CN113578386A - Preparation of Fe2 Co-based metal organic framework CO2 reduction photocatalyst - Google Patents
Preparation of Fe2 Co-based metal organic framework CO2 reduction photocatalyst Download PDFInfo
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- CN113578386A CN113578386A CN202110689397.XA CN202110689397A CN113578386A CN 113578386 A CN113578386 A CN 113578386A CN 202110689397 A CN202110689397 A CN 202110689397A CN 113578386 A CN113578386 A CN 113578386A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000011941 photocatalyst Substances 0.000 title claims description 16
- 239000012921 cobalt-based metal-organic framework Substances 0.000 title claims description 10
- CDOWNLMZVKJRSC-UHFFFAOYSA-N 2-hydroxyterephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C(O)=C1 CDOWNLMZVKJRSC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 3
- 239000001301 oxygen Substances 0.000 claims abstract description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 229960000583 acetic acid Drugs 0.000 claims description 5
- 239000012362 glacial acetic acid Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 230000001603 reducing effect Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 1
- 239000012621 metal-organic framework Substances 0.000 abstract description 12
- 239000013078 crystal Substances 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 16
- 229910002092 carbon dioxide Inorganic materials 0.000 description 16
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 13
- 230000001699 photocatalysis Effects 0.000 description 13
- 239000002184 metal Substances 0.000 description 8
- 239000001569 carbon dioxide Substances 0.000 description 7
- 235000019253 formic acid Nutrition 0.000 description 7
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 6
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 125000000524 functional group Chemical group 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004255 ion exchange chromatography Methods 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000013110 organic ligand Substances 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- GPNNOCMCNFXRAO-UHFFFAOYSA-N 2-aminoterephthalic acid Chemical compound NC1=CC(C(O)=O)=CC=C1C(O)=O GPNNOCMCNFXRAO-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000010757 Reduction Activity Effects 0.000 description 1
- 238000002441 X-ray diffraction 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
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/1691—Coordination polymers, e.g. metal-organic frameworks [MOF]
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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
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
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- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F15/00—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic Table
- C07F15/06—Cobalt compounds
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- B01J2231/00—Catalytic reactions performed with catalysts classified in B01J31/00
- B01J2231/60—Reduction reactions, e.g. hydrogenation
- B01J2231/62—Reductions in general of inorganic substrates, e.g. formal hydrogenation, e.g. of N2
- B01J2231/625—Reductions in general of inorganic substrates, e.g. formal hydrogenation, e.g. of N2 of CO2
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- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/80—Complexes comprising metals of Group VIII as the central metal
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Abstract
The invention belongs to the field of metal organic frameworks, and particularly relates to a preparation method of a novel metal organic framework catalyst, which has a structural formula as follows: [ Fe ]2Co(μ3‑O)(C8H4O5)3(H2O)3]In which mu 3 is oxygen bridged, C8H4O5Is 2-hydroxy terephthalic acid and has a molecular formula of Fe2CoC24H18O19And the molecular weight is 781.01. The structural unit of the crystal belongs to a hexagonal system, P63mmc space group and unit cell parameters
α is 90 °, β is 90 °, γ is 120 °, unit cell volume is
And Z is 2. In the invention, Fe2The metal organic framework synthesized by Co cluster and 2-hydroxy terephthalic acid has high utilization rate of visible light, good photoproduction electron-hole separation effect and CO2The reduction performance is good.
Description
Technical Field
The invention belongs to the field of metal-organic framework material catalysts, and particularly relates to CO2Preparation of a reduction photocatalyst and application thereof in photocatalytic carbon dioxide reduction.
Background
Since the nineteenth century, the development and utilization of fossil fuels have been accelerated by the progress of industrialization, and the combustion of a large amount of fossil fuels has led to an increasing concentration of greenhouse gases (mainly carbon dioxide gas) in the air, and environmental and energy problems have also become serious. Inexhaustible solar energy has attracted the wide attention of scientists because of its cleanliness and no pollution, and the use of solar energy to reduce carbon dioxide into valuable carbon-containing chemicals is one of the hotspots today.
Metal Organic Frameworks (MOFs) have wide application in the field of photocatalysis due to the characteristics of large specific surface area, adjustable pore size, strong adsorption capacity and the like. However, the defects of easy recombination of photo-generated electrons and holes, low photocatalytic efficiency and the like of single MOFs material generally exist, and the limitation of MOFs in photocatalysis of CO is limited2Reduction performance. To further enhance the single MOFs in photocatalytic CO2The invention adopts a solvothermal method to synthesize PCN-242-Fe by using an organic ligand with-OH functional groups and metal nodes of a double metal cluster active center2The Co-OH metal organic framework material promotes the separation of photoproduction electron-hole and the transfer of photoproduction charge, and greatly improves PCN-242-Fe2Photocatalytic CO of Co-OH materials2Reducing and producing formic acid.
Disclosure of Invention
The invention aims to solve the problem of CO in a single MOFs material2Weak adsorption capacity and restriction of photocatalytic CO2Problem of reducing Properties, PCN-242-Fe was synthesized using organic ligands with-OH functional groups and metal nodes of the active center of a double metal cluster2The Co-OH metal organic framework material has good photoproduction charge transfer capability, can be used for photocatalytic reduction of carbon dioxide into formic acid, and can be used as a photocatalyst.
One of the present invention has a hydroxyl functionPCN-242-Fe with clustered and double metal cluster active centers2Co-OH photocatalytic CO2The preparation method of the reduction catalyst is completed according to the following steps:
respectively adding Fe2Co(μ3-O)(CH3COO)6And 2-hydroxy terephthalic acid are dissolved in N, N-dimethylformamide, and then glacial acetic acid is added; uniformly ultrasonically dispersing the mixed system, transferring the mixed system into a high-pressure reaction kettle, and heating the reaction kettle at 130-160 ℃ for reacting for 18-36 h; naturally cooling to room temperature, filtering, washing, and vacuum drying the product to obtain Fe2Co-based metal organic framework CO2Reducing photocatalyst PCN-242-Fe2Co-OH；
Fe described in the above step2Co(μ3-O)(CH3COO)6And 2-hydroxyterephthalic acid is added in a mass ratio of 1: 3;
the volume of the glacial acetic acid added in the step is 0.2-0.4 mL;
in the steps, the ultrasonic frequency is 35-45 KHz, the ultrasonic time is 20-30 min, and the stirring speed is 300-350 r/min.
Photocatalytic CO2The reduction activity test procedure was as follows: firstly, ultrasonically dispersing the photocatalyst obtained in the step in a mixed solvent of acetonitrile and water. Then introducing high-purity CO into the solvent2Gas purge for 30 min to remove solvent and other gases from the reactor sufficiently, CO at 1 atm2Sealing under saturation; in a 300W Xe lamp (lambda)>420 nm), continuously stirring the mixture at the stirring speed of 300 r/min-350 r/min, and analyzing the generation of formic acid in the liquid phase by an ion chromatograph of a reduction product after 5 hours of reaction.
The invention has the beneficial effects that:
the invention prepares PCN-242-Fe with-OH functional group and double metal cluster active center2Co-OH photocatalytic CO2The reduction catalyst solves the defect that photoproduction electron-hole is easy to compound, greatly improves the transfer of photoproduction charge, and improves the photocatalysis CO2Reduction of formic acid production performance, formic acid production in the liquid phase was analyzed by ion chromatography with a yield of 145.3μmolg-1h-1。
Drawings
FIG. 1 shows PCN-242-Fe2Synthetic scheme for Co-OH;
FIG. 2 shows PCN-242-Fe2X-ray powder diffraction pattern of Co-OH.
Detailed Description
The present invention is described in more detail in the following examples, which are not intended to limit the invention thereto.
Example 1:
10mg of 2-aminoterephthalic acid and 10mg of Fe were added to the reaction mixture, respectively2Co metal clusters are simultaneously dissolved in a high-pressure reaction kettle containing 2mL of N, N-Dimethylformamide (DMF) and 15 mL of polytetrafluoroethylene, and 0.4mL of glacial acetic acid is added after the Co metal clusters are dissolved in ultrasonic with the frequency of 40 KHz; uniformly dispersing the mixed system, adding the mixed system into a high-pressure reaction kettle, and then heating and reacting for 24 hours at 150 ℃; naturally cooling to room temperature, collecting solid by centrifugation, washing with 10 mL DMF for 5 times, soaking the collected solid powder in anhydrous acetone for 48 h, replacing solvent for 5 times, and vacuum drying at 120 deg.C for 12 h to obtain 16.5mg PCN-242-Fe2Co-OH。
The product was structurally analyzed by single crystal diffraction (Bruker SMART apaxii X-ray single crystal diffractometer):
the molecular formula is [ Fe2Co(μ3-O) (C8H4O5)3 (H2O)3]In which mu 3 is oxygen bridged, C8H4O5Is 2-hydroxy terephthalic acid and has a molecular formula of Fe2CoC24H18O19The molecular weight is 781.01, the structural unit belongs to a hexagonal system, P63mmc space group, the unit cell parameters are a = 13.282(7) A, b = 13.282(7) A, c =18.169(15) A, alpha =90 degrees, beta =90 degrees, gamma =120 degrees, the unit cell volume is 2776(4) A3，Z=2。
FIG. 1 is a scheme of synthesis of example 1.
FIG. 2 shows the results for PCN-242-Fe obtained in example 12The Co-OH photocatalyst material was subjected to X-ray powder diffraction (PXRD) detection to yield the following results as shown in fig. 2: 1 is PCN-242-Fe2Standard simulated peak of Co-OH; 2 is PCN-242-Fe prepared in example 12Co-OH test Peak, resulting PCN-242-Fe2The X-ray diffraction peak of Co-OH is consistent with the standard simulation peak, which proves that PCN-242-Fe is successfully synthesized2A Co-OH catalytic material.
PCN-242-Fe2Characterization and performance detection of the Co-OH photocatalytic reduction carbon dioxide catalyst material:
5mg of the photocatalyst obtained in the above step was dispersed in a mixed solvent of 4mL of acetonitrile and 1 mL of water. Then introducing high-purity CO into the solvent2Gas purge for 30 min to remove solvent and other gases from the reactor sufficiently, CO at 1 atm2And sealing under saturation. In a 300W Xe lamp (lambda)>420 nm), the mixture was continuously stirred at a stirring speed of 350r/min, and then the reduction product after 5 hours of reaction was analyzed for the production of HCOOH in the liquid phase by ion chromatography, with a yield of 145.3. mu. molg-1h-1。
PCN-242-Fe obtained by the present embodiment2The Co-OH photocatalyst material has good carbon dioxide reduction capability, can be used for photocatalytic reduction of carbon dioxide into formic acid, and can be used as a photocatalyst.
Claims (6)
1. Fe2Co-based metal organic framework CO2A reducing photocatalyst, characterized in that it is a compound of the following formula:
[Fe2Co(μ3-O) (C8H4O5)3 (H2O)3]in which mu 3 is oxygen bridged, C8H4O5Is 2-hydroxy terephthalic acid and has a molecular formula of Fe2CoC24H18O19Molecular weight is 781.01; the structural unit of the material belongs to a hexagonal system, P63mmc space group, unit cell parameters a = 13.282(7) A, b = 13.282(7) A, c =18.169(15) A, α =90 °, β =90 °, γ =120 °, and unit cell volume of 2776(4) A3，Z=2。
2. Fe of claim 12Co-based metal organic framework CO2Reducing lightA method for preparing a catalyst, characterized by comprising the steps of:
respectively adding Fe2Co(μ3-O) (CH3COO)6And 2-hydroxy terephthalic acid are dissolved in N, N-dimethylformamide, and then glacial acetic acid is added; the mixed system is transferred to a high-pressure reaction kettle after being dispersed evenly by ultrasonic, and the reaction kettle is heated and reacted for 24 hours at the temperature of 150 ℃; naturally cooling to room temperature, filtering, washing, and vacuum drying at 120 deg.C for 12 h to obtain Fe2Co-based metal organic framework CO2The photocatalyst is reduced.
3. Fe in claim 22Co-based metal organic framework CO2A process for preparing a reduced photocatalyst, characterized in that in the step (A) Fe2Co(μ3-O) (CH3COO)6And 2-hydroxyterephthalic acid was added in a mass ratio of 1: 3.
4. Fe in claim 22Co-based metal organic framework CO2The preparation method of the reduction photocatalyst is characterized in that the volume of the glacial acetic acid added in the step is 0.2-0.4 mL.
5. Fe in claim 22Co-based metal organic framework CO2The preparation method of the reduction photocatalyst is characterized in that in the steps, the ultrasonic frequency is 35-45 KHz, and the ultrasonic time is 20-30 min.
6. Fe in claim 22Co-based metal organic framework CO2The preparation method of the reduction photocatalyst is characterized in that the stirring speed in the step is 300 r/min-350 r/min.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114989447A (en) * | 2022-08-02 | 2022-09-02 | 广东工业大学 | Water-stable mixed-valence MOF material, preparation method thereof and application thereof in photocatalytic water decomposition |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114989447A (en) * | 2022-08-02 | 2022-09-02 | 广东工业大学 | Water-stable mixed-valence MOF material, preparation method thereof and application thereof in photocatalytic water decomposition |
| CN114989447B (en) * | 2022-08-02 | 2022-12-09 | 广东工业大学 | Water-stable mixed-valence MOF material, preparation method thereof and application thereof in photocatalytic water decomposition |
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