CN114345347B - 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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- cocatalyst
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- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 17
- 239000010941 cobalt Substances 0.000 title claims abstract description 17
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 230000001699 photocatalysis Effects 0.000 claims abstract description 22
- 238000006722 reduction reaction Methods 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 5
- 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 Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 claims description 6
- 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
- 239000002904 solvent Substances 0.000 claims description 4
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 claims description 3
- 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
- 238000005406 washing Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 229910052742 iron Inorganic materials 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000007146 photocatalysis Methods 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
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 2
- 230000010757 Reduction Activity Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 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 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 description 2
- 239000012279 sodium borohydride Substances 0.000 description 2
- 239000007787 solid 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
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 229940011182 cobalt acetate Drugs 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical group [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 1
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 1
- 229940044175 cobalt sulfate Drugs 0.000 description 1
- 229910000361 cobalt sulfate Inorganic materials 0.000 description 1
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 description 1
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 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 description 1
- 229910000360 iron(III) sulfate Inorganic materials 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
- 239000000843 powder Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum 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
Classifications
-
- 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
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Abstract
The invention provides a preparation method and application of a cobalt ferrite cocatalyst, and belongs to the field of energy and environmental photocatalysis. The cobalt ferrite cocatalyst is prepared by preparing a CoFeO X precursor through a cobalt source and an iron source through a coprecipitation method, and then calcining the precursor through a calcining method for 2-4 hours. The cobalt ferrite cocatalyst prepared by the method is a nano layered material, integrates the advantages of the transmission performance of transition metal ions to electrons, the large specific surface area of a two-dimensional material, the high activity exposure ratio and the like, and can effectively promote the performance of photocatalytic CO 2 reduction reaction; the preparation method is simple and easy to implement, the reaction system condition is mild, and the method has wide application prospect in the aspects of realizing fixation and conversion of CO 2 by utilizing solar energy and the like.
Description
Technical Field
The invention belongs to the technical field of novel material preparation and photocatalytic CO 2 reduction, and particularly relates to a cocatalyst CoFeO X, and a preparation method and application thereof.
Background
With the increasing severity of environmental problems such as energy crisis and greenhouse effect, sustainable development of human society faces a great challenge, and how to effectively use solar energy to realize fixation and conversion of carbon dioxide has attracted widespread attention in countries around the world. CO 2 is converted into more valuable chemical raw materials such as CO, CH 4、CH3 OH, HCHO, HCOOH and the like by utilizing a photocatalysis technology, so that the fixation of CO 2 can be realized, the greenhouse effect can be relieved to a certain extent, and important chemical raw materials can be provided for human beings. Therefore, achieving conversion of CO 2 by photocatalytic technology is a very attractive and challenging task. However, the existing reduction reaction of the photocatalytic CO 2 is low in efficiency, so that the practical application is greatly restricted, and the introduction of the cocatalyst is considered as an effective means for improving the reduction efficiency of the photocatalytic CO 2, so that the successful development and design of the novel efficient cocatalyst are one of key technologies for realizing the fixation and conversion of the CO 2 by utilizing solar energy.
Disclosure of Invention
The invention aims to provide a cocatalyst CoFeO X, a preparation method and application thereof, wherein the preparation method is simple and feasible, does not need complex and expensive equipment, has mild synthesis conditions and is beneficial to popularization; the catalyst is applied to the reduction of visible light catalytic CO 2, and can effectively promote the performance of CO 2 photocatalytic reduction reaction.
In order to achieve the above purpose, the invention adopts the following technical scheme:
The preparation method of cobalt ferrite cocatalyst comprises the steps of dissolving compound solids serving as cobalt sources and compound solids serving as iron sources in a solvent to prepare a solution; stirring the obtained solution for 10 minutes; dropwise adding a sodium borohydride solution into the solution while stirring, continuously stirring for 10 minutes, centrifuging by using a centrifugal machine, centrifugally washing the obtained precipitate by using ethanol until the ion concentration is less than 10ppm, drying at 40-120 ℃ for 12-24 hours, and grinding to obtain a CoFeO X precursor; and calcining the precursor in an inert atmosphere muffle furnace at 200-800 ℃ for 2-4 hours to obtain CoFeO X powder, namely the cobalt ferrite cocatalyst.
The cobalt source is cobalt nitrate, cobalt acetate, cobalt chloride and cobalt sulfate; the iron source is ferric nitrate, ferric chloride and ferric sulfate; the solvent is deionized water and ethanol; the concentration of the sodium borohydride is 0.1-1.0 mol/L.
Cobalt ferrite cocatalysts prepared by the above preparation method.
The cobalt ferrite cocatalyst prepared by the preparation method is applied to a photocatalytic CO 2 reduction system as a cocatalyst.
The photocatalytic CO 2 reduction system is an intermittent photocatalytic CO 2 reduction reaction system under normal pressure, wherein bipyridine ruthenium complex [ Ru (bpy) 3]Cl2•6H2 O ] is used as a visible light photosensitizer, triethanolamine is used as an electron sacrificial agent, and acetonitrile or a mixed solution of acetonitrile and water is used as a solvent.
The dosage of the cobalt ferrite cocatalyst is 1-30% of the mass of the photosensitizer.
The reaction temperature of the photocatalytic CO 2 reduction system is 10-80 ℃ and the reaction time is 15-180 min.
The invention has the remarkable advantages that:
(1) The method uses the CoFeO X as the cocatalyst for the photocatalytic field for the first time, and can effectively improve the reduction reaction efficiency of the photocatalytic CO 2.
(2) The preparation method of the cobalt ferrite cocatalyst is simple and feasible, does not need complex and expensive equipment, has mild synthesis conditions, and is favorable for large-scale popularization.
(3) The reaction system applied by the invention is simple and feasible, the dosage of the auxiliary agent is small, the reaction condition is mild, and the method is favorable for popularization and application in the CO 2 fixing technology.
Drawings
FIG. 1 is an X-ray diffraction pattern of CoFeO X in example 1 of the present invention.
FIG. 2 is a scanning electron microscope image of CoFeO X in example 1 of the present invention.
FIG. 3 is a graph showing the photocatalytic CO 2 reduction activity of CoFeO X as a promoter in example 1 of the present invention.
Detailed Description
Example 1
Weighing 0.582 g Co (NO 3)2·6H2 O and 0.808 g Fe (NO 3)3·9H2 O are respectively dissolved in 50 mL deionized water (H 2 O)), stirring the solution for 10 min, slowly dripping 20 mL NaBH 4 (0.25M) solution into the stirred solution, continuously stirring for 5 min, transferring into a 50 mL centrifuge tube, centrifugally washing, vacuum-drying at 60 ℃ for 12H to obtain a CoFeO X precursor, and calcining the CoFeO X precursor for 2 hours at 600 ℃ in Ar atmosphere to obtain CoFeO X.
FIG. 1 is an XRD spectrum of the material prepared in example 1, and it can be seen from the figure that the prepared sample is CoFeO X (PDF # 79-1744) in rhombohedral phase.
FIG. 2 is a scanning electron microscope image of a sample of CoFeO X prepared in example 1 of the present invention, from which it can be seen that the sample exhibits an ultra-thin nanolamellar morphology.
Example 2
0.243.2 G of CoCl 2·6H2 O and 0.553 g FeCl 2·6H2 O are weighed and dissolved in 60mL glycol, the solution is stirred for 30min, 4.92 g CH 3 COONa is added and stirred for 10 min, then the mixture is transferred into a 100 mL reaction kettle for heating for 10 h at 200 ℃, cooled to room temperature, centrifugally washed, and dried in vacuum at 60 ℃ for 12 h, thus obtaining a CoFeOx sample.
Example 3
0.249 GCo (CH 3COOH)2·4H2 O and 0.808 g Fe (NO 3)3·9H2 O in 50mL deionized water with stirring for 10 min, then 1M NaOH was added dropwise to the solution to a solution ph=10, the solution was heated at 100 ℃ for 120 min, washed several times with deionized water until the solution was neutral, and finally the precipitate was dried in 80 ℃ air to give a CoFeOx sample.
Evaluation of the reduction Activity of Co-catalyst CoFeO X photo-catalytic CO 2 prepared in example 1
The CoFeO X material prepared in example 1 is used as a cocatalyst for photocatalytic reduction of CO 2, the 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, 3 mg CoFeO X cocatalyst and 8mg bipyridine ruthenium complex ([ Ru (bpy) 3]Cl2·6H2 O) photosensitizer are weighed into the reactor, and then 3 mL water, 2 mL acetonitrile and 1mL triethanolamine are added and stirred uniformly. The system is vacuumized by a mechanical pump, then high-purity CO 2 gas is filled, and the lamp is turned on for reaction after the adsorption balance is 30 min. The gas phase product formed by the reaction was analyzed by gas chromatography detection.
Fig. 3 is an activity diagram of photocatalytic CO 2 reduction in a system of the sample prepared in example 1 of the present invention, under the system, the main reduction products are CO and H 2, and after 1 hour of illumination, the CO and H 2 yields reach 45.66 μmol and 8.71 μmol, respectively.
The foregoing description is only of the preferred embodiments of the invention, and all changes and modifications that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (1)
1. The application of the cobalt ferrite cocatalyst is characterized in that:
as a promoter in a photocatalytic CO 2 reduction system;
The photocatalytic CO 2 reduction system is an intermittent photocatalytic CO 2 reduction reaction system under normal pressure, wherein a bipyridine ruthenium complex [ Ru (bpy) 3]Cl2•6H2 O ] is used as a visible light photosensitizer, triethanolamine is used as an electron sacrificial agent, and acetonitrile or a mixed solution of acetonitrile and water is used as a solvent; the dosage of the cobalt ferrite cocatalyst is 1-30% of the mass of the photosensitizer, the reaction temperature of the photocatalytic CO 2 reduction system is 10-80 ℃, and the reaction time is 15-180 min;
The preparation method of the cobalt ferrite cocatalyst comprises the following steps:
Weighing 0.582 g Co (NO 3)2·6H2 O and 0.808 g Fe (NO 3)3·9H2 O are respectively dissolved in 50 mL deionized water, stirring the solution for 10 min, slowly dripping 20 mL of 0.25M NaBH 4 solution into the stirred solution, continuously stirring for 5 min, transferring into a 50 mL centrifuge tube, centrifugally washing, vacuum drying at 60 ℃ for 12h to obtain a CoFeO X precursor, and calcining the CoFeO X precursor for 2 hours at 600 ℃ in Ar atmosphere to obtain CoFeO X.
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