CN111841568A - Preparation and application of cuprous oxide loaded Pd composite photocatalytic material for photocatalytic reduction of carbon dioxide - Google Patents
Preparation and application of cuprous oxide loaded Pd composite photocatalytic material for photocatalytic reduction of carbon dioxide Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 46
- 239000000463 material Substances 0.000 title claims abstract description 46
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 41
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 title claims abstract description 36
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229940112669 cuprous oxide Drugs 0.000 title claims abstract description 34
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 30
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 15
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910002094 inorganic tetrachloropalladate Inorganic materials 0.000 claims abstract description 12
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 12
- 239000011591 potassium Substances 0.000 claims abstract description 12
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 9
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 9
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- 239000012467 final product Substances 0.000 claims abstract description 4
- 238000000967 suction filtration Methods 0.000 claims abstract description 4
- 238000001291 vacuum drying Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000006722 reduction reaction Methods 0.000 claims description 39
- 238000007789 sealing Methods 0.000 claims description 6
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 6
- 238000005286 illumination Methods 0.000 claims description 5
- 229910052724 xenon Inorganic materials 0.000 claims description 5
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 235000010265 sodium sulphite Nutrition 0.000 claims description 3
- 229960003280 cupric chloride Drugs 0.000 claims 2
- 238000011049 filling Methods 0.000 claims 1
- 239000010949 copper Substances 0.000 abstract description 25
- 239000011941 photocatalyst Substances 0.000 abstract description 6
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 36
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
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- 238000004627 transmission electron microscopy Methods 0.000 description 3
- 238000004817 gas chromatography Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
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- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 1
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
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- B01J35/39—
-
- 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
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8926—Copper and noble metals
-
- B01J35/393—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
Abstract
The invention belongs to the field of photocatalyst materials, and particularly relates to a preparation method and application of a cuprous oxide loaded Pd composite photocatalytic material for photocatalytic reduction of carbon dioxide. Adding a sodium hydroxide solution into the copper chloride solution, stirring for 30 minutes, adding an ascorbic acid solution, and continuously stirring for 3 hours; then, adding a certain amount of potassium tetrachloropalladate solution, and continuously stirring for reaction for 10-60 minutes, wherein the whole reaction process is carried out under the condition of 55 ℃ water bath; and collecting the final product through suction filtration, and performing vacuum drying to obtain the cuprous oxide loaded Pd composite photocatalytic material for photocatalytic reduction of carbon dioxide. The prepared cuprous oxide loaded Pd composite photocatalytic material can be used for photocatalytic reduction of carbon dioxide. Cu synthesized by the invention2O-Pd composite photocatalysisMaterials for the photocatalytic reduction of CO2The efficiency of the method is more than 3 times of that of single cuprous oxide.
Description
Technical Field
The invention belongs to the field of photocatalyst materials, and particularly relates to a preparation method and application of a cuprous oxide loaded Pd composite photocatalytic material for photocatalytic reduction of carbon dioxide.
Background
Energy crisis and environmental pollution are the common challenges facing the human society at present, and the photocatalytic reduction of CO2The technology is considered as one of the solutions that can solve both of these two problems simultaneously. Currently, semiconductor photocatalysts are widely studied in this field, among which cuprous oxide (Cu)2O) and CO due to its good visible light absorption (forbidden band width 2.2eV)2The multi-selectivity of the reduction products is considered to be an extremely promising photocatalyst. However, the single cuprous oxide photocatalytic material has low carrier mobility, and the photocatalytic activity of the material is limited. Therefore, various cuprous oxide composite photocatalytic materials (such as cuprous oxide-semiconductor, cuprous oxide-metal and the like) are further developed, wherein the cuprous oxide-metal composite photocatalytic material is used for photocatalytic reduction of CO2The performance of the aspect is obviously improved. However, most of the cuprous oxide-metal photocatalytic composite materials are concentrated on cuprous oxide-Au or cuprous oxide-Ag at present, and the cuprous oxide supported palladium composite photocatalytic material is used for photocatalytic reduction of CO2There are few reports. Meanwhile, the prior preparation process of the cuprous oxide-metal composite photocatalytic material is complex or requires environments such as high temperature and high pressure, and the like, so that the production cost and the environmental friendliness are limited to a certain extent.
Existing single cuprous oxide photocatalytic reduction of CO2The efficiency is low, and the cuprous oxide-metal photocatalytic composite material is mainly concentrated on Cu2O-Au or Cu2On O-Ag for the development of Cu2O-Pd composite for CO2Photocatalytic reduction has been rarely reported. In addition, most of the currently adopted preparation methods of the cuprous oxide-metal photocatalytic composite material are complicated in process or require environments such as high temperature and high pressure.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention mainly aims to provide a preparation method of a cuprous oxide loaded Pd composite photocatalytic material for photocatalytic reduction of carbon dioxide. The invention adopts an in-situ reduction method to synthesize the cuprous oxide supported palladium composite photocatalytic material by one step, and the cuprous oxide supported palladium composite photocatalytic material can be used for CO2The photocatalytic reduction efficiency can reach pure cuprous oxideMore than 3 times of the total weight of the composition.
The invention also aims to provide the cuprous oxide loaded Pd composite photocatalytic material prepared by the method.
The invention further aims to provide application of the cuprous oxide loaded Pd composite photocatalytic material in photocatalytic reduction of carbon dioxide.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a cuprous oxide loaded Pd composite photocatalytic material for photocatalytic reduction of carbon dioxide comprises the following steps:
Adding a sodium hydroxide solution into the copper chloride solution, stirring for 30 minutes, adding an ascorbic acid solution, and continuously stirring for 3 hours; then, adding a certain amount of potassium tetrachloropalladate solution and continuously stirring for reaction for 10-60 minutes; the whole reaction process is carried out under the condition of 55 ℃ water bath, the final product is collected by suction filtration and dried in vacuum to prepare the cuprous oxide loaded Pd composite photocatalytic material (Cu) for photocatalytic reduction of carbon dioxide2O-Pd composite photocatalytic material); the concentration of the potassium tetrachloropalladate solution is 15.52mmol/L, and the dosage of the potassium tetrachloropalladate solution is 0.36-5.4 parts by volume.
Preferably, the concentration of the copper chloride solution is 0.01mol/L, the concentration of the sodium hydroxide solution is 2mol/L, and the concentration of the ascorbic acid solution is 0.6 mol/L.
Preferably, the copper chloride solution is used in an amount of 100 parts by volume, the sodium hydroxide solution is used in an amount of 10 parts by volume, and the ascorbic acid solution is used in an amount of 10 parts by volume.
Preferably, the amount of the potassium tetrachloropalladate solution is 3.6 parts by volume.
Preferably, the temperature of the vacuum drying is 50-60 ℃.
The prepared cuprous oxide loaded Pd composite photocatalytic material can be used for photocatalytic reduction of carbon dioxide.
The method comprises the following specific steps of carrying out photocatalytic reduction on carbon dioxide by using the cuprous oxide loaded Pd composite photocatalytic material: the cuprous oxide loaded Pd composite photocatalytic material is dispersed in the containerA container with a sodium sulfite solution, capped, charged into a photocatalytic reduction reaction system (CEL-SPH2N) and sealed; after sealing, the oxygen is removed by a vacuum pump, and then the CO is removed2Introducing through a sealing rubber plug of the reaction system; placing the reaction system under a xenon lamp for illumination after the reaction system is stable.
Preferably, in the above step, the oxygen is removed by a vacuum pump until the vacuum degree of the reaction system is-0.1 MPa, and then CO is introduced2Until the vacuum degree of the reaction system is-0.03 to-0.05 MPa (preferably-0.04 MPa).
Preferably, in the above step, CO is introduced2When the vacuum degree of the reaction system is-0.04 MPa, the reaction system is placed under a 100-one 500W xenon lamp for 30 minutes for illumination.
Compared with the prior art, the invention has the following advantages and beneficial effects:
photocatalytic reduction of CO against single cuprous oxide2Problem of inefficiency, we constructed Cu other than-Au or-Ag2The O-Pd system composite photocatalytic material is synthesized in one step by adopting an in-situ reduction method, the preparation process is simple, a high-temperature and high-pressure environment is not needed, the cost is low, and the environment is friendly.
The invention expands the existing cuprous oxide supported Au or Ag composite photocatalytic material system.
Cu synthesized by the invention2O-Pd composite photocatalytic material for photocatalytic reduction of CO2The efficiency of the method is more than 3 times of that of single cuprous oxide.
Drawings
FIG. 1 shows Cu obtained in example 12XRD pattern of O-0.1 Pd.
FIG. 2 shows Cu obtained in example 12O and Cu2SEM and TEM spectra of O-0.1Pd, wherein: (a) cu2SEM photograph of O, (b) Cu2SEM picture of O-0.1Pd, (c) Cu2TEM image of O, (d) Cu2TEM picture of O-0.1 Pd.
FIG. 3 shows the photocatalytic reduction of CO by Pd supported cuprous oxide composite material2Test results, wherein: (a) cu2Photocatalytic reduction of CO with O loaded with different amounts of Pd respectively2An efficiency map; (b) cu2Photocatalytic reduction of CO by O-0.1Pd2The cycle efficiency map of (1).
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto. The raw materials related to the invention can be directly purchased from the market. For process parameters not specifically noted, reference may be made to conventional techniques.
The materials used in the examples include copper chloride, sodium hydroxide, ascorbic acid, etc., all chemicals being used without further purification.
The material characterization instrument was as follows: transmission Electron Microscopy (TEM), High Resolution TEM (HRTEM) were performed on a 200kV JEM-2100F electron microscope. The crystal structure was determined by a PANalytical X' Pert Powder X-ray diffractometer.
The product was characterized as follows: CO by gas chromatography GC2Reduction of the oxidation product (H)2、CO、CH4、CH3OH、CH3CH2OH) were analyzed.
Example 1
(1)Cu2Preparing an O-Pd composite photocatalytic material: to 100mL of the copper chloride solution (0.01mol/L) was added 10mL of a sodium hydroxide solution (2 mol/L). After stirring for 30 minutes, 10mL of ascorbic acid solution (0.6mol/L) was added and stirring was continued for 3 hours. Subsequently, 0.36mL of a potassium tetrachloropalladate solution (15.52mmol/L) was added and the reaction was stirred for another 10 minutes. The whole reaction process is carried out under the condition of water bath at 55 ℃. Collecting the final product by suction filtration, and drying in a vacuum drying oven at 50 ℃ to obtain Cu with the content of cuprous oxide loaded Pd of 1 w%2An O-Pd composite photocatalytic material.
According to the steps, the Cu loaded with Pd in different proportions is obtained by adding potassium tetrachloropalladate solutions with different volumes2O-Pd composite photocatalytic material: the addition amount of the potassium tetrachloropalladate solution is respectively 0mL, 1.2mL, 1.8mL, 2.9mL, 3.6mL, 4.7mL and 5.4mL, and the composite photocatalytic material with the content of cuprous oxide loaded Pd of 0 w%, 3 w%, 5 w%, 8 w%, 10 w%, 13 w% and 15 w% is obtained respectively. Wherein the amount of Pd supported on the cuprous oxide Is 10 w% (recorded as Cu)2O-0.1Pd) composite material photocatalytic reduction of CO2The efficiency of (2) is highest.
(2) FIG. 1 shows Cu obtained in example 12XRD pattern of O-0.1Pd, XRD pattern shows Cu2The diffraction peak of O-0.1Pd is well matched with the diffraction peak of cuprous oxide (PDF #05-0677) and has no other impurity peak, which shows that Cu2The O-0.1Pd composite photocatalytic material contains Cu2O。
(3) Cu by SEM2The morphology of the O-0.1Pd sample was analyzed, as shown in FIG. 2, Cu2Cu in O-0.1Pd composite photocatalytic material2O is a cube with an edge length of about 2 μm, on which nanoparticles of-10 nm are uniformly loaded. The analysis of the Cu-Cu alloy by TEM shows that the Cu is contained in the alloy2The cubic body in the O-0.1Pd composite photocatalytic material is indeed Cu2O and the nanoparticles are Pd.
(4) Photocatalytic reduction of CO2The experiment of (2): 30mg of a photocatalyst (several photocatalysts having cuprous oxide supported Pd contents of 0 w%, 3 w%, 5 w%, 8 w%, 10 w%, 13 w%, and 15 w%, respectively, were tested) was dispersed in a glass reactor containing 50mL of a sodium sulfite solution (0.01mol/L), and the glass reactor was covered with a quartz plate and then sealed in a photocatalytic reduction reaction system (CEL-SPH 2N). After sealing, deoxidizing by a vacuum pump (till the vacuum degree of the reaction system is-0.1 MPa), and then introducing a certain amount of CO 2(until the vacuum degree of the reaction system is-0.04 MPa). After the reaction system is stable (30 minutes), the reaction system is placed under a 300W xenon lamp for illumination, and products are detected by gas chromatography online sampling at intervals of 1 hour. The detection results are shown in fig. 3 (a).
Photocatalytic reduction of CO by Pd-loaded cuprous oxide composite material2Test results show that the Pd load can effectively improve the photocatalytic reduction of CO of cuprous oxide2Efficiency, and the photocatalytic enhancement efficiency reaches the maximum when the loading of Pd is 10 w%, which is about 3 times of that of pure cuprous oxide. The photocatalytic activity also maintained a certain stability after five cycles, as shown in fig. 3 (b).
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of a cuprous oxide loaded Pd composite photocatalytic material for photocatalytic reduction of carbon dioxide is characterized by comprising the following steps:
adding a sodium hydroxide solution into the copper chloride solution, stirring for 30 minutes, adding an ascorbic acid solution, and continuously stirring for 3 hours; then, adding a certain amount of potassium tetrachloropalladate solution and continuously stirring for reaction for 10-60 minutes; the whole reaction process is carried out under the condition of 55 ℃ water bath, and the final product is collected by suction filtration and dried in vacuum to prepare the cuprous oxide loaded Pd composite photocatalytic material for photocatalytic reduction of carbon dioxide; the concentration of the potassium tetrachloropalladate solution is 15.52mmol/L, and the dosage of the potassium tetrachloropalladate solution is 0.36-5.4 parts by volume.
2. The method for preparing a cuprous oxide-supported Pd composite photocatalytic material for photocatalytic reduction of carbon dioxide according to claim 1, wherein the concentration of the cupric chloride solution is 0.01mol/L, the concentration of the sodium hydroxide solution is 2mol/L, and the concentration of the ascorbic acid solution is 0.6 mol/L.
3. The method for preparing a cuprous oxide-supported Pd composite photocatalytic material for photocatalytic reduction of carbon dioxide according to claim 1, wherein the amount of the cupric chloride solution is 100 parts by volume, the amount of the sodium hydroxide solution is 10 parts by volume, and the amount of the ascorbic acid solution is 10 parts by volume.
4. The method for preparing the cuprous oxide-supported Pd composite photocatalytic material for photocatalytic reduction of carbon dioxide according to claim 1, wherein the amount of the potassium tetrachloropalladate solution is 3.6 parts by volume.
5. The preparation method of the cuprous oxide-supported Pd composite photocatalytic material for photocatalytic reduction of carbon dioxide according to claim 1, wherein the temperature of vacuum drying is 50-60 ℃.
6. A cuprous oxide-supported Pd composite photocatalytic material prepared by the method of any one of claims 1 to 5.
7. The application of the cuprous oxide-supported Pd composite photocatalytic material as claimed in claim 6 in photocatalytic reduction of carbon dioxide.
8. A method for photocatalytic reduction of carbon dioxide is characterized by comprising the following specific steps: dispersing the cuprous oxide-supported Pd composite photocatalytic material as described in claim 7 in a container filled with a sodium sulfite solution, capping the container, filling the container into a photocatalytic reduction reaction system, and sealing the container; after sealing, the oxygen is removed by a vacuum pump, and then the CO is removed2Introducing through a sealing rubber plug of the reaction system; placing the reaction system under a xenon lamp for illumination after the reaction system is stable.
9. The method for photocatalytic reduction of carbon dioxide as claimed in claim 8, wherein the oxygen is removed by vacuum pump to a vacuum degree of-0.1 MPa, and then CO is introduced2Until the vacuum degree of the reaction system is-0.03 to-0.05 MPa.
10. The method of claim 8, wherein the CO is introduced2When the vacuum degree of the reaction system is-0.04 MPa, the reaction system is placed under a 100-one 500W xenon lamp for 30 minutes for illumination.
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| CN113070068A (en) * | 2021-03-29 | 2021-07-06 | 广州大学 | Indium oxide-copper oxide photocatalyst for carbon dioxide reduction and preparation method and application thereof |
| CN113926487A (en) * | 2021-09-14 | 2022-01-14 | 杭州师范大学 | Fullerol/palladium nano composite photocatalyst and preparation method and application thereof |
| CN115463667A (en) * | 2022-08-17 | 2022-12-13 | 广州大学 | Preparation method of composite photocatalytic nitrogen fixation material with different crystal faces of cuprous oxide loaded with iridium |
| CN115595606A (en) * | 2022-09-20 | 2023-01-13 | 山东大学（Cn） | Copper-based catalytic electrode, preparation method and application thereof in preparing ethylene by electrocatalytic reduction of carbon dioxide |
| CN116422378A (en) * | 2023-03-24 | 2023-07-14 | 大连理工大学 | Cu (copper) alloy 2 O-CuXbpy composite material CO 2 Preparation method and application of photoreduction catalyst |
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| YANFANG LI,ET AL: "Octahedral Cu2O-modified TiO2 nanotube arrays for efficient photocatalytic reduction of CO2", 《CHINESE JOURNAL OF CATALYSIS》 * |
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| CN115595606A (en) * | 2022-09-20 | 2023-01-13 | 山东大学（Cn） | Copper-based catalytic electrode, preparation method and application thereof in preparing ethylene by electrocatalytic reduction of carbon dioxide |
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