CN111215033A - Porous CeO wrapped by N, S doped C2Synthesis method of nano rod - Google Patents
Porous CeO wrapped by N, S doped C2Synthesis method of nano rod Download PDFInfo
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- CN111215033A CN111215033A CN201911255050.3A CN201911255050A CN111215033A CN 111215033 A CN111215033 A CN 111215033A CN 201911255050 A CN201911255050 A CN 201911255050A CN 111215033 A CN111215033 A CN 111215033A
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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Abstract
Porous CeO wrapped by N, S doped C2The synthesis method of the nano-rod comprises the steps of dissolving cerium nitrate hexahydrate and trimesic acid in absolute ethyl alcohol and deionized water to obtain mixed solution; adding sulfanilic acid into the mixed solution, and stirring to dissolve sulfanilic acid to obtain a mixed solution; and transferring the mixed solution into a reaction container, heating for reaction for a period of time, centrifugally separating and collecting a product, washing and drying to obtain a precursor. Calcining the precursor in a protective atmosphere to obtain porous CeO2And (4) nanorods. According to the synthesis method, the Ce-based MOF with uniform appearance is synthesized through one-step simple solvothermal reaction; ce-based MOF is used as a precursor, N and S elements are introduced by using sulfanilic acid as a regulator, and the CeO coated with N and S doped C is synthesized by in-situ calcination2Synthesized ofCeO2Has a porous rod-like structure.
Description
Technical Field
The invention relates to synthesis of MOFs nano-materials, in particular to porous CeO wrapped by N, S doped C2A method for synthesizing nano-rods.
Background
CeO2Is a rare earth oxide with wide application and low price, and has the property of an N-type semiconductor. CeO (CeO)2Has the advantages of no toxicity, low cost, high chemical stability, rich reserves and the like. CeO (CeO)2The wide band gap limits its application in the visible region. At the same time, the CeO is bulky2Has a smaller specific surface area and generally exposes fewer active sites. And CeO of porous structure2Will increaseIts specific surface area, generates more active sites. At present, in the process of synthesizing Ce-based MOF, a regulator (sulfanilic acid) is introduced to realize CeO2Studies on the control of size, morphology and composition have not been reported.
Disclosure of Invention
In the process of synthesizing Ce-based MOF, the invention introduces a N, S-containing regulator (sulfanilic acid) to realize the regulation of the morphology and the size of the Ce-based MOF, and the N, S C-doped coated CeO is synthesized by in-situ calcination of the Ce-based MOF under inert gas2And (4) nanorods.
Specifically, the invention provides porous CeO wrapped by N, S doped C2The synthesis method of the nano rod comprises the following steps:
s1: dissolving cerium nitrate hexahydrate and trimesic acid in absolute ethyl alcohol and deionized water to obtain a mixed solution; adding sulfanilic acid into the mixed solution, and stirring to dissolve sulfanilic acid to obtain a mixed solution; transferring the mixed solution into a reaction container, heating and reacting for a period of time, centrifugally separating and collecting a product, washing and drying to obtain a precursor;
s2: calcining the precursor in a protective atmosphere to obtain porous CeO2And (4) nanorods.
Further, the molar ratio of the cerium nitrate hexahydrate to the trimesic acid is 1: 1.
further, the volume ratio of the absolute ethyl alcohol to the deionized water is 1: 1.
further, the heating temperature of the heating reaction in the step S1 is 60 ℃, and the reaction time is 1 h.
Further, the step S2 specifically includes: calcining the precursor in a tube furnace filled with argon to obtain porous CeO2The nano-rods are prepared, wherein the calcining temperature is 600 ℃, and the calcining time is 3-4 h.
The invention also provides porous CeO coated by N, S doped C prepared by the synthesis method2And (4) nanorods.
Compared with the prior art, the invention has the beneficial effects that:
the synthetic method of the invention adopts one-step simple solvothermal reaction,synthesizing Ce-based MOF with uniform appearance; the Ce-based MOF is used, N and S elements are introduced by taking sulfanilic acid as a regulator, and the CeO coated with N and S doped C is synthesized by in-situ calcination2Synthesized CeO2Has a porous rod-like structure.
Drawings
FIG. 1 is an X-ray powder diffraction pattern (a) and a scanning electron micrograph (b) of a precursor prepared according to an embodiment of the present invention;
FIG. 2 shows porous CeO prepared according to an example of the present invention2X-ray powder diffraction pattern (a) of the nano-rods and scanning electron microscope pattern (b) of the product;
FIG. 3 shows porous CeO prepared according to an example of the present invention2A nitrogen adsorption/desorption curve (a) and a pore size distribution map (b) of the nanorods;
FIG. 4 shows porous CeO prepared according to an example of the present invention2Transmission electron micrograph (a) of nanorods and enlarged porous CeO2Transmission electron micrograph (b) of the nanorods;
FIG. 5 shows porous CeO prepared according to an example of the present invention2Single CeO of nano rod2Scanning electron micrograph (a) and elemental map (b-f) of the rod.
The specific implementation mode is as follows:
the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Examples
Porous CeO wrapped by N, S doped C2The synthesis method of the nano rod comprises the following steps:
0.434g (1mmol) of cerium nitrate hexahydrate and 0.210g (1mmol) of trimesic acid were weighed and dissolved in 15mL of absolute ethanol and 15mL of deionized water, 0.250g (1.45mmol) of sulfanilic acid was added to the above solution, and the mixture was stirred and dissolved, and the above mixed solution was transferred to a round-bottomed flask, heated to 60 ℃ and reacted for 1 hour. And collecting the product through centrifugal separation, washing the product for several times by using industrial alcohol, and placing the product in an oven for overnight drying to obtain a precursor. Fig. 1 shows XRD patterns (fig. 1a) and scanning electron micrographs (fig. 1b) of the precursors obtained under the experimental conditions described above. The XRD pattern indicated that the resulting product was a Ce-based MOF, and the scanning electron micrograph indicated that the resulting product was a rod-like structure with relatively uniform particle size.
Calcining the dried product in a tubular furnace filled with argon to obtain porous CeO2The nano-rods are prepared, wherein the calcining temperature is 600 ℃, and the calcining time is 3-4 h. FIG. 2 XRD pattern (FIG. 1a) and scanning electron micrograph (FIG. 1b) of the calcined product under the experimental conditions described above. The XRD pattern indicated that the resulting product was CeO2Scanning electron micrographs show that the obtained product has a relatively uniform rod-like structure. FIG. 3 shows porous CeO prepared in this example2The nitrogen adsorption/desorption curve (a) and the pore size distribution map (b) of the nanorods show that CeO2Has a specific surface area of 27.077m2/g，CeO2The pore size distribution diagram shows that the product is a mesoporous material. FIG. 4 shows (a) CeO2Transmission Electron Micrographs (TEMs); amplified CeO2Transmission Electron Micrograph (TEM) of (c), fig. 4a shows the synthesized CeO2Is a rod-shaped structure formed by stacking a plurality of small particles. FIG. 4b shows a rod-shaped CeO2There are many nanopores. FIG. 5(a) Individual CeO2Scanning Electron Micrographs (SEM) of the rods; (b-f) CeO2Elemental mapping of the rods, it can be seen that the N, S element is incorporated into CeO2In the rod, C is coated in CeO2On a rod.
Claims (6)
1. Porous CeO wrapped by N, S doped C2The synthesis method of the nano rod is characterized by comprising the following steps:
s1: dissolving cerium nitrate hexahydrate and trimesic acid in absolute ethyl alcohol and deionized water to obtain a mixed solution; adding sulfanilic acid into the mixed solution, and stirring to dissolve sulfanilic acid to obtain a mixed solution; transferring the mixed solution into a reaction container, heating and reacting for a period of time, centrifugally separating and collecting a product, washing and drying to obtain a precursor;
s2: in a protective atmosphereCalcining the precursor to obtain porous CeO2And (4) nanorods.
2. The porous CeO coated with N, S doped C as claimed in claim 12The synthesis method of the nanorod is characterized in that the molar ratio of the cerous nitrate hexahydrate to the trimesic acid is 1: 1.
3. the porous CeO coated with N, S doped C as claimed in claim 12The synthesis method of the nanorod is characterized in that the volume ratio of the absolute ethyl alcohol to the deionized water is 1: 1.
4. the porous CeO coated with N, S doped C as claimed in claim 12The synthesis method of the nanorod is characterized in that the heating temperature of the heating reaction in the step S1 is 60 ℃, and the reaction time is 1 h.
5. The porous CeO coated with N, S doped C as claimed in claim 12The nanorod synthesis method is characterized in that the step S2 specifically comprises the following steps: calcining the precursor in a tube furnace filled with argon to obtain porous CeO2The nano-rods are prepared, wherein the calcining temperature is 600 ℃, and the calcining time is 3-4 h.
6. Porous CeO coated with N, S doped C prepared by the synthesis method of any of the preceding claims2And (4) nanorods.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111790380A (en) * | 2020-08-04 | 2020-10-20 | 江苏师范大学 | Preparation method of fan-shaped structure photocatalyst assembled by uniform carbon-coated silver nanoparticles |
| CN115888686A (en) * | 2022-12-27 | 2023-04-04 | 安徽师范大学 | Cerium oxide @ carbon composite catalyst and synthesis method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101982414A (en) * | 2010-10-19 | 2011-03-02 | 北京航空航天大学 | Method for preparing doped nano ceria powder by utilizing solvent-thermal method |
| CN107556329A (en) * | 2017-09-29 | 2018-01-09 | 福州大学 | A kind of porous metals organic framework materials and preparation method thereof |
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2019
- 2019-12-10 CN CN201911255050.3A patent/CN111215033A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101982414A (en) * | 2010-10-19 | 2011-03-02 | 北京航空航天大学 | Method for preparing doped nano ceria powder by utilizing solvent-thermal method |
| CN107556329A (en) * | 2017-09-29 | 2018-01-09 | 福州大学 | A kind of porous metals organic framework materials and preparation method thereof |
Non-Patent Citations (4)
| Title |
|---|
| SUN LIMING等: "Significantly enhanced photocatalytic performance of In2O3 hollow spheres via the coating effect of an N,S-codoped carbon layer", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
| WENJIE SUN等: "Insights into the Pyrolysis Processes of Ce-MOFs for Preparing Highly Active Catalysts of Toluene Combustion", 《CATALYSTS》 * |
| YUFEI XUE等: "The mechanism of photocatalyst and the effects of co-doping CeO2 on refractive index and reflectivity from DFT calculation", 《COMPUTATIONAL MATERIALS SCIENCE》 * |
| 田蕊: "锂硫电池正极材料和结构改性及其电化学性能研究", 《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅱ辑》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111790380A (en) * | 2020-08-04 | 2020-10-20 | 江苏师范大学 | Preparation method of fan-shaped structure photocatalyst assembled by uniform carbon-coated silver nanoparticles |
| CN111790380B (en) * | 2020-08-04 | 2022-10-04 | 江苏师范大学 | Preparation method of fan-shaped structure photocatalyst assembled by uniform carbon-coated silver nanoparticles |
| CN115888686A (en) * | 2022-12-27 | 2023-04-04 | 安徽师范大学 | Cerium oxide @ carbon composite catalyst and synthesis method and application thereof |
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Application publication date: 20200602 |