CN110893343A - Preparation method of ternary oxide non-noble metal catalyst - Google Patents
Preparation method of ternary oxide non-noble metal catalyst Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 49
- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000010453 quartz Substances 0.000 claims abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229920001353 Dextrin Polymers 0.000 claims abstract description 10
- 239000004375 Dextrin Substances 0.000 claims abstract description 10
- 230000003197 catalytic effect Effects 0.000 claims abstract description 10
- 235000019425 dextrin Nutrition 0.000 claims abstract description 10
- 238000000197 pyrolysis Methods 0.000 claims abstract description 9
- 239000000654 additive Substances 0.000 claims abstract description 7
- 230000000996 additive effect Effects 0.000 claims abstract description 6
- 239000000047 product Substances 0.000 claims description 23
- 239000004005 microsphere Substances 0.000 claims description 22
- 238000006243 chemical reaction Methods 0.000 claims description 15
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 14
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 14
- 229910021645 metal ion Inorganic materials 0.000 claims description 13
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 7
- 238000003764 ultrasonic spray pyrolysis Methods 0.000 claims description 7
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt(II) nitrate Inorganic materials [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- 230000009471 action Effects 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000005118 spray pyrolysis Methods 0.000 claims description 2
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 abstract description 5
- 239000010970 precious metal Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 239000002912 waste gas Substances 0.000 abstract description 3
- 239000012159 carrier gas Substances 0.000 abstract description 2
- 238000007084 catalytic combustion reaction Methods 0.000 abstract description 2
- 239000008367 deionised water Substances 0.000 abstract description 2
- 229910021641 deionized water Inorganic materials 0.000 abstract description 2
- 239000007921 spray Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000003981 vehicle Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01D53/46—Removing components of defined structure
- B01D53/62—Carbon oxides
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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
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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Abstract
The invention relates to the technical field of waste gas treatment materials, in particular to a preparation method of a ternary oxide non-noble metal catalyst, which is characterized in that Cu (NO3)3, Co (NO3)2 and Ce (NO3)3 are selected as precursors, dextrin is selected as an additive, and the precursors are dissolved in 100mL of deionized water to form a spray solution with a specific concentration. The method has the advantages that fog drops are formed in the ultrasonic atomizer, the fog drops are carried into the high-temperature quartz tube furnace by carrier gas, products after precursor pyrolysis are collected by filter paper, the problems that platinum group precious metals are high in cost, poor in high temperature resistance, low in low-temperature catalytic efficiency and the like in the prior art are solved, and the method can be used as a substitute of a precious metal catalyst in catalytic combustion application, and is low in cost and high in stability.
Description
Technical Field
The invention relates to the technical field of waste gas treatment materials, in particular to a preparation method of a ternary oxide non-noble metal catalyst.
Background
In order to reduce greenhouse gas emissions and oil consumption, new fuel economy standards for passenger vehicles and light trucks have been proposed by countries throughout the world, and the combination of improving fuel economy while reducing exhaust gas pollutant emissions to meet these standards poses a significant challenge to the automotive industry.
Most commercial catalysts employed in automotive exhaust gas streams use supported noble metals of the platinum group, and the presence of hydrocarbons inhibits the active sites of the noble metals of the platinum group, limiting their use in low temperature catalysis. Meanwhile, the platinum group noble metal catalyst is easy to sinter at high temperature, which also causes the reduction of the conversion rate of key pollutants at low temperature. These key disadvantages and the high cost of precious metal materials have driven the need to develop low cost, high stability catalysts that can meet the requirements of complex exhaust gas streams.
Disclosure of Invention
The invention aims to provide a preparation method of a ternary oxide non-noble metal catalyst with low cost and high stability, which can meet the requirement of complex waste gas flow.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a preparation method of a ternary oxide non-noble metal catalyst, which comprises the step of preparing CuO-Co with a hollow structure through an ultrasonic spray pyrolysis process3O4-CeO2The ternary oxide catalyst microsphere comprises the following steps:
1) mixing three metal salts of Cu, Co and Ce to form a precursor, mixing the precursor with an additive, and dissolving the precursor with a solvent to prepare a precursor solution;
2) spraying the precursor solution by the ultrasonic spraying action of a spray pyrolysis device to obtain fog drops, and feeding the fog drops into a quartz tube furnace;
3) the precursor solution is dried in a quartz tube furnace and then undergoes a thermal decomposition reaction, thereby obtaining a product CuO-Co3O4-CeO2Three-way catalyst microspheres, at which point the product was collected through filter paper.
Product CuO-Co3O4-CeO2The particle size of the three-way catalyst microsphere is 0.4-3 microns, and the three-way catalyst microsphere has a typical hollow structure.
Preferably, the final product is represented by xCuO-yCo3O4-zCeO2Wherein x is the mole fraction of Cu to the total metal ions, y is the mole fraction of Co to the total metal ions, and z is the mole fraction of Ce to the total metal ions; the regulation interval of x is 0.1-0.5, the regulation interval of y is 0.1-0.5, and the regulation interval of z is 0.2-0.8.
Preferably, the metal salt raw material of the precursor is Cu (NO)3)3、Co(NO3)2And Ce (NO)3)3。
Preferably, the additive is dextrin.
Preferably, the total concentration of the metal ions in the precursor solution is 0.1-0.5mol/L, and the addition amount of the dextrin is 0.05-0.2 mol/L.
Preferably, the pyrolysis temperature in the quartz tube furnace is 400-1000 ℃.
Preferably, the prepared ternary non-noble metal catalyst is compared with binary CuO-Co3O4The catalytic performance is greatly improved, and the catalyst is free of C3H8Complete conversion of carbon monoxide is achieved at 130 ℃ and C3H8Complete conversion of carbon monoxide was achieved at 150 ℃ in the presence of this.
Compared with the prior art, the invention has the beneficial effects that: according to the preparation method of the ternary oxide non-noble metal catalyst, Cu (NO3)3, Co (NO3)2 and Ce (NO3)3 are selected as precursors, dextrin is selected as an additive, and the precursors and the additives are dissolved in 100mL of deionized water to form a spray solution with a specific concentration. The method has the advantages that fog drops are formed in the ultrasonic atomizer, the fog drops are carried into the high-temperature quartz tube furnace by carrier gas, products after precursor pyrolysis are collected by filter paper, the problems that platinum group precious metals are high in cost, poor in high temperature resistance, low in low-temperature catalytic efficiency and the like in the prior art are solved, and the method can be used as a substitute of a precious metal catalyst in catalytic combustion application, and is low in cost and high in stability.
Drawings
FIG. 1 is an X-ray diffraction pattern of various products prepared in examples 1-4 and comparative example 1;
FIG. 2(a) is a photograph of the product prepared in example 1 at a resolution of 2 μm under a scanning electron microscope;
FIG. 2(b) is a photograph of the product prepared in example 1 under a scanning electron microscope at a resolution of 500 nm;
FIG. 3(a) is a photograph of the product prepared in example 1 under a transmission electron microscope at a resolution of 500 nm;
FIG. 3(b) is a photograph of the product prepared in example 1 at a resolution of 5 nm under a transmission electron microscope;
FIG. 4(a) is a drawing at C3H8Graphs of catalytic performance of the products prepared in examples 1-4 and comparative example 1 in the absence;
FIG. 4(b) is a drawing at C3H8Graphs of the catalytic performance of the products prepared in examples 1-4 and comparative example 1 in the presence of the catalyst;
in the figure, xCuO-yCo3O4-zCeO2Abbreviated CCC-xyz.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Preparation of CuO-Co with hollow structure by ultrasonic spray pyrolysis process3O4-CeO2Ternary oxide catalyst microsphere, Cu (NO) is selected3)3、Co(NO3)2And Ce (NO)3)3As a precursor, the total concentration of metal ions is 0.2mol/L, the addition amount of dextrin is 0.05mol/L, and xCuO-yCo3O4-zCeO2Wherein x, y, z is 1, 1 and 8. The pyrolysis temperature in the quartz tube furnace is 400 ℃, the particle size of the product three-way catalyst microsphere is 0.8 micron (shown in figure 2), and the product three-way catalyst microsphere has a typical hollow structure (shown in figure 3). As shown in attached figures 1 and 4, the prepared ternary non-noble metal catalyst is compared with binary CuO-Co3O4The catalytic performance is greatly improved, and the catalyst is free of C3H8Complete conversion of carbon monoxide is achieved at 135 ℃ and C3H8Complete conversion of carbon monoxide was achieved at 160 ℃ in the presence of this.
Example 2
Preparation of CuO-Co with hollow structure by ultrasonic spray pyrolysis process3O4-CeO2Ternary oxide catalyst microsphere, Cu (NO) is selected3)3、Co(NO3)2And Ce (NO)3)3As a precursor, the total concentration of metal ions is 0.5mol/L, the addition amount of dextrin is 0.2mol/L, and xCuO-yCo3O4-zCeO2Wherein x, y, z is 2, 2 and 6. The pyrolysis temperature in a quartz tube furnace is 800 ℃, the particle size of the product three-way catalyst microsphere is 2 microns, and the product three-way catalyst microsphere has a typical hollow structure. As shown in attached figures 1 and 4, the prepared ternary non-noble metal catalyst is compared with binary CuO-Co3O4The catalytic performance is greatly improved, and the catalyst is free of C3H8Complete conversion of carbon monoxide is achieved at 130 ℃ and C3H8Complete conversion of carbon monoxide was achieved at 150 ℃ in the presence of this.
Example 3
Preparation of CuO-Co with hollow structure by ultrasonic spray pyrolysis process3O4-CeO2Ternary oxide catalyst microsphere, Cu (NO) is selected3)3、Co(NO3)2And Ce (NO)3)3As a precursor, the total concentration of metal ions is 0.3mol/L, the addition amount of dextrin is 0.1mol/L, and xCuO-yCo3O4-zCeO2Wherein x, y, z is 3, 3 and 4. The pyrolysis temperature in a quartz tube furnace is 600 ℃, the particle size of the product three-way catalyst microsphere is 3 microns, and the product three-way catalyst microsphere has a typical hollow structure. As shown in attached figures 1 and 4, the prepared ternary non-noble metal catalyst is compared with binary CuO-Co3O4The catalytic performance is greatly improved, and the catalyst is free of C3H8Complete conversion of carbon monoxide is achieved at 135 ℃ and C3H8Complete conversion of carbon monoxide was achieved at 160 ℃ in the presence of this.
Example 4
Preparation of CuO-Co with hollow structure by ultrasonic spray pyrolysis process3O4-CeO2Ternary oxide catalyst microsphere, Cu (NO) is selected3)3、Co(NO3)2And Ce (NO)3)3As a precursor, the total concentration of metal ions is 0.3mol/L, the addition amount of dextrin is 0.1mol/L, and xCuO-yCo3O4-zCeO2Wherein x, y, z is 4:4: 2. The pyrolysis temperature in the quartz tube furnace is 1000 ℃, the particle size of the product three-way catalyst microsphere is 3 microns, and the product three-way catalyst microsphere has a typical hollow structure. As shown in attached figures 1 and 4, the prepared ternary non-noble metal catalyst is compared with binary CuO-Co3O4The catalytic performance is greatly improved, and the catalyst is free of C3H8Complete conversion of carbon monoxide is achieved at 150 ℃ and C3H8Complete conversion of carbon monoxide was achieved at 170 ℃ in the presence of this.
Comparative sample 1
Preparation of CuO-Co with hollow structure by ultrasonic spray pyrolysis process3O4Binary oxide catalyst microsphere, Cu (NO) is selected3)3And Co (NO)3)2The total concentration of metal ions is 0.3mol/L, and x, y and z in xCuO-yCo3O4 are 5: 5. Stone (stone)The pyrolysis temperature in the quartz tube furnace is 600 ℃, and the particle size of the product catalyst microsphere is a solid sphere of 3 microns. As shown in the attached FIG. 1 and FIG. 4, binary CuO-Co is prepared3O4Catalytic performance in the absence of C3H8At 240 ℃ complete conversion of carbon monoxide is not yet achieved, at C3H8Complete conversion of carbon monoxide in the presence of the catalyst at 240 ℃ has not been achieved.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. The preparation method of the ternary oxide non-noble metal catalyst is characterized by comprising the step of preparing CuO-Co with a hollow structure through an ultrasonic spray pyrolysis process3O4-CeO2The ternary oxide catalyst microsphere comprises the following steps:
1) mixing three metal salts of Cu, Co and Ce to form a precursor, mixing the precursor with an additive, and dissolving the precursor with a solvent to prepare a precursor solution;
2) spraying the precursor solution by the ultrasonic spraying action of a spray pyrolysis device to obtain fog drops, and feeding the fog drops into a quartz tube furnace;
3) the precursor solution is dried in a quartz tube furnace and then undergoes a thermal decomposition reaction, thereby obtaining a product CuO-Co3O4-CeO2Three-way catalyst microspheres, at which point the product was collected through filter paper.
Product CuO-Co3O4-CeO2The particle size of the three-way catalyst microsphere is 0.4-3 microns, and the three-way catalyst microsphere has a typical hollow structure.
2. The method of claim 1, wherein the method comprises the steps of: the final product is xCuO-yCo3O4-zCeO2Is shown in whichX is the mole fraction of Cu in the total metal ions, y is the mole fraction of Co in the total metal ions, and z is the mole fraction of Ce in the total metal ions; the regulation interval of x is 0.1-0.5, the regulation interval of y is 0.1-0.5, and the regulation interval of z is 0.2-0.8.
3. The method of claim 1, wherein the method comprises the steps of: the metal salt raw material of the precursor is Cu (NO)3)3、Co(NO3)2And Ce (NO)3)3。
4. The method of claim 1, wherein the method comprises the steps of: the additive is dextrin.
5. The method of claim 3, wherein the method comprises the steps of: in the precursor solution, the total concentration of metal ions is 0.1-0.5mol/L, and the addition amount of dextrin is 0.05-0.2 mol/L.
6. The method of claim 1, wherein the method comprises the steps of: the pyrolysis temperature in the quartz tube furnace is 400-1000 ℃.
7. The method of claim 1, wherein the method comprises the steps of: compared with binary CuO-Co, the prepared ternary non-noble metal catalyst3O4The catalytic performance is greatly improved, and the catalyst is free of C3H8Complete conversion of carbon monoxide is achieved at 130 ℃ and C3H8Complete conversion of carbon monoxide was achieved at 150 ℃ in the presence of this.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111085214A (en) * | 2019-12-31 | 2020-05-01 | 华东理工大学 | Cu-Co-Ce ternary metal oxide catalyst and preparation method and application thereof |
| CN114345333A (en) * | 2022-01-14 | 2022-04-15 | 济南大学 | Preparation method of automobile exhaust purification catalyst with controllable precious metal content and obtained product |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111085214A (en) * | 2019-12-31 | 2020-05-01 | 华东理工大学 | Cu-Co-Ce ternary metal oxide catalyst and preparation method and application thereof |
| CN114345333A (en) * | 2022-01-14 | 2022-04-15 | 济南大学 | Preparation method of automobile exhaust purification catalyst with controllable precious metal content and obtained product |
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