CN111589448A - Carbon dioxide electro-reduction catalyst with ultrahigh gas phase selectivity - Google Patents
Carbon dioxide electro-reduction catalyst with ultrahigh gas phase selectivity Download PDFInfo
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- CN111589448A CN111589448A CN202010514944.6A CN202010514944A CN111589448A CN 111589448 A CN111589448 A CN 111589448A CN 202010514944 A CN202010514944 A CN 202010514944A CN 111589448 A CN111589448 A CN 111589448A
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- carbon dioxide
- tubular furnace
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 16
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 12
- 239000003054 catalyst Substances 0.000 title claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000007864 aqueous solution Substances 0.000 claims abstract description 18
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims abstract description 8
- 239000007789 gas Substances 0.000 claims abstract description 8
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 8
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 8
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000013077 target material Substances 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 238000000967 suction filtration Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000012298 atmosphere Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 238000006722 reduction reaction Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000035425 carbon utilization Effects 0.000 description 2
- 229910000420 cerium oxide Inorganic materials 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002073 nanorod Substances 0.000 description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000011946 reduction process Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- -1 copper-substituted cerium oxide Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000006261 foam material Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- IRPLSAGFWHCJIQ-UHFFFAOYSA-N selanylidenecopper Chemical compound [Se]=[Cu] IRPLSAGFWHCJIQ-UHFFFAOYSA-N 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 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
- B01J23/72—Copper
-
- 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
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B3/00—Electrolytic production of organic compounds
- C25B3/20—Processes
- C25B3/25—Reduction
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Catalysts (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a carbon dioxide electro-reduction catalyst with ultrahigh gas phase selectivity, which is prepared by adding copper chloride into deionized water, then adding sodium hydroxide aqueous solution, and violently stirring; adding sodium borohydride aqueous solution, and carrying out suction filtration and drying on the obtained solution; and then, carrying out air burning on the obtained solid sample in a tubular furnace, and carrying out air burning on the sample in the tubular furnace under the nitrogen atmosphere to obtain the target material. The invention has the advantages of good catalytic effect and high Faraday efficiency of gas-phase products.
Description
Technical Field
The invention belongs to the technical field of new energy chemistry and electrocatalysis intersection, and relates to a carbon dioxide electroreduction catalyst with ultrahigh gas phase selectivity and a preparation method thereof.
Background
The combustion of traditional fossil fuels such as coal, oil and natural gas can emit a large amount of CO in the air2CO in air2The high concentration can cause a series of environmental problems such as global warming and sea level rising, and simultaneously, a large amount of CO in the air2Is also a C source with abundant reserves if CO can be mixed2Can be converted into chemical with economic benefit and also can be effectively usedThe energy crisis and other problems faced by human beings are alleviated. Currently, the energy structure is in the key phase of switching from high carbon utilization to low carbon utilization, CO2The global warming caused has become one of the most environmental concerns worldwide. For reducing CO in the atmosphere2Content, vigorously develops low-carbon technology, and uses various technical means to convert CO2Recycling is the most efficient method. In a plurality of CO2In the conversion technique, CO is electrocatalyzed2The reduction can be realized at normal temperature and normal pressure, so that the reaction condition is mild and the operation is simple; and the selective synthesis of the product can be realized by controlling the electrode and the reaction condition in the electro-reduction process. Electrochemical reduction of CO relative to other reduction processes2Has better application prospect. In the catalysis of CO2Of the many catalysts for reduction, copper-based materials have received the most extensive attention, being effective in CO-reduction2And converting into hydrocarbon products. Peter Broekmann et al prepared bimetallic AgCu foam materials using additive assisted electrodeposition with a dynamic hydrogen bubble template. The silver and the copper in the material keep complete phase separation, and the nano silver is highly dispersed in the copper matrix. The thermal annealing is carried out under mild conditions (200 ℃,12 hours), and the CO can be increased2RR ethanol selectivity. The Hanbuxing research group of the chemical institute of Chinese academy of sciences discovers that the copper selenide nano-catalyst has excellent performance in the process of producing methanol by a carbon dioxide electrochemical reduction method, and the current density can reach 41.5mA cm < -2 > under the low overvoltage of 285mV, and the Faraday efficiency is 77.6%. This current density is higher than the current densities reported so far and the faradaic efficiency of methanol production is very high. The professor Zhenggunfeng of chemical department of the university of Compound denier designs and synthesizes a copper-substituted cerium oxide nanorod material (Cu-CeO)2) High dispersion of Cu on the cerium oxide is realized; meanwhile, the (110) surface specifically exposed by the cerium oxide nanorod is a crystal surface which is most prone to generating oxygen vacancies, and the structure of the oxygen vacancies is beneficial to the catalytic reduction reaction of the material. Cu-CeO2The faradaic efficiency of catalyzing ECR reaction to generate methane reaches 58 percent.
Disclosure of Invention
The invention aims to provide a carbon dioxide electro-reduction catalyst with ultrahigh gas phase selectivity, which has the advantages of good catalytic effect and high Faraday efficiency of gas phase products.
The technical scheme adopted by the invention is as follows:
step 1: adding copper chloride into deionized water, then adding a sodium hydroxide aqueous solution, and violently stirring;
step 2: adding sodium borohydride aqueous solution, and carrying out suction filtration and drying on the obtained solution;
and step 3: and then, carrying out air burning on the obtained solid sample in a tubular furnace, and carrying out air burning on the sample in the tubular furnace under the nitrogen atmosphere to obtain the target material.
Further, 50-80mg of copper chloride is added into deionized water, then 20-30ml of 0.5mol/L sodium hydroxide aqueous solution is added, the mixture is stirred vigorously, then 20-30ml of 0.03mol/L sodium borohydride aqueous solution is added, and the obtained solution is filtered and dried.
And further, the solid sample is subjected to air burning in a tubular furnace at 200 ℃ for 3 hours in the air atmosphere, and then the sample is subjected to air burning in a tubular furnace at 300 ℃ for 3 hours in the nitrogen atmosphere, so that the target material is obtained.
Drawings
FIG. 1 is a schematic diagram of a transmission electron microscope morphology of a material;
figure 2 is a graph of voltage versus faraday efficiency.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
Example 1
Adding 50-80mg of copper chloride into deionized water, then adding 20-30ml of 0.5mol/L sodium hydroxide aqueous solution, stirring vigorously, then adding 20-30ml of 0.03mol/L sodium borohydride aqueous solution, and carrying out suction filtration and drying on the obtained solution. And then, carrying out air burning on the obtained solid sample in a tubular furnace at 200 ℃ for 3 hours in the air atmosphere, and then carrying out air burning on the sample in the tubular furnace at 300 ℃ for 3 hours in the nitrogen atmosphere to obtain the target material. The material is subjected to an electrocatalytic carbon dioxide reduction test, and the Faraday efficiency of a gas-phase product can reach 70% under-1.3V vsRhHE.
Example 2
Adding 50-80mg of copper chloride into the nitrogen-removed doped graphene aqueous solution, then adding 20-30ml of 0.5mol/L sodium hydroxide aqueous solution, stirring vigorously, then adding 20-30ml of 0.03mol/L sodium borohydride aqueous solution, and carrying out suction filtration and drying on the obtained solution. And then, carrying out air burning on the obtained solid sample in a tubular furnace at 200 ℃ for 3 hours in the air atmosphere, and then carrying out air burning on the sample in the tubular furnace at 300 ℃ for 3 hours in the nitrogen atmosphere to obtain the target material. The material is subjected to an electrocatalytic carbon dioxide reduction test, and the Faraday efficiency of a gas-phase product can reach 96% under-1.3V vsRhHE.
Example 3
Adding 50-80mg of copper chloride into the nitrogen-removed doped graphene aqueous solution, then adding 20-30ml of 0.5mol/L sodium hydroxide aqueous solution, stirring vigorously, then adding 20-30ml of 0.03mol/L sodium borohydride aqueous solution, and carrying out suction filtration and drying on the obtained solution. And then, the obtained solid sample is subjected to air burning in a tube furnace at 200 ℃ for 3 hours in the air atmosphere, the sample is subjected to material treatment at 200 ℃ in the nitrogen atmosphere, the obtained material catalyzes carbon dioxide to perform electric reduction, and the Faraday efficiency of a gas-phase product can reach 73% under-1.3V.
FIG. 1 is a schematic view of a transmission electron microscope. Figure 2 is a graph of voltage versus faraday efficiency. The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not intended to limit the present invention in any way, and all simple modifications, equivalent variations and modifications made to the above embodiments according to the technical spirit of the present invention are within the scope of the present invention.
Claims (3)
1. A carbon dioxide electro-reduction catalyst with ultrahigh gas phase selectivity is characterized by comprising the following steps:
step 1: adding copper chloride into deionized water, then adding a sodium hydroxide aqueous solution, and violently stirring;
step 2: adding sodium borohydride aqueous solution, and carrying out suction filtration and drying on the obtained solution;
and step 3: and then, carrying out air burning on the obtained solid sample in a tubular furnace, and carrying out air burning on the sample in the tubular furnace under the nitrogen atmosphere to obtain the target material.
2. The carbon dioxide electro-reduction catalyst with ultra-high gas phase selectivity as recited in claim 1, wherein: adding 50-80mg of copper chloride into the deionized water, then adding 20-30ml of 0.5mol/L sodium hydroxide aqueous solution, stirring vigorously, then adding 20-30ml of 0.03mol/L sodium borohydride aqueous solution, and filtering and drying the obtained solution.
3. The carbon dioxide electro-reduction catalyst with ultra-high gas phase selectivity as recited in claim 1, wherein: and (3) air-burning the solid sample in a tubular furnace at 200 ℃ for 3 hours in the air atmosphere, and then air-burning the sample in the tubular furnace at 300 ℃ for 3 hours in the nitrogen atmosphere to obtain the target material.
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| CN202010514944.6A CN111589448B (en) | 2020-06-08 | 2020-06-08 | Carbon dioxide electro-reduction catalyst with ultrahigh gas phase selectivity |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090152500A1 (en) * | 2007-12-17 | 2009-06-18 | Chao Chen | Iron-Based Water Gas Shift Catalyst |
| CN104857958A (en) * | 2015-05-15 | 2015-08-26 | 中国科学院过程工程研究所 | Copper-based Cu-Cu2O-CuO catalyst as well as preparation method and application thereof |
| CN108187713A (en) * | 2017-12-07 | 2018-06-22 | 中国科学院上海高等研究院 | A kind of nitrogen co-doped carbon nano-tube catalyst of copper and its preparation method and application |
| CN110280244A (en) * | 2019-07-17 | 2019-09-27 | 肇庆市华师大光电产业研究院 | A kind of carbon dioxide electrochemical reduction catalyst and preparation method thereof |
| CN110404537A (en) * | 2019-05-30 | 2019-11-05 | 重庆交通大学 | CuO@Cu2The preparation method of O@Cu micro-nano ball |
-
2020
- 2020-06-08 CN CN202010514944.6A patent/CN111589448B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090152500A1 (en) * | 2007-12-17 | 2009-06-18 | Chao Chen | Iron-Based Water Gas Shift Catalyst |
| CN104857958A (en) * | 2015-05-15 | 2015-08-26 | 中国科学院过程工程研究所 | Copper-based Cu-Cu2O-CuO catalyst as well as preparation method and application thereof |
| CN108187713A (en) * | 2017-12-07 | 2018-06-22 | 中国科学院上海高等研究院 | A kind of nitrogen co-doped carbon nano-tube catalyst of copper and its preparation method and application |
| CN110404537A (en) * | 2019-05-30 | 2019-11-05 | 重庆交通大学 | CuO@Cu2The preparation method of O@Cu micro-nano ball |
| CN110280244A (en) * | 2019-07-17 | 2019-09-27 | 肇庆市华师大光电产业研究院 | A kind of carbon dioxide electrochemical reduction catalyst and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 杨满平: "氧化铜电还原二氧化碳合成乙醇和正丙醇的研究", 《中国优秀博硕士学位论文全文数据库（硕士） 工程科技Ⅰ辑》 * |
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