CN114345347A - Cobalt ferrite cocatalyst, and preparation method and application thereof - Google Patents
Cobalt ferrite cocatalyst, and preparation method and application thereof Download PDFInfo
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- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 25
- 239000010941 cobalt Substances 0.000 title claims abstract description 25
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 230000001699 photocatalysis Effects 0.000 claims abstract description 18
- 238000006722 reduction reaction Methods 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000007146 photocatalysis Methods 0.000 claims abstract description 8
- 239000002243 precursor Substances 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 5
- 229910052742 iron Inorganic materials 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims abstract 6
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 7
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000003504 photosensitizing agent Substances 0.000 claims description 5
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical group [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 4
- 239000012279 sodium borohydride Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000012327 Ruthenium complex Substances 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 229940011182 cobalt acetate Drugs 0.000 claims description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical group [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- 229940044175 cobalt sulfate Drugs 0.000 claims description 2
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 2
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 230000009466 transformation Effects 0.000 abstract description 2
- 230000005540 biological transmission Effects 0.000 abstract 1
- 238000000975 co-precipitation Methods 0.000 abstract 1
- 229910001428 transition metal ion Inorganic materials 0.000 abstract 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 14
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 1
- BDAGIHXWWSANSR-UHFFFAOYSA-N Formic acid Chemical compound OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 1
- 229910021577 Iron(II) chloride Inorganic materials 0.000 description 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 1
- 230000010757 Reduction Activity Effects 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- 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
- Y02P20/10—Process efficiency
- Y02P20/133—Renewable energy sources, e.g. sunlight
Abstract
The invention provides a preparation method and application of a cobalt ferrite cocatalyst, belonging to the field of energy and environmental photocatalysis. The CoFeO is prepared by a coprecipitation method through a cobalt source and an iron sourceXAnd calcining the precursor for 2-4 hours by a calcining method to obtain the cobalt ferrite cocatalyst. The cobalt ferrite cocatalyst prepared by the invention is a nano-layered material, and the material combines the advantages of the transmission performance of transition metal ions to electrons and the large specific surface area, high active exposure ratio and the like of a two-dimensional material, and can efficiently promote photocatalysis CO2Performance of the reduction reaction; preparation ofThe method is simple and easy to implement, the reaction system has mild conditions, and CO is realized by using solar energy2Has wide application prospect in the aspects of fixation, transformation and the like.
Description
Technical Field
The invention belongs to novel material preparation and photocatalysis CO2The technical field of reduction, in particular to cocatalystAgent CoFeOXAnd a preparation method and application thereof.
Background
With the increasing severity of environmental problems such as energy crisis and greenhouse effect, the sustainable development of the human society faces a great challenge, and how to effectively utilize solar energy to fix and convert carbon dioxide has attracted wide attention of all countries in the world. By means of photocatalysis2Conversion to more valuable chemicals, e.g. CO, CH4、CH3OH, HCHO, HCOOH and the like, not only can realize the reaction to CO2The fixation of the compound can relieve the greenhouse effect to a certain extent and can also provide important chemical raw materials for human beings. Thus, the CO is treated by the photocatalysis technology2Is a very attractive and challenging issue. But at present photocatalytically CO2The reduction reaction efficiency is low, the practical application of the catalyst is greatly restricted, and the introduction of the cocatalyst is considered to be one of improving the photocatalytic CO2Effective means of reduction efficiency, so that the successful development and design of a novel efficient cocatalyst is to realize CO by utilizing solar energy2One of the key technologies for immobilization and transformation.
Disclosure of Invention
The invention aims to provide a cocatalyst CoFeOXThe preparation method and the application thereof are simple and easy to implement, do not need complex and expensive equipment, have mild synthesis conditions and are beneficial to popularization; application to visible light catalysis of CO2Reducing to promote CO efficiently2Performance of photocatalytic reduction reaction.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of cobalt ferrite cocatalyst is characterized in that a compound solid used as a cobalt source and a compound solid used as an iron source are dissolved in a solvent to prepare a solution; the resulting solution was stirred for 10 minutes; dropwise adding sodium borohydride solution into the solution while stirring, continuously stirring for 10 minutes, centrifuging by using a centrifuge, centrifugally washing the obtained precipitate by using ethanol until the ion concentration is reached<10ppm, drying at 40-120 ℃ for 12-24 hours, and grinding to obtain CoFeOXA precursor; calcining the precursor in an inert atmosphere muffle furnace at 200-XPowder, i.e. cobalt ferrite promoter.
The cobalt source is cobalt nitrate, cobalt acetate, cobalt chloride or cobalt sulfate; the iron source is ferric nitrate, ferric chloride or ferric sulfate; the solvent is deionized water and ethanol; the concentration of the sodium borohydride is 0.1-1.0 mol/L.
The cobalt ferrite cocatalyst prepared by the preparation method is provided.
Application of cobalt ferrite cocatalyst prepared by the preparation method in photocatalysis of CO2As a cocatalyst in the reduction system.
The photocatalytic CO2The reduction system is intermittent photocatalytic CO under normal pressure2Reduction reaction system with bipyridine ruthenium complex [ Ru (bpy) ]3]Cl2•6H2O is used as a visible light photosensitizer, triethanolamine is used as an electron sacrificial agent, and acetonitrile or a mixed solution of the acetonitrile and water is used as a solvent.
The amount of the cobalt ferrite cocatalyst is 1-30% of the mass of the photosensitizer.
The photocatalytic CO2The reaction temperature of the reduction system is 10-80 ℃, and the reaction time is 15-180 min.
The invention has the following remarkable advantages:
(1) the invention firstly uses CoFeOXCan be used as a cocatalyst in the field of photocatalysis and can effectively improve photocatalytic CO2The efficiency of the reduction reaction.
(2) The preparation method of the cobalt ferrite cocatalyst is simple and easy to implement, does not need complex and expensive equipment, has mild synthesis conditions, and is beneficial to large-scale popularization.
(3) The reaction system applied by the invention is simple and easy to implement, the dosage of the auxiliary agent is less, the reaction condition is mild, and the invention is beneficial to CO2Popularization and application in the fixing technology.
Drawings
FIG. 1 shows CoFeO in example 1 of the present inventionXX-ray diffraction pattern of (a).
FIG. 2 shows CoFeO in example 1 of the present inventionXScanning electron micrograph (c).
FIG. 3 is a drawing of the present inventionCoFeO in example 1XPhotocatalytic CO as a cocatalyst2Reduction activity diagram.
Detailed Description
Example 1
Weigh 0.582 g Co (NO)3)2·6H2O and 0.808 g Fe (NO)3)3·9H2O was dissolved in 50 mL of deionized water (H) respectively2O), the solution was stirred for 10 min and 20 mL of NaBH was added4Slowly dropping (0.25M) solution into the stirred solution, continuously stirring for 5 min, transferring into a 50 mL centrifuge tube, centrifugally washing, and vacuum drying at 60 ℃ for 12 h to obtain CoFeOXA precursor; CoFeO is addedXCalcining the precursor for 2h at 600 ℃ in Ar atmosphere to obtain CoFeOX。
FIG. 1 is the XRD spectrum of the material prepared in this example 1, from which it can be seen that the sample prepared is CoFeO in rhombohedral phaseX（PDF#79-1744）。
FIG. 2 shows the preparation of CoFeO in example 1 of the present inventionXAnd (3) a scanning electron microscope image of the sample, wherein the sample can be seen to be in an ultrathin nanometer layered shape.
Example 2
0.243.2 g CoCl were weighed out2·6H2O and 0.553 g FeCl2·6H2O in 60 mL ethylene glycol, stir the solution for 30 min, add 4.92 g CH3COONa is stirred for 10 min, then the mixture is moved into a 100 mL reaction kettle and heated at 200 ℃ for 10 h, cooled to room temperature, centrifugally washed, and dried in vacuum at 60 ℃ for 12 h to obtain a CoFeOx sample.
Example 3
Weighing 0.249 gCo (CH)3COOH)2·4H2O and 0.808 g Fe (NO)3)3·9H2O was dissolved in 50 mL deionized water and stirred for 10 min, then 1M NaOH was added dropwise to the solution to pH =10, after heating the solution at 100 ℃ for 120 min, washing with deionized water several times until the solution was neutral, and finally the precipitate was dried in air at 80 ℃ to give a sample of coffeox.
Example 1 preparation of the resulting cocatalyst CoFeOXPhotocatalytic CO2Evaluation of reduction Activity
CoFeO prepared in example 1XMaterial used as cocatalyst for photocatalytic reduction of CO2The reaction is carried out in a self-made normal-pressure batch reaction device, a 300W xenon lamp is used as a light source (a 420 nm optical filter is added), the temperature of the reaction system is controlled at 25 ℃ by circulating condensed water, and 3 mg CoFeO is weighedXCocatalyst and 8 mg of bipyridine ruthenium Complex ([ Ru (bpy))3]Cl2·6H2O) photosensitizer, then adding 3 mL of water, 2 mL of acetonitrile and 1 mL of triethanolamine, and uniformly stirring. Vacuumizing the system by a mechanical pump, and then filling high-purity CO2And (5) carrying out adsorption equilibrium on the gas for 30 min, and then turning on the lamp for reaction. The gas phase product generated by the reaction is detected and analyzed by gas chromatography.
FIG. 3 shows that example 1 of the present invention is used to prepare samples for photocatalytic CO reaction in the system2Activity diagram of reduction, under the system, the main reduction products are CO and H2After 1 hour of light exposure, CO and H2The yield reaches 45.66 mu mol and 8.71 mu mol respectively.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (7)
1. A preparation method of a cobalt ferrite cocatalyst is characterized by comprising the following steps:
dissolving a compound solid serving as a cobalt source and a compound solid serving as an iron source in a solvent to prepare a solution; the resulting solution was stirred for 10 minutes; dropwise adding sodium borohydride solution into the solution while stirring, continuously stirring for 10 minutes, centrifuging by using a centrifuge, centrifugally washing the obtained precipitate by using ethanol until the ion concentration is reached<10ppm, drying at 40-120 ℃ for 12-24 hours, and grinding to obtain CoFeOXA precursor; calcining the precursor in an inert atmosphere muffle furnace at 200-XPowder, i.e. cobalt ferrite promoter.
2. The method for preparing cobalt ferrite promoter according to claim 1, characterized in that:
the cobalt source is cobalt nitrate, cobalt acetate, cobalt chloride or cobalt sulfate; the iron source is ferric nitrate, ferric chloride or ferric sulfate; the solvent is deionized water and ethanol; the concentration of the sodium borohydride is 0.1-1.0 mol/L.
3. The cobalt ferrite promoter obtained by the method according to claim 1.
4. Use of a cobalt ferrite promoter prepared by the method of claim 1, wherein:
in the photocatalysis of CO2As a cocatalyst in the reduction system.
5. Use of a cobalt ferrite promoter according to claim 4, characterized in that:
the photocatalytic CO2The reduction system is intermittent photocatalytic CO under normal pressure2Reduction reaction system with bipyridine ruthenium complex [ Ru (bpy) ]3]Cl2•6H2O is used as a visible light photosensitizer, triethanolamine is used as an electron sacrificial agent, and acetonitrile or a mixed solution of the acetonitrile and water is used as a solvent.
6. Use of a cobalt ferrite promoter according to claim 5, characterized in that:
the amount of the cobalt ferrite cocatalyst is 1-30% of the mass of the photosensitizer.
7. Use of a cobalt ferrite promoter according to claim 6, characterized in that:
the photocatalytic CO2The reaction temperature of the reduction system is 10-80 ℃, and the reaction time is 15-180 min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116328785A (en) * | 2023-03-27 | 2023-06-27 | 辽宁大学 | Manganese ferrite/tubular graphite phase carbon nitride heterojunction photocatalyst and preparation method and application thereof |
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- 2022-01-20 CN CN202210066381.8A patent/CN114345347A/en active Pending
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