description is only of the preferred embodiments of the present application and is not intended to limit the present application, but various modifications and variations can be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (9)
1. A ceria nanotube, characterized by: the inner diameter of the cerium dioxide nano tube is between 4 and 10nm, the outer diameter is between 20 and 60nm, and the tube length is between 100 and 5 mu m;
the cerium dioxide nanotube takes a magnesium hydroxide nanotube as a reaction template, performs cation exchange with the magnesium hydroxide nanotube through cerium salt solution, and is placed in alkaline solution for anion exchange to directly obtain the cerium dioxide nanotube;
the magnesium hydroxide nano tube is prepared by the following steps: adding an alkali source and a magnesium source into a polytetrafluoroethylene hydrothermal kettle, uniformly stirring, sealing the hydrothermal reaction kettle in a stainless steel autoclave, fixing the stainless steel autoclave in a homogeneous phase reactor, carrying out hydrothermal reaction at 100-300 ℃ for 12-60 h at a rotating speed of 5-200 rpm, and centrifuging and drying the product to obtain a magnesium hydroxide nanotube template;
the magnesium source is one or more of magnesium oxide, magnesium carbonate, basic magnesium carbonate, magnesium acetate, magnesium sulfate, magnesium nitrate or magnesium chloride.
2. A method for preparing the ceria nano tube according to claim 1, comprising the steps of:
(1) Mg (OH) 2 Adding the nanotube into cerium salt aqueous solution, stirring for 1-60 h at room temperature, filtering and drying to obtain cation-exchanged nanotube;
(2) Adding the nano tube obtained in the step (1) into an alkali solution, stirring for 1-10 h at room temperature, filtering and drying to obtain the cerium dioxide nano tube.
3. The preparation method according to claim 2, characterized in that: mg (OH) in said step (1) 2 The nano tube is prepared by the following steps: adding a magnesium source into an alkali source solution, fully stirring, and placing the mixture in a homogeneous reactor at 100-300 DEG CHydrothermal reaction is carried out for 12-60 h, the rotating speed is 5-200 rpm, and the product is centrifugally dried to obtain Mg (OH) 2 Nanotube templates.
4. A method of preparation according to claim 3, characterized in that: the magnesium source is one or more of magnesium oxide, magnesium carbonate, basic magnesium carbonate, magnesium acetate, magnesium sulfate, magnesium nitrate or magnesium chloride.
5. A method of preparation according to claim 3, characterized in that: the alkali source is one or a mixture of more than two of sodium hydroxide, potassium hydroxide or ammonia water, and the concentration is 0.1-10.0 mol/L.
6. The preparation method according to claim 2, characterized in that: the cerium salt in the step (1) is Ce (Ac) 3 、Ce(NO 3 ) 3 、(NH 4 ) 2 Ce(SO 4 ) 2 Or CeCl 3 。
7. The preparation method according to claim 2, characterized in that: the cerium salt and Mg (OH) in the step (1) 2 In the nanotube, the molar ratio of Ce to Mg is 1-5:1.
8. The preparation method according to claim 2, characterized in that: the alkali solution in the step (2) is sodium hydroxide or potassium hydroxide solution or a mixture of the two.
9. The preparation method according to claim 2, characterized in that: the concentration of the alkali solution in the step (2) is 0.1-0.6 mol/L.
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