CN115571904A - Growing CeO on SiC powder 2 Method for preparing nano-rod and SiC loaded CeO prepared by method 2 Nano-rod composite structure - Google Patents
Growing CeO on SiC powder 2 Method for preparing nano-rod and SiC loaded CeO prepared by method 2 Nano-rod composite structure Download PDFInfo
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- CN115571904A CN115571904A CN202211175464.7A CN202211175464A CN115571904A CN 115571904 A CN115571904 A CN 115571904A CN 202211175464 A CN202211175464 A CN 202211175464A CN 115571904 A CN115571904 A CN 115571904A
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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
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
- B01J27/224—Silicon carbide
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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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- 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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- 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
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- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Abstract
The invention discloses a method for growing CeO on SiC powder 2 Method for preparing nano-rod and SiC loaded CeO prepared by method 2 And (3) a nanorod composite structure. The method comprises the following steps: (1) calcining SiC powder; (2) Adding Ce (NO) 3 ) 3 Mixing the aqueous solution and the NaOH solution, and stirring at normal temperature to prepare a precursor solution; then, adding the calcined SiC powder into the precursor solution, and continuously stirring to obtain mixed slurry; (3) Carrying out hydrothermal reaction on the mixed slurry, carrying out suction filtration separation, washing and drying after the reaction is cooled, and obtaining intermediate product powder; (4) Calcining the intermediate product powder at high temperature in air atmosphere,cooling to obtain the CeO grown 2 SiC powder of nano-rods. CeO grown by the invention 2 The nano-rod structure is a nano-rod structure, is not polycrystalline particles, and has large specific surface area, high catalytic activity and high utilization rate; the synthesis process is simple, the preparation period is short, and the large-scale batch production is facilitated.
Description
Technical Field
The invention relates to the technical field of catalysts, in particular to a method for growing CeO on SiC powder 2 Method for preparing nano-rod and SiC loaded CeO prepared by method 2 A nanorod composite structure.
Background
The support has a significant effect on the performance of the catalyst. Suitable carriers not only can carry catalytically active components, but also can improve the stability and activity of the catalyst. SiC is a catalyst carrier which has a high attention degree in recent years, and has the characteristics of high mechanical strength, high thermal conductivity, small thermal expansion coefficient, high thermal stability, acid and alkali corrosion resistance and the like. Therefore, the SiC is used as the carrier, so that the catalyst deactivation caused by sintering and agglomeration of the noble metal in the reaction process can be effectively prevented, and the catalyst can be ensured to play a catalytic performance more stably under various environments. CeO (CeO) 2 Is an important noble metal catalyst promoter. The unique valence-changing capability of Ce element enables CeO 2 The surface is rich in oxygen vacancies so that small oxygen-containing molecules can be activated. CeO (CeO) 2 The strong interaction with the noble metal leads the metal to be in CeO 2 The surface high dispersion degree is high, and the utilization rate of the noble metal can be effectively improved. Thus, with SiC as carrier, ceO 2 The noble metal-loaded catalyst serving as an auxiliary agent has wide and important application prospects in various high and new technical fields of environmental management, synthetic chemistry, new energy and the like.
Preparation of SiC loaded CeO with large specific surface area and high catalytic activity 2 The structure is the premise and the basis for preparing the noble metal catalyst with high catalytic activity, while the prior SiC loads CeO 2 In the structure of CeO 2 In polycrystalline, planar formCovering the surface of SiC, the catalyst has small specific surface area, low utilization rate and low catalytic activity.
Disclosure of Invention
The invention aims to provide a method for simply, conveniently and efficiently growing CeO on SiC powder in order to overcome the defects in the prior art 2 Method for preparing nano-rod, siC loaded CeO obtained by the method 2 The nano-rod composite structure has large specific surface area and high catalytic activity.
The invention relates to a method for growing CeO on SiC powder 2 A method for nanorods, comprising the steps of:
(1) Calcining the SiC powder;
(2) Adding Ce (NO) 3 ) 3 Mixing the aqueous solution and the NaOH solution, and stirring at normal temperature to prepare a precursor solution; then, adding the calcined SiC powder into the precursor solution, and continuously stirring to obtain mixed slurry;
(3) Carrying out hydrothermal reaction on the mixed slurry, carrying out suction filtration separation, washing and drying after the reaction is cooled to obtain intermediate product powder;
(4) Calcining the intermediate product powder at high temperature in air atmosphere, and cooling to obtain the CeO grown 2 SiC powder of nano-rod; the calcining temperature is 500-900 ℃, the calcining time is 2-6 hours, the calcining atmosphere is air atmosphere, and the calcining pressure is normal pressure.
Further, the grain diameter of the SiC powder in the step (1) is 200nm-5 μm.
Further, in the step (4), the calcining temperature is 500-900 ℃, the calcining time is 2-6 hours, the calcining atmosphere is air atmosphere, and the calcining pressure is normal pressure.
Further, ce (NO) in step (2) 3 ) 3 The concentration of the solution is 0.3-0.5mol/L, the concentration of the NaOH solution is 4-10mol/L, and the temperature of the solution is room temperature.
Further, the stirring mode in the step (2) is constant-temperature magnetic stirring, and the stirring speed is 100-400r/min.
Furthermore, when the precursor solution is prepared, the stirring time is 0.5-3 hours, and the molar ratio of Ce to Na ions in the precursor solution is 0.005-0.02.
Furthermore, when the mixed slurry is prepared, the stirring time is 3-24 hours, and the molar ratio of Ce to Si in the mixed slurry is 0.01-0.1.
Further, the reaction temperature in the step (3) is 100-200 ℃, and the reaction time is 18-30 hours.
Further, in the step (3), the drying temperature is 60 ℃, and the drying time is 8-18 hours.
The SiC loaded CeO prepared by the method 2 And (3) a nanorod composite structure.
The invention and the prior SiC loaded CeO 2 Compared with the structure, the structure has the following beneficial effects: (1) CeO grown by the invention 2 The nano-rod structure is a nano-rod structure, is not polycrystalline particles, and has large specific surface area, high catalytic activity and high utilization rate; (2) The synthesis process is simple, the preparation period is short, and large-scale batch production is facilitated.
Drawings
FIG. 1 is a graph showing CeO grown on the obtained material in example 1 of the present invention 2 XRD pattern of SiC powder of nano rod.
FIG. 2 shows CeO grown on the glass substrate obtained in example 1 of the present invention 2 SEM photograph of SiC powder of the nano-rod.
Detailed Description
The following are specific embodiments of the present invention and are further described with reference to the accompanying drawings, but the present invention is not limited to these embodiments.
Example 1
A method for growing CeO2 nanorods on SiC powder comprises the following steps:
(1) The SiC powder with the grain diameter of 400nm is calcined in the air atmosphere at normal pressure at 700 ℃ for 6 hours.
(2) First Ce (NO) 3 ) 3 ·6H 2 Dissolving O in deionized water to prepare Ce (NO) with concentration of 0.4mol/L 3 ) 3 A solution; dissolving NaOH in deionized water to prepare a NaOH solution with the concentration of 6 mol/L; adding Ce (NO) 3 ) 3 Mixing the solution and NaOH solution, stirring for 0.5 hr at normal temperatureStirring speed is 200r/min, and precursor solution is obtained. The molar ratio of Ce to Na ions in the precursor solution is 0.01; then, adding the calcined SiC powder into the precursor solution, and stirring at normal temperature for 3 hours at a stirring speed of 200r/min to obtain mixed slurry, wherein the molar ratio of Ce to Si in the slurry is 0.02;
(3) Transferring the mixed slurry into a polytetrafluoroethylene high-pressure reaction kettle for reaction at the reaction temperature of 100 ℃ for 24 hours, cooling the reaction, performing suction filtration and separation, washing, and drying at the temperature of 60 ℃ for 12 hours to obtain intermediate product powder;
(4) Calcining the intermediate product powder at high temperature of 600 ℃ for 3 hours in an air atmosphere at normal pressure, and cooling to obtain the CeO grown in the air atmosphere 2 SiC powder of nano-rods.
FIG. 1 shows CeO grown thereon obtained in example 1 of the present invention 2 XRD pattern of SiC powder of nano rod. XRD pattern shows that the synthesized powder only contains SiC and CeO 2 Composition, no other impurity phase exists. FIG. 2 shows CeO grown on the glass substrate obtained in example 1 of the present invention 2 SEM photograph of SiC powder of the nanorods. CeO among SiC powder 2 The nanorods were clearly visible.
Example 2
A method for growing CeO2 nanorods on SiC powder comprises the following steps:
(1) And (2) carrying out calcination treatment on the SiC powder with the particle size of 500nm, wherein the calcination atmosphere is air atmosphere, the calcination pressure is normal pressure, the calcination temperature is 800 ℃, and the calcination time is 2 hours.
(2) First Ce (NO) 3 ) 3 ·6H 2 Dissolving O in deionized water to prepare Ce (NO) with concentration of 0.3mol/L 3 ) 3 A solution; dissolving NaOH in deionized water to prepare a NaOH solution with the concentration of 10 mol/L; ce (NO) 3 ) 3 And mixing the solution with NaOH solution, and stirring for 3 hours at normal temperature at the stirring speed of 400r/min to obtain a precursor solution. The molar ratio of Ce to Na ions in the precursor solution is 0.005; then, adding the calcined SiC powder into the precursor solution, and carrying out normal temperature treatmentStirring for 10 hours at the stirring speed of 400r/min to obtain mixed slurry, wherein the molar ratio of Ce to Si in the slurry is 0.05;
(3) Transferring the mixed slurry into a polytetrafluoroethylene high-pressure reaction kettle for reaction at the reaction temperature of 200 ℃ for 18 hours, cooling the reaction, performing suction filtration separation, washing, and drying at the temperature of 60 ℃ for 18 hours to obtain intermediate product powder;
(4) Calcining the intermediate product powder at high temperature of 900 ℃ for 2 hours in air atmosphere at normal pressure, and cooling to obtain the CeO grown in the air atmosphere 2 SiC powder of nano-rods.
Example 3
A method for growing CeO2 nanorods on SiC powder comprises the following steps:
(1) The SiC powder with the grain diameter of 5 mu m is calcined in the air atmosphere at the normal pressure at 800 ℃ for 2 hours.
(2) First Ce (NO) 3 ) 3 ·6H 2 Dissolving O in deionized water to prepare Ce (NO) with concentration of 0.5mol/L 3 ) 3 A solution; dissolving NaOH in deionized water to prepare a NaOH solution with the concentration of 4 mol/L; ce (NO) 3 ) 3 And mixing the solution with NaOH solution, and stirring for 6 hours at normal temperature at the stirring speed of 500r/min to obtain a precursor solution. The molar ratio of Ce to Na ions in the precursor solution is 0.02; then, adding the calcined SiC powder into the precursor solution, and stirring at normal temperature for 24 hours at a stirring speed of 500r/min to obtain mixed slurry, wherein the molar ratio of Ce to Si in the slurry is 0.1;
(3) Transferring the mixed slurry into a polytetrafluoroethylene high-pressure reaction kettle for reaction at the reaction temperature of 100 ℃ for 30 hours, cooling the reaction, performing suction filtration and separation, washing, and drying at the temperature of 60 ℃ for 8 hours to obtain intermediate product powder;
(4) Calcining the intermediate product powder at high temperature in air atmosphere, wherein the calcining temperature is 500 ℃, the calcining time is 6 hours, the calcining atmosphere is air atmosphere, and the calcining pressure isAt normal pressure, cooling to obtain CeO 2 SiC powder of nano-rods.
The above is not mentioned, is suitable for the prior art.
While certain specific embodiments of the present invention have been described in detail by way of illustration, it should be understood by those skilled in the art that the foregoing description is for purposes of illustration only and not by way of limitation, and that various modifications, additions and substitutions can be made to the specific embodiments described without departing from the scope of the invention as defined in the accompanying claims. It should be understood by those skilled in the art that any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention shall be included in the scope of the present invention.
Claims (10)
1. CeO growing on SiC powder 2 The method for preparing the nano rod is characterized by comprising the following steps:
(1) Calcining the SiC powder;
(2) Adding Ce (NO) 3 ) 3 Mixing the aqueous solution and the NaOH solution, and stirring at normal temperature to prepare a precursor solution; then, adding the calcined SiC powder into the precursor solution, and continuously stirring to obtain mixed slurry;
(3) Carrying out hydrothermal reaction on the mixed slurry, carrying out suction filtration separation, washing and drying after the reaction is cooled, and obtaining intermediate product powder;
(4) Calcining the intermediate product powder at high temperature in the air atmosphere, and cooling to obtain the CeO grown 2 SiC powder of nanorods, i.e. SiC-loaded CeO 2 A nanorod composite structure; the calcining temperature is 500-900 ℃, the calcining time is 2-6 hours, the calcining atmosphere is air atmosphere, and the calcining pressure is normal pressure.
2. Growing CeO on SiC powder according to claim 1 2 The method of the nano rod is characterized in that the grain diameter of the SiC powder in the step (1) is 200nm-5 mu m.
3. Growing CeO on SiC powder according to claim 1 2 The method for preparing the nano-rod is characterized in that the calcining temperature in the step (4) is 500-900 ℃, the calcining time is 2-6 hours, the calcining atmosphere is air atmosphere, and the calcining pressure is normal pressure.
4. Growing CeO on SiC powder according to claim 1 2 The method of nanorods, characterized in that, in step (2), ce (NO) is added 3 ) 3 The concentration of the solution is 0.3-0.5mol/L, the concentration of the NaOH solution is 4-10mol/L, and the temperature of the solution is room temperature.
5. Growing CeO on SiC powder according to claim 1 2 The method for preparing the nano-rods is characterized in that the stirring mode in the step (2) is constant-temperature magnetic stirring, and the stirring speed is 100-400r/min.
6. Growing CeO on SiC powder according to claim 1 2 The method of the nano rod is characterized in that when the precursor solution is prepared, the stirring time is 0.5 to 3 hours, and the molar ratio of Ce to Na ions in the precursor solution is 0.005 to 0.02.
7. Growing CeO on SiC powder according to claim 1 2 The method for preparing the nano-rod is characterized in that when mixed slurry is prepared, the stirring time is 3-24 hours, and the molar ratio of Ce to Si in the mixed slurry is 0.01-0.1.
8. Growing CeO on SiC powder according to claim 1 2 The method of the nano rod is characterized in that the reaction temperature in the step (3) is 100-200 ℃, and the reaction time is 18-30 hours.
9. Growing CeO on SiC powder according to claim 1 2 The method for preparing the nano-rod is characterized in that the drying temperature in the step (3) is 60 ℃, and the drying time is 8-18 hours.
10. SiC loaded CeO prepared by the method according to any one of claims 1 to 9 2 A nanorod composite structure.
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2022
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