CN111547776A - Method for preparing inverse water gas ferric oxide catalyst by using copper oxide nanosheets - Google Patents
Method for preparing inverse water gas ferric oxide catalyst by using copper oxide nanosheets Download PDFInfo
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- CN111547776A CN111547776A CN202010362905.9A CN202010362905A CN111547776A CN 111547776 A CN111547776 A CN 111547776A CN 202010362905 A CN202010362905 A CN 202010362905A CN 111547776 A CN111547776 A CN 111547776A
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- copper oxide
- deionized water
- water gas
- copper
- oxide catalyst
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 40
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 239000005751 Copper oxide Substances 0.000 title claims abstract description 27
- 239000003054 catalyst Substances 0.000 title claims abstract description 27
- 229910000431 copper oxide Inorganic materials 0.000 title claims abstract description 27
- 239000002135 nanosheet Substances 0.000 title claims abstract description 26
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910001868 water Inorganic materials 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 13
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- 239000002244 precipitate Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 6
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 5
- 239000012692 Fe precursor Substances 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 229910001431 copper ion Inorganic materials 0.000 claims description 5
- 229910000336 copper(I) sulfate Inorganic materials 0.000 claims description 5
- WIVXEZIMDUGYRW-UHFFFAOYSA-L copper(i) sulfate Chemical compound [Cu+].[Cu+].[O-]S([O-])(=O)=O WIVXEZIMDUGYRW-UHFFFAOYSA-L 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 150000002500 ions Chemical class 0.000 claims description 5
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- XNCMOUSLNOHBKY-UHFFFAOYSA-H iron(3+);trisulfate;heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O XNCMOUSLNOHBKY-UHFFFAOYSA-H 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000003814 drug Substances 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000002055 nanoplate Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- -1 zinc aluminate Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- 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
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/40—Carbon monoxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a method for preparing a reverse water gas ferric oxide catalyst by using a copper oxide nanosheet, wherein a ferric oxide two-dimensional nanosheet (20 +/-3 nm) with uniform thickness is obtained, and raw material medicaments used for reverse water gas catalysis are safe and easily available, show higher catalytic reaction activity at a lower temperature of 300 ℃, and are CO2The conversion rate reaches over 73.4 percent, and the material has special value for reverse water gas reaction and water gas conversion reaction.
Description
Technical Field
The invention belongs to the field of chemical industry, and relates to a method for preparing a reverse water gas ferric oxide catalyst by using a copper oxide nanosheet.
Background
The Water Gas (WGS) shift reaction has been studied for nearly a century with a relatively mature process. The reverse water gas shift Reaction (RWGS) can utilize abundant and cheap carbon dioxide as a carbon source, utilize carbon monoxide generated by the RWGS reaction as an intermediate product, and adopt an F-T synthesis method to prepare olefin; ethanol can also be produced using RWGS. The CAMERE process, which is currently widely used for the production of methanol, wherein the RWGS reaction at high temperature is the key step, the higher the carbon monoxide conversion, the more beneficial the methanol synthesis. Therefore, a high stability catalyst is critical for the CAMERE reaction.
The traditional RWGS catalyst mainly comprises zinc aluminate catalyst and Pt/CeO2Catalysts, copper-based catalysts, manganese-based catalysts, and the like. Most of the catalysts contain noble metals, so the cost is high, and the catalysts are not suitable for large-scale industrial popularization. Therefore, in recent years, iron-based catalysts, the main component of which is iron oxide, have been developed in the industry as industrial catalysts for RWGS. At present, the iron oxide catalyst is mainly prepared by a precipitation method, and the method mainly comprises the steps of raw material dissolving and mixing, neutralization, hot boiling, washing, filtering, drying and roasting. Because RWGS is a heterogeneous reaction, catalysts are required to have a complex chemical composition and a specific physical structure. Different preparation methods are adopted, the chemical compositions of the catalysts are the same, but the physical structures of the catalysts are different, and the catalytic effect difference is larger. The iron oxide catalyst prepared by the precipitation method has the advantages of non-uniform particle size, low dispersity and poor catalytic effect.
Disclosure of Invention
In order to overcome the defects, the invention aims to provide a method for preparing a reverse water gas ferric oxide catalyst by using a copper oxide nanosheet.
In order to realize the purpose of the invention, the technical scheme adopted by the invention is as follows:
a method for preparing a reverse water gas ferric oxide catalyst by using a copper oxide nanosheet is characterized by comprising the following steps:
1) mixing copper oxide nanosheets with deionized water in a mass ratio of 1: 1000-1: 2000, stirring for 2-5h at the rotating speed of 30-60r/min to fully disperse the copper oxide nano-sheets in the deionized water;
2) heating the solution to 50-80 ℃, and adding ferric sulfate heptahydrate [ FeSO ] with the same mole number as that of the copper oxide nanosheet at the temperature and at the rotating speed of 30-60r/min4·7H2O]Completely dissolving the mixture in the solution;
3) after stirring for 2-5h, the following reaction takes place:
2FeSO4+2CuO+H2O→Cu2SO4+Fe2O3+H2SO4(ii) a Meanwhile, the color of the solution gradually changes from black to dark orange; then separating the precipitate by filtration and washing with excess deionized water to remove unreacted iron precursor ions;
4) in order to remove the copper oxide nano-sheets, washing the precipitate with excessive alkali liquor to take away the complex produced by copper ions; rinsing until the filtrate is no longer blue;
5) the remaining orange sample was rinsed with deionized water and finally vacuum dried and crushed to give the iron oxide catalyst.
The method can obtain the following beneficial effects: the obtained ferric oxide two-dimensional nano-sheet (20 +/-3 nm) with uniform thickness is safe and easily obtained, is used for reverse water gas catalysis, shows higher catalytic reaction activity at a lower temperature of 300 ℃, and contains CO2The conversion rate reaches over 73.4 percent, and the material has special value for reverse water gas reaction and water gas conversion reaction.
Detailed Description
The following description is given with reference to specific examples:
example 1
1. Mixing 800mg of copper oxide nano-sheets with 800ml of deionized water, and stirring for 2 hours at the rotating speed of 30r/min to fully disperse the copper oxide nano-sheets in the deionized water.
2. Heating the solution to 50 ℃, and adding ferric sulfate heptahydrate [ FeSO ] with the same mole number as that of the copper oxide nanosheet at the rotating speed of 30r/min at the temperature4·7H2O]So that it is completely dissolved in the solution.
3. After stirring for 2h, the following reaction occurred:
2FeSO4+2CuO+H2O→Cu2SO4+Fe2O3+H2SO4. At the same time, the color of the solution is changed from black to blackGradually turning dark orange. The precipitate was then separated by filtration and washed with excess deionized water to remove unreacted iron precursor ions.
4. To remove the copper oxide nanoplates, the precipitate is washed with excess lye, allowing the copper ion production complex to be carried away. Rinse until the filtrate was no longer blue.
5. The remaining orange sample was rinsed with deionized water and finally vacuum dried and crushed to give the iron oxide catalyst.
The average thickness of the material is 22nm, and CO is generated at 300 DEG C2The conversion rate reaches 74.1%.
Example 2
1. Mixing 500mg of copper oxide nano-sheets with 500ml of deionized water, and then stirring for 3 hours at a rotating speed of 50r/min to fully disperse the copper oxide nano-sheets in the deionized water.
2. Heating the solution to 60 ℃, and adding ferric sulfate heptahydrate [ FeSO ] with the same mole number as that of the copper oxide nanosheet at the rotating speed of 50r/min at the temperature4·7H2O]So that it is completely dissolved in the solution.
3. After stirring for 2h, the following reaction occurred:
2FeSO4+2CuO+H2O→Cu2SO4+Fe2O3+H2SO4. While the color of the solution gradually changed from black to dark orange. The precipitate was then separated by filtration and washed with excess deionized water to remove unreacted iron precursor ions.
4. To remove the copper oxide nanoplates, the precipitate is washed with excess lye, allowing the copper ion production complex to be carried away. Rinse until the filtrate was no longer blue.
5. The remaining orange sample was rinsed with deionized water and finally vacuum dried and crushed to give the iron oxide catalyst.
The average thickness of the material is 20nm, and CO is generated at 300 DEG C2The conversion rate reaches 74.4%.
Example 3
1. 1200mg of copper oxide nanosheets are mixed with 1200ml of deionized water, and then stirred for 5 hours at the rotating speed of 60r/min, so that the copper oxide nanosheets are fully dispersed in the deionized water.
2. Heating the solution to 80 ℃, and adding iron sulfate heptahydrate [ FeSO ] with the same mole number as that of the copper oxide nanosheet at the rotating speed of 60r/min at the temperature4·7H2O]So that it is completely dissolved in the solution.
3. After stirring for 2h, the following reaction occurred:
2FeSO4+2CuO+H2O→Cu2SO4+Fe2O3+H2SO4. While the color of the solution gradually changed from black to dark orange. The precipitate was then separated by filtration and washed with excess deionized water to remove unreacted iron precursor ions.
4. To remove the copper oxide nanoplates, the precipitate is washed with excess lye, allowing the copper ion production complex to be carried away. Rinse until the filtrate was no longer blue.
5. The remaining orange sample was rinsed with deionized water and finally vacuum dried and crushed to give the iron oxide catalyst.
The average thickness of the material is 18nm, and CO is generated at 300 DEG C2The conversion rate reaches 75.2 percent.
Claims (1)
1. A method for preparing a reverse water gas ferric oxide catalyst by using a copper oxide nanosheet is characterized by comprising the following steps:
1) mixing copper oxide nanosheets with deionized water in a mass ratio of 1: 1000-1: 2000, stirring for 2-5h at the rotating speed of 30-60r/min to fully disperse the copper oxide nano-sheets in the deionized water;
2) heating the solution to 50-80 ℃, and adding ferric sulfate heptahydrate [ FeSO ] with the same mole number as that of the copper oxide nanosheet at the temperature and at the rotating speed of 30-60r/min4·7H2O]Completely dissolving the mixture in the solution;
3) after stirring for 2-5h, the following reaction takes place:
2FeSO4+2CuO+H2O→Cu2SO4+Fe2O3+H2SO4(ii) a Simultaneous color of solutionGradually changing from black to dark orange; then separating the precipitate by filtration and washing with excess deionized water to remove unreacted iron precursor ions;
4) in order to remove the copper oxide nano-sheets, washing the precipitate with excessive alkali liquor to take away the complex produced by copper ions; rinsing until the filtrate is no longer blue;
5) the remaining orange sample was rinsed with deionized water and finally vacuum dried and crushed to give the iron oxide catalyst.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010362905.9A CN111547776A (en) | 2020-04-30 | 2020-04-30 | Method for preparing inverse water gas ferric oxide catalyst by using copper oxide nanosheets |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010362905.9A CN111547776A (en) | 2020-04-30 | 2020-04-30 | Method for preparing inverse water gas ferric oxide catalyst by using copper oxide nanosheets |
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| CN202010362905.9A Pending CN111547776A (en) | 2020-04-30 | 2020-04-30 | Method for preparing inverse water gas ferric oxide catalyst by using copper oxide nanosheets |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090152500A1 (en) * | 2007-12-17 | 2009-06-18 | Chao Chen | Iron-Based Water Gas Shift Catalyst |
| CN106881082A (en) * | 2015-12-15 | 2017-06-23 | 中国科学院大连化学物理研究所 | For the Ir bases catalyst of reverse water-gas-shift reaction and its preparation and application |
| CN107497439A (en) * | 2017-08-09 | 2017-12-22 | 浙江海洋大学 | A kind of copper-based catalysts for reverse water-gas-shift reaction and preparation method thereof |
-
2020
- 2020-04-30 CN CN202010362905.9A patent/CN111547776A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090152500A1 (en) * | 2007-12-17 | 2009-06-18 | Chao Chen | Iron-Based Water Gas Shift Catalyst |
| CN106881082A (en) * | 2015-12-15 | 2017-06-23 | 中国科学院大连化学物理研究所 | For the Ir bases catalyst of reverse water-gas-shift reaction and its preparation and application |
| CN107497439A (en) * | 2017-08-09 | 2017-12-22 | 浙江海洋大学 | A kind of copper-based catalysts for reverse water-gas-shift reaction and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 宋天佑等编: "《无机化学（上册）》", 30 June 2019, 北京：高等教育出版社 * |
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Application publication date: 20200818 |