CN115282974A - Catalyst for catalyzing oxidation of carbon monoxide - Google Patents
Catalyst for catalyzing oxidation of carbon monoxide Download PDFInfo
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- CN115282974A CN115282974A CN202111509254.2A CN202111509254A CN115282974A CN 115282974 A CN115282974 A CN 115282974A CN 202111509254 A CN202111509254 A CN 202111509254A CN 115282974 A CN115282974 A CN 115282974A
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- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 229910002091 carbon monoxide Inorganic materials 0.000 title claims abstract description 79
- 239000003054 catalyst Substances 0.000 title claims abstract description 73
- 238000007254 oxidation reaction Methods 0.000 title claims description 45
- 230000003647 oxidation Effects 0.000 title claims description 44
- 239000002135 nanosheet Substances 0.000 claims abstract description 103
- UMWXOUAFWWUNGR-UHFFFAOYSA-N aluminum cobalt(2+) oxygen(2-) Chemical class [Co+2].[O-2].[Al+3] UMWXOUAFWWUNGR-UHFFFAOYSA-N 0.000 claims abstract description 96
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 11
- 229910052720 vanadium Inorganic materials 0.000 claims abstract description 6
- 229910052738 indium Inorganic materials 0.000 claims description 12
- 239000011148 porous material Substances 0.000 claims description 6
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical group [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 13
- 238000006243 chemical reaction Methods 0.000 description 69
- 230000000052 comparative effect Effects 0.000 description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 24
- LTXHKPDRHPMBKA-UHFFFAOYSA-N dialuminum;cobalt(2+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Al+3].[Al+3].[Co+2] LTXHKPDRHPMBKA-UHFFFAOYSA-N 0.000 description 18
- 230000003197 catalytic effect Effects 0.000 description 15
- 239000000463 material Substances 0.000 description 15
- 238000000034 method Methods 0.000 description 14
- 239000013078 crystal Substances 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 12
- 239000002184 metal Substances 0.000 description 12
- 238000002474 experimental method Methods 0.000 description 11
- 239000002243 precursor Substances 0.000 description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 229910017052 cobalt Inorganic materials 0.000 description 8
- 239000010941 cobalt Substances 0.000 description 8
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 8
- 230000009849 deactivation Effects 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- -1 cobalt-aluminum oxide modified cobalt-aluminum oxide Chemical class 0.000 description 7
- 229910052782 aluminium Inorganic materials 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000003513 alkali Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 229910052596 spinel Inorganic materials 0.000 description 5
- 239000011029 spinel Substances 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 238000009835 boiling Methods 0.000 description 4
- 238000010304 firing Methods 0.000 description 4
- 229910001701 hydrotalcite Inorganic materials 0.000 description 4
- 229960001545 hydrotalcite Drugs 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 230000010718 Oxidation Activity Effects 0.000 description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 239000004202 carbamide Substances 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002055 nanoplate Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 230000009257 reactivity Effects 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 230000032683 aging Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 1
- BLJNPOIVYYWHMA-UHFFFAOYSA-N alumane;cobalt Chemical class [AlH3].[Co] BLJNPOIVYYWHMA-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J23/83—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 with rare earths or actinides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- 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
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/864—Removing carbon monoxide or hydrocarbons
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
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- B01J23/825—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 with gallium, indium or thallium
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- 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
- B01J23/84—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 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/847—Vanadium, niobium or tantalum or polonium
- B01J23/8472—Vanadium
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Abstract
The embodiment of the application provides a catalyst for catalyzing carbon monoxide to oxidize, which comprises modified cobalt aluminum oxide nanosheets, wherein the chemical formula of the modified cobalt aluminum oxide nanosheets is Co x‑a M a AlO z M is selected from at least one of La, in and V, x and a satisfy formula 1:
wherein the value range of k is 0.1-0.9, and x is more than or equal to 2 and less than or equal to 6.The modified cobalt aluminum oxide nanosheet provided by the embodiment of the application has waterproof performance, and the activity of catalyzing carbon monoxide to oxidize by the modified cobalt aluminum oxide nanosheet in a high-humidity environment is enhanced.
Description
Technical Field
The invention belongs to the technical field of catalysts, and particularly relates to a catalyst for catalyzing carbon monoxide to oxidize.
Background
Carbon monoxide is a toxic gas to the human body. The carbon monoxide catalytic oxidation process has higher use value in the aspects of eliminating environmental pollution, purifying air, reducing the toxicity of automobile emissions and the like. The catalyst for low-temperature CO catalytic oxidation mainly comprises a noble metal catalyst and a non-noble metal catalyst. The metal oxide catalyst (such as cobalt oxide) is cheap, and has a better development prospect in the actual application of catalyzing carbon monoxide oxidation.
Generally, cobalt-containing oxide catalysts are easily deactivated in a high-humidity environment, so that the conversion rate of carbon monoxide in a catalytic reaction is reduced, and the effect of catalyzing the conversion of carbon monoxide is poor.
Therefore, there is a need for new catalysts for catalyzing the oxidation of carbon monoxide.
Disclosure of Invention
The embodiment of the application provides a catalyst for catalyzing carbon monoxide oxidation, which comprises modified cobalt aluminum oxide nanosheets, wherein the chemical formula of the modified cobalt aluminum oxide nanosheets is Co x-a M a AlO z M is selected from at least one of La, in and V, x and a satisfy formula 1:
wherein the value range of k is 0.1-0.9, and x is more than or equal to 2 and less than or equal to 6.
In the catalyst for catalyzing carbon monoxide oxidation provided by the first aspect of the embodiment of the present application, co and M in the modified cobalt aluminum oxide nanosheet both provide a catalytic active site for a carbon monoxide catalytic oxidation reaction, and M is doped in the cobalt aluminum oxide to form the modified cobalt aluminum oxide nanosheet, so that a lattice local of an original cobalt aluminum oxide spinel structure has a "spreading" phenomenon, and a positive distortion is generated. The crystal lattice of the original cobalt aluminum oxide spinel structure is locally propped open, the combination of water molecules in a humid environment and reaction active sites for catalyzing carbon monoxide oxidation in the modified cobalt aluminum oxide nanosheets is inhibited, the waterproof performance of the modified cobalt aluminum oxide nanosheets is further improved, and the reaction activity of the modified cobalt aluminum oxide nanosheets for catalyzing carbon monoxide oxidation in the high-humidity environment is enhanced.
In one possible embodiment of the present application, M is La or In, and k has a value ranging from 0.2 to 0.6.
In one possible embodiment of the present application, k has a value in the range of 0.3 to 0.5.
In one possible embodiment of the present application, M includes La and In, and k has a value ranging from 0.2 to 0.8.
In one possible embodiment of the present application, in the modified cobalt aluminum oxide nanosheet, the molar ratio m of La to In ranges from 1 to 10.
In one possible embodiment of the present application, the thickness of the modified cobalt aluminum oxide nanosheet ranges from 10nm to 25nm.
In one possible embodiment of the present application, the modified cobalt aluminum oxide nanosheet has mesopores, and the pore size of the mesopores ranges from 3nm to 50nm.
In one possible embodiment of the present application, the pore size of the mesopores ranges from 3nm to 5nm.
In one possible embodiment of the present application, the value of x in the modified cobalt aluminum oxide nanosheet ranges from 2.5 to 4.5.
In one possible embodiment of the present application, the modified cobalt aluminum oxide nanosheets have a layered hydrotalcite structure.
Drawings
Other features, objects and advantages of the invention will become apparent from the following detailed description of non-limiting embodiments thereof, when read in conjunction with the accompanying drawings, in which like reference characters designate the same or similar parts throughout the figures thereof, and which are not to scale.
FIG. 1 is a graph showing the conversion of carbon monoxide by oxidation under 10% relative humidity conditions in the catalysts of example 1 and comparative example 1 of the present application as a function of reaction temperature;
FIG. 2 is a graph showing the conversion of carbon monoxide to oxidation catalyzed by the catalysts of example 1 and comparative example 1 of the present application at 50% relative humidity as a function of reaction temperature;
FIG. 3 is a graph showing the conversion of carbon monoxide by oxidation catalyzed by the catalysts of example 1 and comparative example 1 of the present application at 90% relative humidity as a function of reaction temperature;
FIG. 4 is a graphical representation of the conversion of carbon monoxide over catalyst catalyzed oxidation with reaction temperature for different relative humidities as a function of the present application in example 1;
FIG. 5 is a graph showing the conversion of carbon monoxide to oxidation catalyzed by the catalysts of example 2 and comparative example 1 of the present application at 10% relative humidity as a function of reaction temperature;
FIG. 6 is a graph showing the conversion of carbon monoxide to oxidation catalyzed by the catalysts of example 2 and comparative example 1 of the present application at 50% relative humidity as a function of reaction temperature;
FIG. 7 is a graphical representation of the conversion of carbon monoxide to carbon monoxide catalyzed oxidation at 90% relative humidity for the catalysts of example 2 and comparative example 1 of the present application as a function of reaction temperature;
FIG. 8 is a graphical representation of the conversion of carbon monoxide to oxidation over the catalyst as a function of reaction temperature at various relative humidities as used in example 2 herein;
FIG. 9 is a graphical representation of the conversion of catalytic carbon monoxide oxidation over 10% relative humidity with reaction temperature for the catalysts of comparative example 1 and example 3 of the present application;
FIG. 10 is a graphical representation of the conversion of catalytic carbon monoxide oxidation as a function of reaction temperature for the catalysts of comparative example 1, example 4, and example 5 of the present application at 10% relative humidity;
FIG. 11 is a graphical representation of the conversion of the catalytic carbon monoxide oxidation over 10% relative humidity for the catalysts of comparative example 1, example 1 and example 6 of the present application as a function of reaction temperature;
fig. 12 is a graphical representation of the conversion of the catalytic carbon monoxide oxidation over 10% rh for the catalysts of comparative example 1, and example 7 of the present application as a function of reaction temperature.
Detailed Description
Features and exemplary embodiments of various aspects of the present invention will be described in detail below, and in order to make objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not to be construed as limiting the invention. It will be apparent to one skilled in the art that the present invention may be practiced without some of these specific details. The following description of the embodiments is merely intended to provide a better understanding of the present invention by illustrating examples of the present invention.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrases "comprising 8230; \8230;" 8230; "does not exclude the presence of additional like elements in a process, method, article, or apparatus that comprises the element.
The "ranges" disclosed herein are defined in terms of lower limits and upper limits, with a given range being defined by a selection of one lower limit and one upper limit that define the boundaries of the particular range. Ranges defined in this manner may or may not include endpoints and may be arbitrarily combined, i.e., any lower limit may be combined with any upper limit to form a range. For example, if ranges of 60-120 and 80-110 are listed for a particular parameter, it is understood that ranges of 60-110 and 80-120 are also contemplated. Furthermore, if the minimum range values 1 and 2 are listed, and if the maximum range values 3,4, and 5 are listed, the following ranges are all contemplated: 1-3, 1-4, 1-5, 2-3, 2-4 and 2-5. In this application, unless otherwise stated, the numerical range "a-b" represents a shorthand representation of any combination of real numbers between a and b, where a and b are both real numbers. For example, a numerical range of "0 to 5" indicates that all real numbers between "0 to 5" have been listed herein, and "0 to 5" is simply an abbreviated representation of the combination of these numbers. In addition, when a parameter is an integer of 2 or more, it is equivalent to disclose that the parameter is, for example, an integer of 2, 3,4, 5, 6, 7, 8, 9, 10, 11, 12, or the like.
All embodiments and alternative embodiments of the present application may be combined with each other to form new solutions, if not specifically stated.
All technical and optional features of the present application may be combined with each other to form new solutions, if not specifically mentioned.
All steps of the present application may be performed sequentially or randomly, preferably sequentially, if not specifically stated. For example, the method comprises steps (a) and (b), meaning that the method may comprise steps (a) and (b) performed sequentially, and may also comprise steps (b) and (a) performed sequentially. For example, reference to the process further comprising step (c) means that step (c) may be added to the process in any order, for example, the process may comprise steps (a), (b) and (c), may also comprise steps (a), (c) and (b), may also comprise steps (c), (a) and (b), etc.
The terms "comprises" and "comprising" as used herein mean either open or closed unless otherwise specified. For example, the terms "comprising" and "comprises" may mean that additional components not listed may also be included or included, or that only listed components may be included or included.
In this application, the term "or" is inclusive, if not otherwise specified. For example, the phrase "a or B" means "a, B, or both a and B. More specifically, any one of the following conditions satisfies the condition "a or B": a is true (or present) and B is false (or not present); a is false (or not present) and B is true (or present); or both a and B are true (or present).
The inventor finds that the common cobalt aluminum oxide is prepared by long-term intensive researchThe nanosheets have two (110) crystal planes opposite to each other in the thickness direction of the nanosheets. (110) More Co is exposed on the crystal face 3+ The active site, and therefore the (110) crystal plane, is a crystal plane having catalytic carbon monoxide oxidation activity. However, through the intensive research of the inventor, the size matching degree of the (110) crystal face of the cobalt-aluminum oxide nanosheet and water molecules is high, and the Co on the (110) crystal face is high 3+ The active sites are easy to combine with water molecules in the environment, so that the active sites available for catalyzing carbon monoxide oxidation in the cobalt aluminum oxide nanosheets are reduced, and the cobalt aluminum oxide nanosheets are volatile under a high humidity environment.
The present application has been made in view of research and analysis of the above technical problems.
The embodiment of the application provides a catalyst for catalyzing carbon monoxide oxidation, which comprises modified cobalt aluminum oxide nanosheets, wherein the chemical formula of the modified cobalt aluminum oxide nanosheets is Co x-a M a AlO z M is selected from at least one of La, in and V, x and a satisfy formula 1:
wherein the value range of k is 0.1-0.9, and x is more than or equal to 2 and less than or equal to 6.
k represents a ratio of the amount of the M substance to the sum of the amount of the M substance and the amount of the Co substance.
x is the amount of Al species relative to the sum of the amount of M species and the amount of Co species.
The modified cobalt-aluminum oxide nanosheet provided by the embodiment of the application is doped with a metal element M for enhancing catalytic activity. The modified cobalt-aluminum oxide nanosheet doped with the metal element M still has spinel type (AB) 2 O 4 ) And (5) structure. The metal element M replaces part of aluminum in the crystal structure of the modified cobalt-aluminum oxide nanosheet, and the atomic number of the metal element M is greater than that of aluminum (Al), so that after the metal element M is doped into the cobalt-aluminum oxide modified cobalt-aluminum oxide nanosheet, the crystal lattice of the original cobalt-aluminum oxide spinel structure locally has a 'propping' phenomenon, and orthodontic treatment is generatedAnd (6) changing. After the crystal lattice of the original cobalt-aluminum oxide spinel structure is locally propped open, the combination of water molecules in a humid environment and reaction active sites for catalyzing carbon monoxide oxidation in the modified cobalt-aluminum oxide nanosheets is inhibited, so that the modified cobalt-aluminum oxide nanosheets have waterproof performance, and the activity of catalyzing carbon monoxide oxidation by the modified cobalt-aluminum oxide nanosheets in the high-humidity environment is enhanced.
In some optional embodiments, M is La or In, and k has a value ranging from 0.2 to 0.6.
In some optional embodiments, k has a value in the range of 0.3 to 0.5.
In some optional embodiments, M includes La and In, and k has a value ranging from 0.2 to 0.8. In the embodiments, the cobalt aluminum oxide nanosheet is modified by doping La and In at the same time, and the activity of the modified cobalt aluminum oxide nanosheet for catalyzing oxidation of carbon monoxide In a high humidity environment is further increased through the synergistic effect of La and In, so that the catalytic life of the modified cobalt aluminum oxide nanosheet is increased.
In some optional embodiments, in the modified cobalt aluminum oxide nanosheets, the molar amount of La to In, m, ranges from 1 to 10. In these examples, the modified cobalt aluminum oxide has superior catalytic carbon monoxide oxidation activity in a relatively humid environment.
In some optional embodiments, the thickness of the modified cobalt aluminum oxide nanosheet ranges from 10nm to 25nm.
In the embodiments, the thickness of the modified cobalt-aluminum oxide nanosheet is within a range of 10nm to 25nm, which is beneficial to keeping the modified cobalt-aluminum oxide nanosheet in a sheet structure in long-term use. When the thickness of the modified cobalt aluminum oxide nanosheet is less than 10nm, the modified cobalt aluminum oxide nanosheet is easy to collapse in structure in the use process and does not have a flaky structure any more, so that the number of active sites for catalyzing carbon monoxide to be oxidized by the modified cobalt aluminum oxide is reduced. When the thickness of the modified cobalt aluminum oxide nanosheet is higher than 25nm, the area proportion of the (110) crystal face area with the activity of catalyzing carbon monoxide to be oxidized in the modified cobalt aluminum oxide nanosheet is reduced, and the total area of the (110) crystal face in the unit mass of the modified cobalt aluminum oxide nanosheet is reduced, so that the activity of catalyzing carbon monoxide to be oxidized by the modified cobalt aluminum oxide is reduced.
In some optional embodiments, the modified cobalt aluminum oxide nanosheet has mesopores, and the pore diameter of the mesopores ranges from 3nm to 50nm. In the embodiments, the modified cobalt aluminum oxide nanosheet has a mesoporous structure, so that the specific surface area of the modified cobalt aluminum oxide nanosheet is increased, the carbon monoxide and oxygen adsorption capacity of the modified cobalt aluminum oxide is improved, and the activity of the modified cobalt aluminum oxide in catalyzing the carbon monoxide for oxidation is further increased.
In one possible embodiment of the present application, the pore size of the mesopores ranges from 3nm to 5nm.
In one possible embodiment of the present application, the value of x in the modified cobalt aluminum oxide nanosheet ranges from 2.5 to 4.5.
In one possible embodiment of the present application, the modified cobalt aluminum oxide nanosheets have a layered hydrotalcite structure.
In another aspect, the present application provides a method for preparing a modified cobalt aluminum oxide nanosheet, including:
adding a cobalt source material, an aluminum source material and a doped metal source material into a solution containing urea according to a preset proportion, and uniformly mixing to form a precursor mixed solution, wherein the doped metal M In the doped metal source material is selected from at least one of La, in and V. The preset proportion enables the ratio of the amount of Co, M and Al in the precursor mixture to satisfy Co: M: al = x-a: x:1, x and a satisfy the formula 1:
wherein the value range of k is 0.1-0.9, and x is more than or equal to 2 and less than or equal to 6.
Heating the precursor mixed liquid to a boiling state to ensure that the precursor mixed liquid is in a first preset time t 1 The mixture was kept boiling to obtain a pink suspension. In some embodiments, the first preset duration t 1 Is in the range of 0.5 to 1 hour.
Step (c), at a first preset temperature T 1 Stirring the pink turbid liquid for a second preset time t 2 Cooling the pink suspension to room temperature after stirring is finished, and aging the pink suspension for a second preset time t at the room temperature 3 Filtering, washing the filter residue, and drying the filter residue to obtain the hydrotalcite compound containing Co, M and Al. In some embodiments, the first preset temperature T 1 The value range is 100-110 ℃. A second preset duration t 2 Is in the range of 8 hours to 14 hours.
And (d) roasting the hydrotalcite compound containing Co, M and Al to obtain the modified cobalt-aluminum oxide nanosheet. In some embodiments, the firing is performed in an air atmosphere for a time period of 3 hours to 5 hours at a firing temperature of 400 ℃ to 450 ℃.
Step (f), carrying out alkali treatment on the modified cobalt aluminum oxide nanosheet obtained in the step (d) to obtain a modified cobalt aluminum oxide sodium nanosheet with a mesoporous, wherein the chemical formula of the modified cobalt aluminum oxide nanosheet is Co x-a M a AlO z . In some embodiments, the modified cobalt aluminum oxide nanoplates obtained in step (d) are subjected to an alkaline treatment with an alkaline solution of sodium hydroxide.
Examples
The present disclosure is more particularly described in the following examples that are intended as illustrative only, since various modifications and changes within the scope of the present disclosure will be apparent to those skilled in the art. Unless otherwise indicated, all parts, percentages, and ratios reported in the following examples are on a weight basis, and all reagents used in the examples are commercially available or synthesized according to conventional methods and can be used directly without further treatment, and the equipment used in the examples is commercially available.
x-a a z 1. Preparation method of modified cobalt-aluminum oxide nanosheet CoMAlO
Adding a cobalt source material, an aluminum source material and a doped metal source material into a solution containing urea according to a preset proportion, and uniformly mixing to form a precursor mixed solution. The doping metal M In the doping metal source material is at least one selected from La, in and V. The preset proportion enables the ratio of the amount of Co, M and Al in the precursor mixture to satisfy Co: M: al = x-a: x:1, x and a satisfy the formula 1:
wherein the value range of k is 0.1-0.9, and x is more than or equal to 2 and less than or equal to 6.
The cobalt source material is Co (NO) 3 ) 2 ·6H 2 O, al (NO) as the aluminum source material 3 ) 3 ·9H 2 And O. The doped metal source material is selected from La (NO) 3 ) 3 ，In(NO 3 ) 3 And NH 4 VO 3 (ammonium metavanadate).
And (b) carrying out oil bath heating on the precursor mixed solution at 105 ℃, heating the precursor mixed solution to a boiling state, and keeping the precursor mixed solution in the boiling state within 0.5 hour to obtain pink turbid liquid.
And (c) stirring the pink suspension for 8 hours at 105 ℃, cooling the pink suspension to room temperature after stirring is finished, aging overnight at room temperature, filtering, washing filter residues, and drying the filter residues to obtain the hydrotalcite compound containing Co, M and Al.
And (d) roasting the hydrotalcite compound containing Co, M and Al to obtain the modified cobalt-aluminum oxide nanosheet. In some examples, firing was carried out under an air atmosphere for 4 hours at a firing temperature of 400 ℃.
Step (f), carrying out alkali treatment on the modified cobalt aluminum oxide nanosheets obtained in the step (d) to obtain modified cobalt aluminum oxide sodium nanosheets with mesopores, wherein the chemical formula of the modified cobalt aluminum oxide nanosheets is Co x-a M a AlO z . In this specific example, the modified cobalt aluminum obtained in step (d) was oxidized with 3mol/L NaOH aqueous solutionAnd (d) carrying out alkali treatment on the nano-material sheets, wherein 1g of the modified cobalt aluminum oxide nano-material sheets obtained in the step (d) are subjected to alkali treatment for 20 hours at 80 ℃ by adopting 50ml of the NaOH aqueous solution. And after the alkali treatment is finished, washing the modified cobalt-aluminum oxide nanosheets with a large amount of water to finally obtain the modified cobalt-aluminum oxide nanosheets with mesopores.
2、 x z Preparation method of cobalt-aluminum oxide nanosheet CoAlO in comparative example
Adding a cobalt source material and an aluminum source material into a solution containing urea according to a preset proportion, and uniformly mixing to form a precursor mixed solution. The preset proportion enables the quantity ratio of the Co and the Al in the precursor mixture to satisfy Co: al = x:1, wherein x satisfies 2 ≤ x ≤ 6.
The cobalt source material is Co (NO) 3 ) 2 ·6H 2 O, al source material is Al (NO 3) 3 ·9H 2 O。
Cobalt aluminum oxide nanosheet Co in comparative example x AlO z The subsequent steps of the preparation method and the modified cobalt aluminum oxide nanosheet Co x-a M a AlO z The steps (b) to (f) in the preparation method are the same, and are not described again here.
3. Table 1 shows the chemical formula of the modified cobalt aluminum oxide nanosheets in each example, the chemical formula of the cobalt aluminum oxide nanosheets in the comparative example, and the relevant ratio parameters. Modified cobalt aluminum oxide nanosheets of examples in Table 1 the modified cobalt aluminum oxide nanosheets Co described above were used x-a M a AlO z The modified cobalt aluminum oxide nanosheet in the comparative example in the table 1 is prepared by adopting the cobalt aluminum oxide nanosheet Co in the comparative example x AlO z The preparation method is used for preparing the compound.
TABLE 1
4. The modified cobalt aluminum oxide nanosheets in the examples and the cobalt aluminum oxide nanosheets in the comparative examples were subjected to a water resistance test, respectively
Test method
In a humid environment, the modified cobalt aluminum oxide nanosheets in the examples and the cobalt aluminum oxide nanosheets in the comparative examples are used as catalysts to catalyze the conversion of carbon monoxide, and the water resistance of the catalysts is evaluated according to the conversion rates of the carbon monoxide at different humidities and temperatures, wherein the specific test method comprises the following steps:
(1) Either 200mg of the catalyst comprising modified cobalt aluminum oxide nanoplates in the example, or 200mg of the catalyst comprising cobalt aluminum oxide nanoplates in the comparative example, were weighed.
(2) At 20% of O 2 The catalyst was pretreated for 1 hour at 300 ℃ under a/He atmosphere.
(3) Introducing mixed gas (the volume fraction of each component in the mixed gas is 1% CO +19% 2 +80% He) to perform the catalytic carbon monoxide conversion experiment, the mixed gas flow rate was 100ml/min, and the reaction space velocity was 30,000ml/gcat/hr.
The preset humidity conditions are expressed in terms of relative humidity of 30 ℃. For example, a water saturation vapor pressure at 30 ℃ of 4.246kpa, a relative humidity of 10% means that the partial pressure of water in the reaction atmosphere is 0.4246kPa, and the normal pressure is 101kPa, wherein the water content is 0.4246/101=0.42%.
It should be noted that, when the reaction temperature is higher than 30 ℃, the water content in the environment is maintained at the water content level when the temperature is 30 ℃; when the reaction temperature is lower than 30 ℃, the reaction atmosphere is substantially saturated with water.
(4) And setting a plurality of groups of experiments under different humidity conditions, wherein each group of experiments detect the conversion rate of the same catalyst for catalyzing the conversion of carbon monoxide under the same humidity condition and at different reaction temperatures.
5. Results and analysis of the experiments
(1) The results of the tests of the first set of comparative experiments, including comparative example 1 and example 1, are shown in fig. 1 to 4. As shown in fig. 1, the comparative example 1 and the example 1 are easily inactivated at a moderate reaction temperature (herein, the moderate reaction temperature is defined as between-18 c and 180 c) such that the conversion rate of carbon monoxide (CO) in the carbon monoxide conversion reaction is decreased. As shown in fig. 1 to 3, the catalyst in example 1 has a narrower deactivation temperature range at the same relative humidity as the catalyst in comparative example 1, demonstrating that the water resistance of the catalyst in example 1 is superior to that of the catalyst in comparative example 1. The modified cobalt-aluminum oxide nanosheets are doped with cobalt (Co) to inhibit combination of water molecules in a humid environment and reactive sites in the modified cobalt-aluminum oxide nanosheets for catalyzing carbon monoxide oxidation, so that the waterproof performance of the modified cobalt-aluminum oxide nanosheets is improved, and the reactive activity of the modified cobalt-aluminum oxide nanosheets for catalyzing carbon monoxide oxidation in a high-humidity environment is enhanced.
As shown in fig. 4, the lower the relative humidity, the narrower the catalyst deactivation temperature range, and the stronger the reactivity of the catalyst in example 1 for catalyzing the oxidation of carbon monoxide.
(2) The results of the second set of comparative experiments are shown in fig. 5-8, the first set of comparative experiments including comparative example 1 and example 2. As shown in fig. 1, the comparative example 1 and the example 2 are easily inactivated at a moderate reaction temperature (herein, the moderate reaction temperature is defined as between-18 c and 180 c) such that the conversion rate of carbon monoxide (CO) in the carbon monoxide conversion reaction is decreased. As shown in fig. 5 to 7, the catalyst in example 2 has a narrower deactivation temperature range at the same relative humidity as that of the catalyst in comparative example 1, demonstrating that the water resistance of the catalyst in example 2 is superior to that of the catalyst in comparative example 1. The modified cobalt aluminum oxide nanosheet is doped with indium (In) to inhibit combination of water molecules In a humid environment and reactive sites In the modified cobalt aluminum oxide nanosheet for catalyzing carbon monoxide oxidation, so that the waterproof performance of the modified cobalt aluminum oxide nanosheet is improved, and the reactive activity of the modified cobalt aluminum oxide nanosheet for catalyzing carbon monoxide oxidation In a high-humidity environment is enhanced.
As shown in fig. 8, the lower the relative humidity, the narrower the range of catalyst deactivation temperature, and the stronger the reactivity of the catalyst in example 2 for catalyzing the oxidation of carbon monoxide.
(3) The results of the third set of comparative experiments, including comparative example 1 and example 3, are shown in fig. 9. As shown in fig. 9, the comparative example 1 and the example 3 are easily inactivated at a moderate reaction temperature (herein, the moderate reaction temperature is defined as between-18 c and 180 c) such that the conversion rate of carbon monoxide (CO) in the carbon monoxide conversion reaction is decreased. The catalyst in example 3 has a narrower deactivation temperature range at the same relative humidity as the catalyst in comparative example 1, demonstrating that the water resistance of the catalyst in example 3 is better than that of the catalyst in comparative example 1. Vanadium (V) doped in the modified cobalt aluminum oxide nanosheet inhibits the combination of water molecules in a humid environment and reactive sites in the modified cobalt aluminum oxide nanosheet for catalyzing the oxidation of carbon monoxide, so that the waterproof performance of the modified cobalt aluminum oxide nanosheet is improved, and the reactivity of the modified cobalt aluminum oxide nanosheet for catalyzing the oxidation of carbon monoxide in a high-humidity environment is enhanced.
(4) The results of the fourth set of comparative experiments, including comparative example 1, example 4, and example 5, are shown in fig. 10. As shown in fig. 10, the conversion of the catalysts of comparative example 1, example 4 and example 5 to catalyze the oxidative conversion of carbon monoxide at different reaction temperatures was examined at 10% relative humidity.
Example 1, example 4 and example 5 generally have higher conversions at moderate reaction temperatures (where moderate reaction temperatures are defined as between-18 ℃ to 180 ℃) than comparative example 1. And when K is equal to 0.1, the doping amount of M in the modified cobalt-aluminum oxide nanosheet is small, and the optimization degree of the water resistance of the catalyst is low. When K is equal to 0.9, the doping amount of M in the modified cobalt aluminum oxide nanosheets is likely to be large, and the active site density of cobalt in the modified cobalt aluminum oxide nanosheets is reduced. Example 1 (K equal to 0.5) provides modified cobalt aluminum oxide nanosheets with a narrower deactivation temperature range and superior catalytic carbon monoxide oxidation activity as compared to examples 4 and 5.
And is easily deactivated to reduce the conversion rate of carbon monoxide (CO) in the carbon monoxide conversion reaction. The catalyst in example 3 has a narrower deactivation temperature range at the same relative humidity as the catalyst in comparative example 1, demonstrating that the water resistance of the catalyst in example 3 is better than that of the catalyst in comparative example 1. Vanadium (V) doped in the modified cobalt-aluminum oxide nanosheets inhibits water molecules in a humid environment from being combined with reactive sites in the modified cobalt-aluminum oxide nanosheets for catalyzing carbon monoxide oxidation, so that the waterproof performance of the modified cobalt-aluminum oxide nanosheets is improved, and the reactive activity of the modified cobalt-aluminum oxide nanosheets for catalyzing carbon monoxide oxidation in a high-humidity environment is enhanced.
(5) The results of the fifth set of comparative experiments, including comparative example 1, and example 6, are shown in fig. 11. As shown in fig. 11, the catalysts of comparative example 1, example 1 and example 6 were tested for conversion to catalyze the oxidation of carbon monoxide at different reaction temperatures at 10% relative humidity.
Example 1 and example 6 generally have higher conversions at moderate reaction temperatures (defined herein as between-18 ℃ to 180 ℃) than comparative example 1. In addition, the water resistance of the catalyst was optimized only by doping La In example 1, and the catalyst was modified by doping both La and In example 6. The catalyst in example 6 has a narrower deactivation temperature range than the catalyst in example 1, and the lowest conversion in example 6 is higher than that in example 1, and the catalyst in example 6 has a more significant improvement in water resistance than that in example 1, and is more favorable for catalyzing carbon monoxide oxidation at high humidity. Example 6 the cobalt aluminum oxide is modified by doping La and In simultaneously, and the activity of the modified cobalt aluminum oxide nanosheet for catalyzing oxidation of carbon monoxide In a high humidity environment is further increased by the synergistic effect of La and In, so that the catalytic life of the modified cobalt aluminum oxide nanosheet is increased.
(6) The results of the sixth comparative experiment, including comparative example 1, and example 7, are shown in fig. 12. Fig. 12 shows that the catalysts of comparative example 1, example 1 and example 7 were tested for conversion to carbon monoxide oxidation at different reaction temperatures at 10% relative humidity.
Example 1, as well as example 7, generally had higher conversion at moderate reaction temperatures (defined herein as between-18 ℃ to 180 ℃) than comparative example 1. In addition, the conversion rate of the catalyst provided in example 7 for oxidizing carbon monoxide in the medium reaction temperature range is slightly lower than that of the catalyst provided in example 1 for oxidizing carbon monoxide in the medium reaction temperature range, which indicates that the value of x in the modified cobalt-aluminum oxide nanosheet is near 2.5, which can further improve the waterproof performance of the modified cobalt-aluminum oxide nanosheet and enhance the reaction activity of the modified cobalt-aluminum oxide nanosheet for catalyzing oxidation of carbon monoxide in a high humidity environment.
In accordance with the above-described embodiments of the present invention, these embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention and various embodiments with various modifications as are suited to the particular use contemplated. The invention is limited only by the claims and their full scope and equivalents.
Claims (9)
1. A catalyst for catalyzing the oxidation of carbon monoxide, wherein the catalyst comprises modified cobalt aluminum oxide nanosheets having the chemical formula Co x-a M a AlO z M is selected from at least one of La, in and V, and x and a satisfy formula 1:
wherein the value range of k is 0.1-0.9, and x is more than or equal to 2 and less than or equal to 6.
2. The catalyst according to claim 1, wherein M is La or In, and k has a value ranging from 0.2 to 0.6.
3. The catalyst of claim 2, wherein k has a value in the range of 0.3 to 0.5.
4. The catalyst of claim 1, wherein M comprises La and In, and k has a value ranging from 0.2 to 0.8.
5. The catalyst according to claim 4, wherein m, the molar weight ratio of La to In the modified cobalt-aluminum oxide nanosheet, ranges from 1 to 10.
6. The catalyst of claim 1, wherein the thickness of the modified cobalt aluminum oxide nanosheet ranges from 10nm to 25nm.
7. The catalyst according to claim 1, wherein the modified cobalt aluminum oxide nanosheet has mesopores with a pore size ranging from 3nm to 50nm;
preferably, the pore diameter of the mesopores ranges from 3nm to 5nm.
8. The catalyst of any one of claims 1 to 7, wherein the value of x in the modified cobalt aluminum oxide nanosheets ranges from 2.5 to 4.5.
9. The catalyst of claim 8, wherein the modified cobalt aluminum oxide nanosheets have a layered hydrotalcite structure.
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