CN110327934B - Porous Cu-Ce-OxSolid solution catalyst, preparation method and application thereof - Google Patents
Porous Cu-Ce-OxSolid solution catalyst, preparation method and application thereof Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 239000006104 solid solution Substances 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 19
- 239000002243 precursor Substances 0.000 claims abstract description 19
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 11
- RVGRUAULSDPKGF-UHFFFAOYSA-N Poloxamer Chemical compound C1CO1.CC1CO1 RVGRUAULSDPKGF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229960000502 poloxamer Drugs 0.000 claims abstract description 7
- 229920001983 poloxamer Polymers 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000001354 calcination Methods 0.000 claims abstract description 5
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium nitrate Inorganic materials [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000007921 spray Substances 0.000 claims abstract description 5
- 238000005979 thermal decomposition reaction Methods 0.000 claims abstract description 5
- 230000003197 catalytic effect Effects 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 7
- 230000003647 oxidation Effects 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
- 229910002492 Ce(NO3)3·6H2O Inorganic materials 0.000 claims description 2
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- 238000000889 atomisation Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- 238000003764 ultrasonic spray pyrolysis Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 description 5
- 229910002091 carbon monoxide Inorganic materials 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 230000010718 Oxidation Activity Effects 0.000 description 2
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 description 2
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000851 scanning transmission electron micrograph Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/62—Carbon oxides
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
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Abstract
The invention discloses a porous Cu-Ce-OxA solid solution catalyst, a preparation method and application thereof, wherein the preparation method comprises the following steps: adding Cu (NO)3)2·3H2O、Ce(NO3)3·6H2Mixing O, poloxamer F127 and water to obtain a mixed solution A; carrying out ultrasonic spray thermal decomposition treatment on the mixed solution A to obtain precursor powder; calcining the precursor powder at high temperature, and then treating the calcined precursor powder with strong ammonia water to obtain the catalyst; solves the problems of poor thermal stability, large grain size, low specific surface area, limited exposure of active sites and low activity of the traditional Cu-based oxide catalyst.
Description
Technical Field
The invention relates to the field of catalysts, in particular to porous Cu-Ce-OxSolid solution catalyst, preparation method and application thereof.
Background
The low-temperature oxidation of CO is an important component of processes such as automobile exhaust control and hydrogen purification of Proton Exchange Membrane Fuel Cells (PEMFCs). For example, a "150 ℃ challenge" requires the treatment of CO, NO in automobile exhaust at 150 ℃xAnd the conversion of the pollutants reaches 90 percent. For another example, the hydrogen source of PEMFCs is industrial hydrogen, and the trace amount of CO contained therein can cause poisoning of the stack catalyst, so it is necessary to completely remove H at a low operating temperature of 80-120 ℃ for PEMFCs2Trace CO in the fuel. At present, the catalyst for low-temperature catalytic oxidation of CO is mainly noble metal components such as Pt, Pd, Au and the like loaded by metal oxides. However, there areLimited crustal reserves and high prices make noble metals difficult to meet for large-scale commercial applications, and therefore, there is a need to develop catalysts for low-temperature oxidation of CO with relatively high crustal reserves.
In recent years, Cu-based oxide catalysts have been found to have CO low temperature catalytic oxidation activity. Currently, Cu-based oxide catalysts are predominantly Cu2O, CuO and simple complexes thereof with other oxides. These catalysts have a common feature that the active components are Cu oxides (Cu)2O or CuO), but, since Cu2O and CuO have poor thermal stability, are easy to grow into crystal grains with the size of more than 20nm, and have the specific surface area of generally less than 100m2The activity is not high due to the limited exposure of active sites per gram.
Disclosure of Invention
The invention aims to provide porous Cu-Ce-OxThe solid solution catalyst, the preparation method and the application thereof solve the problems of poor thermal stability, large grain size, low specific surface area, limited exposure of active sites and low activity of the traditional Cu-based oxide catalyst.
In order to achieve the above object, the present invention provides a porous Cu-Ce-OxA method for preparing a solid solution catalyst, the method comprising:
(1) adding Cu (NO)3)2·3H2O、Ce(NO3)3·6H2Mixing O, poloxamer F127 and water to obtain a mixed solution A;
(2) carrying out ultrasonic spray thermal decomposition treatment on the mixed solution A to obtain precursor powder;
(3) and calcining the precursor powder at high temperature, and treating with strong ammonia water to obtain the catalyst.
The invention also provides porous Cu-Ce-OxSolid solution catalyst, said porous Cu-Ce-OxThe solid solution catalyst is prepared by the preparation method.
The invention also provides the porous Cu-Ce-OxThe application of solid solution catalyst in CO low-temperature catalytic oxidation.
The invention provides a porous Cu-Ce-OxThe solid solution catalyst and the preparation method and the application thereof, wherein the preparation method comprises the following steps: adding Cu (NO)3)2·3H2O、Ce(NO3)3·6H2Mixing O, poloxamer F127 and water to obtain a mixed solution A; carrying out ultrasonic spray thermal decomposition treatment on the mixed solution A to obtain precursor powder; calcining the precursor powder at high temperature, and then treating the calcined precursor powder with strong ammonia water to obtain the catalyst; porous Cu-Ce-O of the inventionxCu and Ce elements in the solid solution catalyst are uniformly distributed, and independent CuO and CeO are not contained2Crystalline phase, specific surface area up to 150m2More than 196 m/g, the maximum2The catalyst belongs to the same type and is highest at present; the catalyst phase has extremely high CO low-temperature catalytic oxidation activity, and has 1 percent of CO and 1 percent of O2+ 98% He reaction system with Cu0.2-Ce0.8-OxAnd Cu0.3-Ce0.7-OxThe representative catalysts can achieve 100% conversion of CO at temperatures below 80 ℃; meanwhile, the catalyst has extremely high sintering resistance, and the catalytic activity of the catalyst is hardly influenced by high-temperature treatment at 600 ℃. The preparation method is simple and feasible, and the proportion of the Cu element and the Ce element is continuously adjustable.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 shows the porous Cu-Ce-O obtained in examples 1 and 2xSolid solution catalyst and pure CeO2And a plot comparing the X-ray diffraction patterns of CuO;
FIG. 2 shows the porous Cu-Ce-O obtained in example 1xHigh (a), low (b) transmission electron micrographs of solid solution catalysts;
FIG. 3 shows the porous Cu-Ce-O obtained in example 2xScanning transmission electron micrographs of the solid solution catalyst;
FIG. 4 shows the porous Cu-Ce-O obtained in examples 1 and 2xSolid solution catalyst for 1% CO + 1% O2The catalytic performance curve of the + 98% He reaction system;
FIG. 5 is a graph of catalytic performance of the porous Cu-Ce-Ox solid solution catalyst obtained in example 1 after high temperature treatment at 400 ℃ and 600 ℃ for a reaction system of 1% CO + 1% O2+ 98% He.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are given by way of illustration and explanation only, not limitation.
The invention provides a porous Cu-Ce-OxA method for preparing a solid solution catalyst, the method comprising:
(1) adding Cu (NO)3)2·3H2O、Ce(NO3)3·6H2Mixing O, poloxamer F127 and water to obtain a mixed solution A;
(2) carrying out ultrasonic spray thermal decomposition treatment on the mixed solution A to obtain precursor powder;
(3) and calcining the precursor powder at high temperature, and treating with strong ammonia water to obtain the catalyst.
In a preferred embodiment of the invention, Cu (NO) is used in order to obtain a catalyst with smaller particle unit size and higher specific surface area and improved thermal stability and catalytic activity3)2·3H2O、Ce(NO3)3·6H2O, poloxamer F127 and water in a mass ratio of 0.03-1.3: 7: 2.5: 200 are mixed.
In a preferred embodiment of the present invention, in order to make the prepared catalyst have smaller particle unit size and higher specific surface area, and improve the thermal stability and catalytic activity thereof, the step of ultrasonic spray pyrolysis comprises: carrying out ultrasonic atomization on the mixed solution A, and then introducing the mixed solution A into a tube furnace for heating to obtain precursor powder;
wherein the heating conditions include: the temperature is 500 ℃ and 700 ℃, and the time is 3-5 s.
In a preferred embodiment of the present invention, in order to make the particle unit size of the prepared catalyst smaller and the specific surface area higher, and to improve the thermal stability and catalytic activity thereof, the conditions of high-temperature calcination include: the temperature is 300 ℃ and 800 ℃, and the time is 1-4 h.
In a preferred embodiment of the present invention, in order to make the prepared catalyst have smaller particle unit size and higher specific surface area, and improve the thermal stability and catalytic activity thereof, the concentrated ammonia water treatment step comprises: and (3) immersing the precursor powder calcined at high temperature into strong ammonia water at 45-55 ℃ for 55-65min, and centrifugally drying to obtain the catalyst.
In a preferred embodiment of the present invention, in order to make the prepared catalyst smaller in unit size of fine particles, higher in specific surface area, and improved in thermal stability and catalytic activity, the amount of concentrated ammonia water is 8 to 12mL per 1g of precursor powder.
The invention also provides porous Cu-Ce-OxSolid solution catalyst, said porous Cu-Ce-OxThe solid solution catalyst is prepared by the preparation method.
Prepared porous Cu-Ce-OxThe solid solution catalyst is a solid solution crystal phase and has a porous structure, the particle unit size of the solid solution catalyst is 0.2-2.5 mu m, and the specific surface area is more than 150m2(ii) in terms of/g. The Cu and Ce elements of the catalyst are uniformly distributed, and independent CuO and CeO are not contained2A crystalline phase; wherein the molar ratio of Cu to Ce is 0.01-0.4: 1.
the invention also provides the porous Cu-Ce-OxThe application of solid solution catalyst in CO low-temperature catalytic oxidation.
The following description will be made by specific examples.
Example 1
Adding Cu (NO)3)2·3H2O、Ce(NO3)3·6H2O, poloxamer F127 and water in a mass ratio of 1: 7: 2.5: 200 to obtain a mixed solution A; carrying out ultrasonic atomization on the mixed solution A, and then introducing the mixed solution A into a tubular furnace for heating (the temperature is 600 ℃, and the time is 4s) to obtain precursor powder; calcining the precursor powder at high temperature (400 ℃ for 2h), and then passing through strong ammonia waterTreating (soaking in 50 ℃ strong ammonia water for 60min) to obtain the catalyst; the amount of concentrated aqueous ammonia used was 10mL per 1g of precursor powder.
Example 2
Adding Cu (NO)3)2·3H2O、Ce(NO3)3·6H2O, poloxamer F127 and water according to the mass ratio of 3: 7: 2.5: 200 to obtain a mixed solution A; carrying out ultrasonic atomization on the mixed solution A, and then introducing the mixed solution A into a tubular furnace for heating (the temperature is 600 ℃ and the time is 4s) to obtain precursor powder; calcining the precursor powder at high temperature (the temperature is 400 ℃ and the time is 2 hours), and then treating the calcined precursor powder by using strong ammonia water (soaking the calcined precursor powder in strong ammonia water at 50 ℃ for 60 minutes) to obtain the catalyst; the amount of concentrated aqueous ammonia used was 10mL per 1g of precursor powder.
Example 3
Adding Cu (NO)3)2·3H2O、Ce(NO3)3·6H2O, poloxamer F127 and water in a mass ratio of 1: 7: 2.5: 200 to obtain a mixed solution A; carrying out ultrasonic atomization on the mixed solution A, and then introducing the mixed solution A into a tubular furnace for heating (the temperature is 600 ℃ and the time is 4s) to obtain precursor powder; calcining the precursor powder at high temperature (the temperature is 600 ℃ and the time is 2 hours), and then treating the calcined precursor powder by using strong ammonia water (soaking the calcined precursor powder in strong ammonia water at 50 ℃ for 60 minutes) to obtain the catalyst; the amount of concentrated aqueous ammonia used was 10mL per 1g of precursor powder.
Example 4
Adding Cu (NO)3)2·3H2O、Ce(NO3)3·6H2O, poloxamer F127 and water according to the mass ratio of 0.2: 7: 2.5: 200 to obtain a mixed solution A; carrying out ultrasonic atomization on the mixed solution A, and then introducing the mixed solution A into a tubular furnace for heating (the temperature is 700 ℃ and the time is 4s) to obtain precursor powder; calcining the precursor powder at high temperature (400 ℃ for 2h), and then treating the calcined precursor powder with strong ammonia water (soaking the calcined precursor powder in strong ammonia water at 50 ℃ for 60min) to obtain the catalyst; the amount of concentrated aqueous ammonia used was 10mL per 1g of precursor powder.
FIG. 1 shows porous Cu-Ce-O obtained in examples 1 and 2 of the present inventionxSolid solution catalyst and pure CeO2And a plot comparing the X-ray diffraction patterns of CuO; FIG. 2 shows the porous Cu-Ce-O obtained in example 1xHigh (a), low (b) transmission electron micrographs of solid solution catalysts; FIG. 3 shows the porous Cu-Ce-O obtained in example 2xScanning transmission electron micrographs of the solid solution catalyst; the particle unit size of the prepared catalyst is 0.2-2.5 mu m; FIG. 4 shows the porous Cu-Ce-O obtained in examples 1 and 2xSolid solution catalyst for 1% CO + 1% O2The catalytic performance curve of the + 98% He reaction system; FIG. 5 is a graph of catalytic performance of the porous Cu-Ce-Ox solid solution catalyst obtained in example 1 after high temperature treatment at 400 and 600 ℃ for the reaction system of 1% CO + 1% O2+ 98% He; the catalyst has extremely high sintering resistance, and the catalytic activity of the catalyst is hardly influenced by high-temperature treatment at 600 ℃; with Cu0.2-Ce0.8-OxAnd Cu0.3-Ce0.7-OxRepresentative catalysts can achieve 100% conversion of CO at temperatures below 80 ℃.
The preferred embodiments of the present invention have been described in detail with reference to the accompanying drawings, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (5)
1. Porous Cu-Ce-OxA method for producing a solid solution catalyst, characterized in that the production method comprises:
(1) adding Cu (NO)3)2·3H2O、Ce(NO3)3·6H2Mixing O, poloxamer F127 and water to obtain a mixed solution A;
(2) carrying out ultrasonic spray thermal decomposition treatment on the mixed solution A to obtain precursor powder;
(3) calcining the precursor powder at high temperature, and then treating the calcined precursor powder with strong ammonia water to obtain the catalyst;
wherein Cu (NO)3)2·3H2O、Ce(NO3)3·6H2O, poloxamer F127 and water in a mass ratio of 0.03-1.3: 7: 2.5: 200, mixing;
the ultrasonic spray pyrolysis method comprises the following steps: carrying out ultrasonic atomization on the mixed solution A, and then introducing the mixed solution A into a tube furnace for heating to obtain precursor powder;
wherein the heating conditions include: the temperature is 600-700 ℃, and the time is 3-5 s;
the conditions of the high-temperature calcination include: the temperature is 400 ℃ and 600 ℃, and the time is 1-4 h;
the concentrated ammonia water treatment method comprises the following steps: immersing the precursor powder calcined at high temperature into strong ammonia water at 45-55 ℃ for 55-65min, and centrifugally drying to obtain the catalyst;
the amount of concentrated ammonia water used was 8-12mL per 1g of precursor powder.
2. Porous Cu-Ce-OxA solid solution catalyst, characterized in that said porous Cu-Ce-OxThe solid solution catalyst is produced by the production method according to claim 1.
3. Porous Cu-Ce-O according to claim 2xA solid solution catalyst, wherein the porous Cu-Ce-OxThe solid solution catalyst is a solid solution crystal phase and has a porous structure, the particle unit size of the solid solution catalyst is 0.2-2.5 mu m, and the specific surface area is more than 150m2/g。
4. Porous Cu-Ce-O according to claim 2xThe solid solution catalyst comprises Cu and Ce at a molar ratio of 0.01-0.4: 1.
5. the porous Cu-Ce-O of claims 2-4xThe application of solid solution catalyst in CO low-temperature catalytic oxidation.
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