CN111790383A - Method for preparing CeO derived from Ce-BTC by in-situ reduction one-bath process2Method for loading Pd nano-catalyst - Google Patents
Method for preparing CeO derived from Ce-BTC by in-situ reduction one-bath process2Method for loading Pd nano-catalyst Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 34
- 238000011068 loading method Methods 0.000 title claims abstract description 12
- 239000011943 nanocatalyst Substances 0.000 title claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 39
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 21
- 230000003197 catalytic effect Effects 0.000 claims abstract description 17
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 claims abstract description 14
- 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 claims abstract description 14
- 230000003647 oxidation Effects 0.000 claims abstract description 13
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 11
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 7
- 230000001590 oxidative effect Effects 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 3
- 229910002666 PdCl2 Inorganic materials 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 24
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 12
- 229910000510 noble metal Inorganic materials 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 4
- 101150003085 Pdcl gene Proteins 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 6
- 239000011148 porous material Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 229910052684 Cerium Inorganic materials 0.000 description 2
- 230000010718 Oxidation Activity Effects 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000012621 metal-organic framework Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 231100000344 non-irritating Toxicity 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
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Abstract
Method for preparing CeO derived from Ce-BTC by in-situ reduction one-bath process2A method for loading a Pd nano catalyst, belonging to the field of nano material preparation. Firstly, dimethylformamide is added into a container, and then cerium nitrate, trimesic acid and PdCl are sequentially added2The solution is stirred for 1h, then heated to 100 ℃ and kept for 24h, and then cooled to 140 ℃ and kept for 6h, and stirring is kept during the process. Obtained by centrifuging, washing and drying the solutionThe product is roasted at 800 ℃ in the atmosphere of air and nitrogen to obtain the final in-situ xPd-CeO2A catalyst. Compared with the traditional two-step supported catalyst, the sample of the application has better CO catalytic oxidation performance. The material has the advantages of novel and simple preparation method, controllable process, high specific surface area, narrow particle size distribution of noble metal, excellent CO catalytic oxidation performance and the like.
Description
Technical Field
The invention relates to Ce-BTC derived CeO prepared by an in-situ reduction one-bath method2The Pd nano-catalyst is loaded, so that the high-efficiency catalytic oxidation of CO can be realized. In particular to a method for successfully preparing xPd-Ce-BTC-A500, xPd-Ce-BTC-A800, xPd-Ce-BTC-N500, xPd-Ce-BTC-N800 and other series in-situ xPd-CeO by adopting an in-situ reduction one-bath method2And (3) a nano catalyst. The performance of a sample calcined by reducing nitrogen in situ by a one-bath method for catalyzing CO oxidation is superior to that of a traditional two-step method supported catalyst, and belongs to the field of nano material preparation.
Background
CO is a gas which has wide source, is easy to generate in daily life and has great harmfulness. It is colorless, odorless, non-irritating, and has blood and nerve toxicity. Any carbonaceous matter may produce CO when the combustion is insufficient, such as fuel combustion, thermal power generation, and the like, and trace CO is also commonly discharged from automobile exhaust. One of the most effective methods for eliminating CO exhaust gas is catalytic oxidation, and common catalysts include non-noble metal oxide catalysts and supported noble metal catalysts. CeO (CeO)2As a typical transition metal oxide, the catalyst has good catalytic performance, and has coordination with noble metals such as Au, Pd and the like, so that the catalytic activity can be further improved. Ce-BTC is a very excellent cerium source as a cerium-based MOFs material, and CeO can be obtained by calcining it2. For Ce-BTC, a material, researchers have attempted to apply it to CO catalytic oxidation. Although the research is carried out, on one hand, the process of loading the precious metal to the Ce-BTC is complex, and the metal particle size is large; on the other hand, the prepared catalyst has no high temperature resistance and is difficult to be applied to practical scenes such as automobile exhaust treatment and the like. Therefore, it is required to develop a simple method for preparing a Ce-BTC supported noble metal catalyst, and simultaneously, the catalyst has good thermal stability and excellent catalysis through subsequent treatmentCO oxidation performance. To our knowledge, no relevant report that the catalyst prepared by the in-situ reduction one-bath method has good performance of catalyzing and oxidizing CO at high temperature exists at present. In the invention, a precursor required by Ce-BTC and a precursor of Pd are mixed in dimethylformamide, the reduction rate of Pd and the self-assembly rate of Ce-BTC are controlled by temperature, the precursor of Pd is reduced in a Ce-BTC pore channel, fine particle size and high dispersion are kept under the action of pore channel confinement, and the in-situ Pd-Ce-BTC catalyst is successfully prepared in situ in one bath2But still keeps the porous structure, and the Pd particles are still limited in the pore channels, and still keeps the small particle size and the high dispersion state, which is beneficial to improving the thermal stability and the catalytic performance. Therefore, the in-situ reduction one-bath method is used for successfully preparing the in-situ xPd-CeO2(x is the mass ratio of Pd to Ce, about 1%) and has innovativeness; meanwhile, the catalytic activity of the sample calcined by nitrogen on CO oxidation is better.
Disclosure of Invention
The invention aims to provide a method for preparing CeO derived from Ce-BTC by an in-situ reduction one-bath process2Pd-loaded in-situ xPd-CeO2The specific catalyst is xPd-Ce-BTC (x is the mass ratio of Pd to Ce and is about 1 percent), and the catalyst calcined by the one-bath method in-situ reduction nitrogen shows excellent CO catalytic oxidation activity.
In-situ reduction one-bath method for preparing Ce-BTC derived CeO by efficiently catalyzing and oxidizing CO2The method for supporting the Pd nano-catalyst is characterized by comprising the following steps of:
in-situ reduction one-bath method is adopted to prepare in-situ xPd-CeO2The catalyst, usually dimethylformamide, is added to a vessel, followed by the sequential addition of cerium nitrate, trimesic acid and PdCl2Solution (corresponding to Pd load capacity), wherein the solution needs to be uniformly dispersed before adding new reactant every time, the solution is stirred for 1h, then heated to 90-120 ℃ and kept for at least 24h, then heated to 130-150 ℃ and kept for at least 6h, and stirring is kept during the period; the solution is then centrifuged, washed and dried, for example at 1000r/min, and the product obtained is charged with methanol and deionized waterWashing, and drying in a drying oven at 60 ℃; the obtained product is marked as in-situ xPd-Ce-BTC and is placed in a tube furnace, the temperature is raised to 500-800 ℃ under the atmosphere of air or nitrogen according to the heating rate of 2 ℃/min, and the product is roasted for 3 h; finally obtaining the catalyst. According to different roasting atmospheres and temperatures, the catalyst is recorded as xPd-Ce-BTC-A500, xPd-Ce-BTC-A800, xPd-Ce-BTC-N500 and xPd-Ce-BTC-N800, the number in the catalyst represents the final roasting temperature, A represents air, N represents nitrogen, and x represents the mass ratio of Pd to Ce and is 0.5-1.2%.
The molar ratio of the cerium nitrate to the trimesic acid is preferably 10 (6-7).
CO is selected as a probe molecule to perform related catalyst evaluation, and the composition of CO gas distribution is 1 vol% CO +20 vol% O2+79vol％N2The space velocity was taken as 100,000mL/(g h). The catalytic performance of the four catalysts with Ce-BTC as the carrier is superior to that of bulk CeO2A supported catalyst; in addition, the catalytic performance of the sample treated by nitrogen is better than that of the sample treated by air, and the catalytic performance of the sample subjected to in-situ reduction by the one-bath method is also better than that of the two-step supported catalyst treated by the same atmosphere. In consideration of the actual CO elimination environment of automobile exhaust and the like, the CO catalytic oxidation activity of the Pd-Ce-BTC series catalyst prepared by the in-situ reduction one-bath method with the most excellent performance after high-temperature treatment is further researched. Although the catalyst after calcination at a high temperature of 800 ℃ for 3 hours showed a decrease in activity, it was heat-treated with CeO under the same conditions2Compared with the supported catalyst, the supported catalyst still has good CO oxidation catalytic activity, and the rule that the activity of a nitrogen treatment sample is superior to that of an air treatment sample is not changed.
The material of the invention has novel preparation method, simple preparation process, controllable process, high specific surface area and narrow noble metal particle size distribution. The sample roasted by reducing nitrogen in situ by the one-bath method shows the best CO catalytic oxidation performance and has very strong practical application value.
Drawings
FIG. 1 is an XRD pattern of Pd-Ce-BTC and Ce-BTC.
FIG. 2 is an XRD pattern of Pd-Ce-BTC and Pd/Ce-BTC series catalysts.
Fig. 3 is a TEM image and a Pd particle size distribution diagram of the prepared catalyst. Wherein panels (a, b, c)0.93Pd-Ce-BTC-N500 and (e, f, g)0.96Pd/Ce-BTC-N500 are TEM images; panel (d)0.93Pd-Ce-BTC-N500 and panel (h)0.96Pd/Ce-BTC-N500 are Pd particle size distribution plots.
Fig. 4 shows nitrogen adsorption-desorption curves (internal BET specific surface area) and pore size distribution curves of the catalysts prepared in the corresponding examples and comparative examples.
Fig. 5 is a graph showing the temperature dependence of the conversion of CO oxidation catalyzed by the catalysts prepared in the corresponding examples and comparative examples.
FIG. 6 is a graph showing the temperature dependence of the conversion rate of CO oxidation catalyzed by samples calcined at different temperatures according to the corresponding examples and comparative examples.
Detailed Description
The present invention will be further illustrated by the following examples, but the present invention is not limited to the following examples.
Comparative example 1: Ce-BTC was synthesized according to the usual method. 60mL of dimethylformamide was added to the vessel, 10mmol of cerium nitrate was added thereto and stirred to disperse uniformly, 6.67mmol of trimesic acid was added thereto and stirred for 1 hour. After the vessel was sealed, it was heated and held at 100 ℃ for 24h while maintaining stirring. And then centrifuging the solution at the rotating speed of 10,000r/min, fully washing the obtained product with methanol and deionized water, and drying in a drying oven at the temperature of 60 ℃ to obtain the Ce-BTC.
Example 1: in-situ reduction one-bath method is adopted to prepare in-situ xPd-CeO2A catalyst. In general, 60mL of dimethylformamide was placed in a vessel, followed by the addition of 10mmol of cerium nitrate, 6.67mmol of trimesic acid and the appropriate amount of PdCl in that order2Solution (corresponding to Pd loading) was kept well dispersed before adding new reactants. The solution was stirred for 1h, heated to 100 ℃ and held for 24h, then raised to 140 ℃ and held for 6h, while stirring was maintained. Then the solution is centrifuged at the rotating speed of 1000r/min, the obtained product is fully washed by methanol and deionized water and dried in a drying box at the temperature of 60 ℃. The obtained product is marked as in-situ xPd-Ce-BTC, and is divided into two groups which are respectively placed in a tube furnace, respectively heated to 500/800 ℃ under the atmosphere of air and nitrogen at the heating rate of 2 ℃/min, and roasted for 3 h. Most preferablyThe finally obtained catalysts are recorded as xPd-Ce-BTC-A500, xPd-Ce-BTC-A800, xPd-Ce-BTC-N500 and xPd-Ce-BTC-N800 according to different roasting atmospheres and temperatures. According to the test results of ICP, the actual Pd loading of the catalyst is 0.97 wt%, 1.02 wt%, 0.53 wt% and 0.83 wt% in sequence, and the mass ratio (x) of Pd to Ce is 1.01%, 1.02%, 0.93% and 0.95% in sequence.
Comparative example 2: yPd/CeO synthesis by common stepwise synthesis strategy2Catalyst as a control. After Ce-BTC was synthesized according to the method of example 1, it was uniformly dispersed in 60mL dimethylformamide, and then appropriate amount of PdCl was added2Solution (corresponding to Pd loading). The solution was heated to 140 ℃ and held for 6h while maintaining stirring. Then the solution is centrifuged at the rotating speed of 1000r/min, the obtained product is fully washed by methanol and deionized water, and is dried in a drying oven at the temperature of 60 ℃. The obtained product is recorded as yPd/Ce-BTC, and is divided into two groups which are respectively placed in a tube furnace, and are respectively roasted to 500/800 ℃ under the atmosphere of air and nitrogen according to the heating rate of 2 ℃/min and are kept for 3 hours. The finally obtained catalysts are recorded as yPd/Ce-BTC-A500, yPd/Ce-BTC-A800, yPd/Ce-BTC-N500 and yPd/Ce-BTC-N800 according to different roasting atmospheres and temperatures. According to the results of the ICP test, the actual Pd loading of the catalyst was 0.95 wt%, 0.98 wt%, 0.57 wt%, 0.87 wt% in this order, and the mass ratio (y) of Pd to Ce was 0.96%, 0.98%, 0.97%, 0.96% in this order.
Comparative example 3: in addition, CeO in bulk phase is prepared2Pd/CeO as carrier2The catalyst was used as a control and is designated as Pd/CeO2A500, the supporting method is the same as above, and the heat treatment condition is roasting in air at 500 ℃.
Claims (6)
1. In-situ reduction one-bath method for preparing Ce-BTC derived CeO by efficiently catalyzing and oxidizing CO2The method for supporting the Pd nano-catalyst is characterized by comprising the following steps of:
in-situ reduction one-bath method is adopted to prepare in-situ xPd-CeO2The catalyst, usually dimethylformamide, is added to a vessel, followed by the sequential addition of cerium nitrate, trimesic acid and PdCl2Solutions, added each timeBefore adding a new reactant, ensuring that the solution is uniformly dispersed, stirring the solution for 1h, heating to 90-120 ℃, keeping the temperature for at least 24h, then heating to 130-150 ℃, keeping the temperature for at least 6h, and keeping stirring; then centrifuging, washing and drying the solution, recording the obtained product as in-situ xPd-Ce-BTC, placing the in-situ xPd-Ce-BTC in a tube furnace, raising the temperature to 800 ℃ at the heating rate of 2 ℃/min in the air or nitrogen atmosphere, and roasting for 3 h; finally obtaining the catalyst.
2. The in-situ reduction one-bath method for preparing Ce-BTC derived CeO by efficiently catalyzing and oxidizing CO according to claim 12The method for loading the Pd nano-catalyst is characterized by comprising the following steps of centrifuging, washing and drying: centrifuging at 1000r/min, washing the obtained product with methanol and deionized water, and drying in a drying oven at 60 deg.C.
3. The in-situ reduction one-bath method for preparing Ce-BTC derived CeO by efficiently catalyzing and oxidizing CO according to claim 12The method for loading the Pd nano-catalyst is characterized in that the mass ratio of Pd to Ce is 0.5-1.2%.
4. The in-situ reduction one-bath method for preparing Ce-BTC derived CeO by efficiently catalyzing and oxidizing CO according to claim 12The method for loading the Pd nano-catalyst is characterized in that the molar ratio of cerium nitrate to trimesic acid is 10 (6-7).
5. Ce-BTC derived CeO prepared according to any one of claims 1 to 42And loading the Pd nano-catalyst.
6. Ce-BTC derived CeO prepared according to any one of claims 1 to 42The application of the supported Pd nano-catalyst is used for the catalytic oxidation of CO.
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| CN114345332A (en) * | 2021-12-02 | 2022-04-15 | 济南大学寿光产业技术研究院 | Bimetallic composite rod-like nano catalyst and application thereof in C-H bond oxidation reaction |
| CN115845843A (en) * | 2022-12-02 | 2023-03-28 | 桂林理工大学 | VOCs (volatile organic compounds) low-temperature oxidation catalyst with highly dispersed Pd component on cerium-zirconium-carbon porous composite carrier and preparation method thereof |
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