CN117619436A - RP/TpPa-1-COF photocatalyst, preparation method thereof and application thereof in photocatalytic water splitting hydrogen production reaction - Google Patents
RP/TpPa-1-COF photocatalyst, preparation method thereof and application thereof in photocatalytic water splitting hydrogen production reaction Download PDFInfo
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- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 27
- 239000001257 hydrogen Substances 0.000 title claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 24
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- 238000000265 homogenisation Methods 0.000 claims abstract description 6
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- 239000011668 ascorbic acid Substances 0.000 claims abstract description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 4
- 239000001301 oxygen Substances 0.000 claims abstract description 4
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- QCDYQQDYXPDABM-UHFFFAOYSA-N phloroglucinol Chemical compound OC1=CC(O)=CC(O)=C1 QCDYQQDYXPDABM-UHFFFAOYSA-N 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims description 5
- JPYHHZQJCSQRJY-UHFFFAOYSA-N Phloroglucinol Natural products CCC=CCC=CCC=CCC=CCCCCC(=O)C1=C(O)C=C(O)C=C1O JPYHHZQJCSQRJY-UHFFFAOYSA-N 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 229960001553 phloroglucinol Drugs 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000002064 nanoplatelet Substances 0.000 claims description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
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- 239000013310 covalent-organic framework Substances 0.000 description 52
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
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- 230000009897 systematic effect Effects 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Catalysts (AREA)
Abstract
The invention belongs to the technical field of catalytic hydrogen production, and particularly relates to an RP/TpPa-1-COF photocatalyst, a preparation method thereof and application thereof in photocatalytic water splitting hydrogen production reaction. According to the invention, RP nano sheets are prepared by a hydrothermal method and an ultrasonic method, then RP is added into the synthesis process of TpPa-1-COF, and the RP and the TpPa-1-COF are tightly combined by solvothermal reaction, so that the photocatalyst RP/TpPa-1-COF with high stability and high activity is obtained. Dispersing the catalyst into an aqueous solution of ascorbic acid, carrying out ultrasonic homogenization, adding a chloroplatinic acid solution, then introducing nitrogen into the solution to remove oxygen, and keeping the reaction system at 5 ℃ for catalytic reaction under visible light (lambda is more than or equal to 420 nm), so that high-efficiency catalytic water decomposition under visible light can be realized to produce hydrogen. The RP/TpPa-1-COF photocatalyst has higher photocatalytic performance and stability, and the preparation strategy is simple and easy to implement, so that the RP/TpPa-1-COF photocatalyst has good prospect in the field of photocatalytic water splitting hydrogen production.
Description
Technical Field
The invention belongs to the technical field of catalytic hydrogen production, and particularly relates to an RP/TpPa-1-COF photocatalyst, a preparation method thereof and application thereof in photocatalytic water splitting hydrogen production reaction.
Background
Photocatalytic water splitting hydrogen evolution is considered one of the most promising green technologies for clean sustainable energy and environmental remediation. In recent years, photocatalysts containing elements such as carbon, boron, sulfur, silicon, and phosphorus have been developed and exhibit good photocatalytic activity. Among them, the single element RP is used as a metal-free semiconductor material, has proper band gap structure, medium oxidation-reduction potential and relatively low toxicity, and is the most potential and reliable catalyst in the field of photocatalysis. Unfortunately, the photocatalytic hydrogen production activity of pure RP is severely limited due to the inherently low specific surface area, low light absorption range and slow photogenerated carrier transfer capability. Covalent Organic Frameworks (COFs) are highly crystalline porous materials formed by condensation of organic building units and have great potential in the field of photocatalysis due to their high specific surface area, extraordinary chemical stability, designable structure. COFs materials have many advantages in photocatalytic applications: COFs have a porous structure, which is favorable for diffusion of substrates and can provide more reaction sites; COFs are assembled from different building blocks, which enables them to achieve customized structures and corresponding functions. Thus, by adjusting the nature of the functional groups on the ligands, their light absorption range can be extended; the crystallinity of COFs facilitates further study of its photocatalytic mechanism; COFs are linked by strong covalent bonds and thus have excellent chemical stability. However, the low electron-hole pair separation efficiency and the rapid recombination of carriers remain major drawbacks of COFs materials photocatalysis. In recent years, systematic studies have been made on the application of COFs-based materials in the field of photocatalysis. In order to increase the photocatalytic activity of materials, a series of modification strategies have been developed, including metal doping, ligand modification, construction of heterojunctions, and defect engineering, wherein the construction of heterojunctions is considered an effective approach. How to improve the separation efficiency of photo-generated electron-hole pairs to obtain a photo-catalytic material with high activity and high stability is the key point of current research and development, and the modification of a photo-catalyst based on a COFs material by utilizing a heterojunction construction strategy is widely used in the field of photo-catalytic hydrogen production.
Disclosure of Invention
The invention aims to compound RP and TpPa-1-COF by a solvothermal method to obtain a novel material RP/TpPa-1-COF, and the material has good application prospect in photocatalytic water splitting hydrogen production.
The technical scheme adopted by the invention is as follows:
RP/TpPa-1-COF photocatalyst, wherein the mass ratio of RP to TpPa-1-COF=9:100.
The preparation method of the RP/TpPa-1-COF photocatalyst comprises the following steps: fully grinding the trialdehyde phloroglucinol Tp and the p-phenylenediamine Pa, adding the obtained solid and RP nano-sheets into DMF, adding acetic acid solution, carrying out ultrasonic homogenization, carrying out solvothermal reaction, centrifuging the obtained reactant, washing the obtained solid with tetrahydrofuran and acetone respectively, and carrying out vacuum drying to obtain the target product.
Further, according to the preparation method, the preparation method of the RP nano-sheet comprises the following steps: dispersing 5g of commercial red phosphorus into 75mL of deionized water, carrying out ultrasonic homogenization, collecting red phosphorus dispersion in the supernatant, carrying out hydrothermal reaction at 200 ℃ for 12h, centrifugally collecting the obtained product, then dispersing into 50mL of deionized water, and carrying out ultrasonic treatment for 6h to obtain the RP nano-sheet.
Further, according to the preparation method, the grinding time is 15min.
Further, in the above preparation method, the concentration of the acetic acid solution is 3M.
Further, according to the preparation method, the ultrasonic time is 30min.
Further, according to the preparation method, the solvothermal reaction condition is that the reaction is carried out for 72 hours at 120 ℃.
The RP/TpPa-1-COF photocatalyst is applied to hydrogen production by photocatalytic water splitting as a catalyst.
Further, the application method comprises the following steps: dispersing RP/TpPa-1-COF photocatalyst in water solution dissolved with sacrificial agent, adding chloroplatinic acid solution, introducing nitrogen into the solution to remove oxygen, keeping the reaction system at 5 ℃ through a low-temperature constant-temperature tank, and carrying out catalytic reaction under visible light.
Further, in the above application, the sacrificial agent is ascorbic acid.
The beneficial effects of the invention are as follows:
1. according to the invention, RP nano sheets are obtained by a simple hydrothermal method and an ultrasonic method, after being fully ground, the trialdehyde phloroglucinol (Tp) and the p-phenylenediamine (Pa) are added into DMF together with the RP nano sheets, then acetic acid is added and ultrasonic is uniform, and a catalyst RP/TpPa-1-COF with higher photocatalytic performance is obtained by a solvothermal method, and can realize high-efficiency photocatalytic water splitting hydrogen production under visible light.
2. After RP and TpPa-1-COF are compounded to form a heterojunction, the reaction active site is increased due to the improvement of the carrier separation efficiency, the migration rate of charges between material interfaces is accelerated, and the catalytic water decomposition hydrogen release activity of the TpPa-1-COF is improved by about 4.1 times compared with that of the TpPa-1-COF. Therefore, the RP/TpPa-1-COF photocatalyst has higher photocatalytic performance and stability, and the preparation strategy is simple and easy to implement, and has good prospect in the field of photocatalytic water splitting hydrogen production.
Drawings
FIG. 1 is a solid ultraviolet-visible diffuse reflectance spectrum of TpPa-1-COF, RP nanoplatelets, and RP/TpPa-1-COF composites.
FIG. 2 (a) is a transmission electron microscope image of TpPa-1-COF; FIG. 2 (b) is a transmission electron microscope image of RP nanoplatelets; FIG. 2 (c) is a scanning electron microscope image of the RP/TpPa-1-COF complex.
FIG. 3 is a schematic diagram of catalytic hydrolysis hydrogen production of RP/TpPa-1-COF composite under visible light (lambda. Gtoreq.420 nm).
FIG. 4 is a graph showing the comparison of the catalytic water decomposition of TpPa-1-COF, RP and RP/TpPa-1-COF under visible light (lambda. Gtoreq.420 nm).
Detailed Description
Example 1
Firstly, preparing RP nano-sheets:
dispersing 5g of commercial red phosphorus into 75mL of deionized water, carrying out ultrasonic homogenization, collecting red phosphorus dispersion in the supernatant, carrying out hydrothermal reaction at 200 ℃ for 12h, centrifugally collecting the obtained product, dispersing into 50mL of deionized water, and carrying out ultrasonic treatment for 6h to obtain the RP nano-sheet.
(II) preparing TpPa-1-COF:
grinding 0.021g of trialdehyde phloroglucinol (Tp) and 0.017g of p-phenylenediamine (Pa) for 15min, filling into a 10mL tubular solvent storage bottle, adding 3mL of DMF and 0.5mL of acetic acid solution with the concentration of 3M, carrying out ultrasonic treatment for 30min, freezing by liquid nitrogen, vacuumizing, carrying out solvothermal reaction at 120 ℃ for 72h, collecting a product solid by centrifugation, washing three times by tetrahydrofuran and acetone respectively, and carrying out vacuum drying to obtain TpPa-1-COF.
(III) preparing RP/TpPa-1-COF:
grinding 0.021g of trialdehyde phloroglucinol (Tp) and 0.017g of p-phenylenediamine (Pa) for 15min, adding RP nano-sheets, uniformly mixing, filling into a 10mL tubular solvent storage bottle, respectively adding 3mL DMF and 0.5mL acetic acid solution with the concentration of 3M, carrying out ultrasonic treatment for 30min, freezing by liquid nitrogen, vacuumizing, carrying out solvothermal reaction at 120 ℃ for 72h, collecting a product solid by centrifugation, washing three times by tetrahydrofuran and acetone respectively, and carrying out vacuum drying at 60 ℃ for 12h to obtain RP/TpPa-1-COF.
(IV) detection results
FIG. 1 is a solid ultraviolet-visible diffuse reflectance spectrum of TpPa-1-COF, RP nanoplatelets and RP/TpPa-1-COF composites. As can be seen from FIG. 1, the light response capability of TpPa-1-COF is relatively weak, while the light absorption range of RP is obviously large, and the absorption and utilization of visible light are facilitated after the RP and the TpPa-1-COF are compounded.
FIG. 2 is a transmission electron micrograph of TpPa-1-COF (a), RP (b), and a scanning electron micrograph of RP/TpPa-1-COF (c). As can be seen from fig. 2 (a), tpPa-1-COF exhibits a nanorod structure; as shown in fig. 2 (b), RP is a lamellar sheet structure; as shown in FIG. 2 (c), RP/TpPa-1-COF hybrid materials have been successfully prepared, with RP and TpPa-1-COF being tightly bound together.
Example 2RP/TpPa-1-COF photocatalyst catalyzed hydrolysis to Hydrogen production
The method comprises the following steps: the reaction was carried out in a quartz glass reactor, simulating sunlight using a 300W xenon lamp as a light source. Catalyst RP/TpPa-1-COF (10 mg) was ultrasonically dispersed in 100mL of an aqueous solution of ascorbic acid having a concentration of 5.7mM, chloroplatinic acid solution was added, high-purity nitrogen gas was introduced into the reaction system for 30 minutes to remove oxygen, the reaction system was kept at 5℃by a low-temperature constant-temperature bath, and then reacted under irradiation of visible light (lambda. Gtoreq.420 nm) for 5 hours. The amount of hydrogen generated was measured every 30 minutes during the reaction by gas chromatography. In the reference experiment, RP and TpPa-1-COF are used as catalysts instead of RP/TpPa-1-COF respectively.
FIG. 3 is a schematic diagram of the catalytic hydrolysis of RP/TpPa-1-COF photocatalyst to produce hydrogen under visible light. As shown in the experimental results in FIG. 4, when RP is used as the catalyst, the specific surface area is low, the charge transfer rate is slow, and therefore the hydrogen yield in the reaction for 5 hours is low, namely 34.1 mu mol; when TpPa-1-COF is used as a catalyst, the recombination of electron-hole pairs in the photocatalysis process is serious, and the hydrogen yield in 5 hours is only 84.9 mu mol; when RP/TpPa-1-COF is used as a catalyst, the catalytic activity is obviously improved, the hydrogen yield is linearly increased along with the increase of the reaction time, no activity attenuation is seen in the reaction for 5 hours, and the total hydrogen yield for 5 hours is up to 346.5 mu mol. Therefore, after RP and TpPa-1-COF are compounded to form a heterojunction, the reaction active sites are increased due to the improvement of carrier separation efficiency, the migration rate of charges between material interfaces is accelerated, and the catalytic water decomposition hydrogen release activity of the TpPa-1-COF is improved by about 4.1 times. Therefore, the RP/TpPa-1-COF photocatalyst has higher photocatalytic performance and stability, and the preparation strategy is simple and easy to implement, and has good prospect in the field of photocatalytic water splitting hydrogen production.
Claims (10)
- The RP/TpPa-1-COF photocatalyst is characterized in that the RP/TpPa-1-COF photocatalyst comprises the components of RP, tpPa-1-COF=9:100 according to the mass ratio.
- 2. The method for preparing the RP/TpPa-1-COF photocatalyst according to claim 1, comprising the following steps: fully grinding the trialdehyde phloroglucinol Tp and the p-phenylenediamine Pa, adding the obtained solid and RP nano-sheets into DMF, adding acetic acid solution, carrying out ultrasonic homogenization, carrying out solvothermal reaction, centrifuging the obtained reactant, washing the obtained solid with tetrahydrofuran and acetone respectively, and carrying out vacuum drying to obtain the target product.
- 3. The method of manufacturing according to claim 2, wherein the method of manufacturing RP nanoplatelets comprises the steps of: dispersing 5g of commercial red phosphorus into 75mL of deionized water, carrying out ultrasonic homogenization, collecting red phosphorus dispersion in the supernatant, carrying out hydrothermal reaction at 200 ℃ for 12h, centrifugally collecting the obtained product, then dispersing into 50mL of deionized water, and carrying out ultrasonic treatment for 6h to obtain the RP nano-sheet.
- 4. The method of claim 2, wherein the milling time is 15 minutes.
- 5. The method of claim 2, wherein the concentration of the acetic acid solution is 3M.
- 6. The method of claim 2, wherein the sonication time is 30 minutes.
- 7. The method of claim 2, wherein the solvothermal reaction condition is a reaction at 120 ℃ for 72 hours.
- 8. Use of the RP/TpPa-1-COF photocatalyst of claim 1 as a catalyst in photocatalytic hydrogen production by water splitting.
- 9. Use according to claim 1, characterized in that the method is as follows: dispersing RP/TpPa-1-COF photocatalyst in water solution dissolved with sacrificial agent, adding chloroplatinic acid solution, introducing nitrogen into the solution to remove oxygen, keeping the reaction system at 5 ℃ through a low-temperature constant-temperature tank, and carrying out catalytic reaction under visible light.
- 10. The use according to claim 9, wherein the sacrificial agent is ascorbic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311588416.5A CN117619436A (en) | 2023-11-27 | 2023-11-27 | RP/TpPa-1-COF photocatalyst, preparation method thereof and application thereof in photocatalytic water splitting hydrogen production reaction |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311588416.5A CN117619436A (en) | 2023-11-27 | 2023-11-27 | RP/TpPa-1-COF photocatalyst, preparation method thereof and application thereof in photocatalytic water splitting hydrogen production reaction |
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| CN117619436A true CN117619436A (en) | 2024-03-01 |
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| CN202311588416.5A Pending CN117619436A (en) | 2023-11-27 | 2023-11-27 | RP/TpPa-1-COF photocatalyst, preparation method thereof and application thereof in photocatalytic water splitting hydrogen production reaction |
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