CN116371423A - Mn with leaf petal-shaped three-dimensional dendritic structure x Cd 1-x Preparation method and application of S photocatalyst - Google Patents
Mn with leaf petal-shaped three-dimensional dendritic structure x Cd 1-x Preparation method and application of S photocatalyst Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 17
- 125000000896 monocarboxylic acid group Chemical group 0.000 claims abstract description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 12
- 239000001257 hydrogen Substances 0.000 claims abstract description 12
- 230000001699 photocatalysis Effects 0.000 claims abstract description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 4
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 3
- 239000012295 chemical reaction liquid Substances 0.000 abstract 1
- 239000011572 manganese Substances 0.000 description 45
- 239000000243 solution Substances 0.000 description 15
- 239000000047 product Substances 0.000 description 8
- 239000006104 solid solution Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002073 nanorod Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000000851 scanning transmission electron micrograph Methods 0.000 description 2
- 230000010757 Reduction Activity Effects 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001661 cadmium Chemical class 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 150000002696 manganese Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
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- B01J35/39—
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
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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
- 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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Abstract
The invention discloses Mn with a leaf petal-shaped three-dimensional dendritic structure x Cd 1‑x Preparation method and application of S photocatalyst, and Mn (COOH) 2 ·4H 2 O、CdCl 2 ·2.5H 2 O and thiourea were placed in deionized water, wherein Mn (COOH) 2 With CdCl 2 The molar ratio is 1:9, 3:7 or 5:5, and the reaction solution is obtained after stirring, dissolving and reacting for 2 hours at room temperature, wherein CdCl in the reaction solution is obtained 2 The concentration of (2) is 0.1mol/L, and the concentration of thiourea is 0.08mol/L; pouring the obtained reaction liquid into a reaction kettle with a polytetrafluoroethylene lining, and performing hydrothermal reaction for 15h at 150 ℃; centrifugally separating, washing and drying the solid in the reaction product to obtain Mn with a leaf petal-shaped three-dimensional dendritic structure x Cd 1‑x S photo-catalyst; mn with leaf petal-shaped three-dimensional dendritic structure of the invention x Cd 1‑x The S photocatalyst is applied to photocatalytic hydrogen production reaction and has higher photocatalytic hydrogen production performance.
Description
Technical Field
The invention relates to the technical field of catalyst preparation, in particular to Mn with a leaf petal-shaped three-dimensional dendritic structure x Cd 1-x A preparation method and application of an S photocatalyst.
Background
Mn x Cd 1-x S is a novel non-stoichiometric photocatalytic materialThe solar energy collector has the unique properties of an easily-adjusted structure, a narrower band gap, a more suitable conduction band edge and the like, and can realize the effective utilization of sunlight. Mn (Mn) x Cd 1-x S solid solutions are suitable for photocatalytic hydrogen evolution reactions under visible light because of having a medium band gap energy (2.1-2.4 eV) and deeper negative conduction band edge sites (more negative than CdS).
It is well known that the size and morphology of semiconductor photocatalysts have a significant impact on their performance. However, at present, mn is regulated x Cd 1-x S morphology to improve its photocatalytic performance has been rarely studied. So far, researchers have successfully prepared Mn with different morphologies x Cd 1-x S, mainly comprises nano particles, nano rods, three-dimensional flowers and the like. Nanoparticles and one-dimensional nanorod Mn compared to zero-dimensional x Cd 1-x S, three-dimensional Mn x Cd 1-x S has the advantages of expanding the visible light response range, improving the photoinduced carrier separation efficiency, expanding the synergistic effect between the specific surface areas and the like, so that the hydrogen evolution performance is remarkably enhanced.
Chinese patent application No. CN202110697833.8 discloses an organic-inorganic hybrid Mn x Cd 1-x The preparation method of the S solid solution photocatalyst comprises the following steps: (1) Firstly, adding cadmium salt and manganese salt into a beaker, adding deionized water, and stirring until the solution A is transparent; (2) Putting a sulfur compound into a reaction kettle, then adding an amine organic solution, and uniformly stirring to obtain a solution B; (3) Dropwise adding the solution A into a reaction kettle while stirring the obtained solution B, continuously stirring the solution, finally placing the reaction kettle into an oven, carrying out heat preservation reaction, washing, centrifuging and drying after the reaction is finished to obtain a target product; the prepared MnxCd1-xS solid solution has a sea-tangle star-shaped structure, has higher photocatalytic performance and stability compared with pure CdS and MnS, and has high photocatalytic carbon dioxide reduction activity, but does not disclose photocatalytic hydrogen production performance.
Disclosure of Invention
In order to solve the technical problems, the invention provides Mn with a leaf petal-shaped three-dimensional dendritic structure x Cd 1-x S photo-catalysisA preparation method and application of the agent.
In order to achieve the above purpose, the invention is implemented according to the following technical scheme:
the first object of the present invention is to provide Mn having a leaf-petal-shaped three-dimensional dendritic structure x Cd 1-x The preparation method of the S photocatalyst comprises the following steps:
s1, mn (COOH) 2 ·4H 2 O、CdCl 2 ·2.5H 2 O and thiourea were placed in deionized water, wherein Mn (COOH) 2 With CdCl 2 The molar ratio is 1:9, 3:7 or 5:5, and the reaction solution is obtained after stirring, dissolving and reacting for 2 hours at room temperature, wherein CdCl in the reaction solution is obtained 2 The concentration of (2) is 0.1mol/L, and the concentration of thiourea is 0.08mol/L;
s2, pouring the reaction solution obtained in the step S1 into a reaction kettle with a polytetrafluoroethylene lining, and performing hydrothermal reaction for 15h at 150 ℃;
s3, centrifugally separating, washing and drying the solid in the reaction product of the step S2 to obtain Mn with a leaf petal-shaped three-dimensional dendritic structure x Cd 1-x S photocatalyst.
Further, in the step S3, the centrifugal revolution is 1000r/min, the drying temperature is 60 ℃, and the drying time is 6-12 h.
A second object of the present invention is to provide Mn having a leaf-petal-shaped three-dimensional dendritic structure prepared by the above method x Cd 1-x S photocatalyst.
A third object of the present invention is to provide Mn having a leaf-petal-shaped three-dimensional dendritic structure x Cd 1-x The application of the S photocatalyst in photocatalytic hydrogen production.
Compared with the prior art, the invention prepares Mn x Cd 1-x The S photocatalyst has special appearance and is Mn for synthesizing a three-dimensional dendritic structure x Cd 1-x The S photocatalyst provides a new method, and the preparation method is simple, low in cost, good in safety and strong in practicability, does not use any surfactant or template in the preparation process, and adopts one-step simple hydrothermal synthesis to prepare the three-dimensional dendritic Mn with leaf petals x Cd 1-x S nano structure, thiourea can be used as a sulfur source and a bidentate ligand to form a Mn-Cd-thiourea stable system, and S is slowly released 2- Reaction to produce Mn x Cd 1-x S nuclei, which preferentially grow to form rod-like Mn x Cd 1-x S crystal. Subsequently, anisotropic growth results in the formation of dendrite structures. Mn of the prepared leaf petal-shaped three-dimensional dendritic structure x Cd 1-x The S photocatalyst has the advantages of high product purity, stability and the like, and has higher photocatalytic hydrogen production performance.
Drawings
FIG. 1 shows Mn of the three-dimensional dendritic structure having leaf rosettes obtained in example 1 of the present invention 0.3 Cd 0.7 XRD pattern of S photocatalyst;
FIG. 2, panel (A), shows the product Mn obtained in example 2 0.1 Cd 0.9 SEM image of S photocatalyst, and image (B) is the product Mn obtained in example 1 0.3 Cd 0.7 STEM image and element map of S photocatalyst.
FIG. 3 shows Mn of the three-dimensional dendritic structure having leaf rosettes obtained in example 1 0.3 Cd 0.7 Hydrogen production curve of S photocatalyst.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. The specific embodiments described herein are for purposes of illustration only and are not intended to limit the invention.
Example 1
1) 2.143mmol Mn (COOH) 2 ·4H 2 O、5mmol CdCl 2 ·2.5H 2 O and 4mmol thiourea were dissolved and reacted at room temperature in 50mL deionized water for 2h with Mn (COOH) 2 ·4H 2 O is added in such an amount that Mn (COOH) 2 With CdCl 2 The molar ratio is 3:7;
2) Pouring the reaction solution obtained in the step 1) into a reaction kettle with a polytetrafluoroethylene lining, and reacting for 15 hours at 150 ℃;
3) Centrifuging, washing and drying the solid obtained by the reaction in the step 2) to obtain the product with the following characteristicsMn of leaf petal-shaped three-dimensional dendritic structure 0.3 Cd 0.7 S photocatalyst. Centrifugal revolution: 1000r/min, the drying temperature is 60 ℃, and the drying time is 6h.
Example 2
1) Will be 0.56mmol Mn (COOH) 2 ·4H 2 O、5mmol CdCl 2 ·2.5H 2 O and 4mmol thiourea were dissolved and reacted at room temperature in 50mL deionized water for 2h with Mn (COOH) 2 ·4H 2 O is added in such an amount that Mn (COOH) 2 With CdCl 2 The molar ratio is 1:9;
2) Pouring the reaction solution obtained in the step 1) into a reaction kettle with a polytetrafluoroethylene lining, and reacting for 15 hours at 150 ℃;
3) Centrifugally separating, washing and drying the solid obtained by the reaction in the step 2) to obtain Mn with a leaf petal-shaped three-dimensional dendritic structure 0.1 Cd 0.9 S photocatalyst. Centrifugal revolution: 1000r/min, the drying temperature is 60 ℃, and the drying time is 6h.
Example 3
1) 5mmol Mn (COOH) 2 ·4H 2 O、5mmol CdCl 2 ·2.5H 2 O and 4mmol thiourea were dissolved and reacted at room temperature in 50mL deionized water for 2h with Mn (COOH) 2 ·4H 2 O is added in such an amount that Mn (COOH) 2 With CdCl 2 The molar ratio is 5:5;
2) Pouring the reaction solution obtained in the step 1) into a reaction kettle with a polytetrafluoroethylene lining, and reacting for 15 hours at 150 ℃;
3) Centrifugally separating, washing and drying the solid obtained by the reaction in the step 2) to obtain Mn with a leaf petal-shaped three-dimensional dendritic structure 0.5 Cd 0.5 S photocatalyst. Centrifugal revolution: 1000r/min, the drying temperature is 60 ℃, and the drying time is 6h.
FIG. 1 shows the product Mn obtained in example 1 0.3 Cd 0.7 The XRD pattern of the S photocatalyst was Mn at 2θ=24.99 °, 26.74 °, 28.37 °, 36.81 °, 43.91 °, 48.05 °, 51.09 °, 52.06 °, 53.00 °, 54.81 °, 58.51 °, 67.01 °, 69.54 °, 71.13 °, 72.61 °, 75.79 °, 80.51 °, 83.61 ° x Cd 1-x S feature diffractionThe peak has no other miscellaneous peaks, has higher purity, is consistent with the report of the literature, and shows Mn x Cd 1-x S is successfully prepared.
FIG. 2, panel (A), shows the product Mn obtained in example 2 0.1 Cd 0.9 SEM image of S photocatalyst, it can be clearly observed in fig. 2 (a) that the catalyst consists of a number of dendritic structures with leaf lengths of 2-3 μm. FIG. 2 (B) shows the product Mn obtained in example 1 0.3 Cd 0.7 STEM image and element map of S photocatalyst, in the spectrum of each element, it can be observed that each element is uniformly distributed in Mn x Cd 1-x S surface.
Application instance
Mn of the three-dimensional dendritic structure having leaf rosettes obtained in example 1 0.3 Cd 0.7 S photocatalyst is put into 0.1MNA 2 S、0.3MNa 2 SO 3 Hydrogen production was performed in a sacrificial solution with a promoter Pt loading of 1.5 wt%.
FIG. 3 shows Mn of the three-dimensional dendritic structure having leaf rosettes obtained in example 1 0.3 Cd 0.7 S photocatalyst in 0.1MNA 2 S、0.3MNa 2 SO 3 The hydrogen production curve in the sacrificial solution and with a Pt loading of 1.5wt% promoter, as can be seen from fig. 3, illustrates the Mn prepared according to the present invention x Cd 1-x The S photocatalyst has good photocatalytic hydrogen production activity.
The technical scheme of the invention is not limited to the specific embodiment, and all technical modifications made according to the technical scheme of the invention fall within the protection scope of the invention.
Claims (4)
1. Mn with leaf petal-shaped three-dimensional dendritic structure x Cd 1-x The preparation method of the S photocatalyst is characterized by comprising the following steps:
s1, mn (COOH) 2 ·4H 2 O、CdCl 2 ·2.5H 2 O and thiourea were placed in deionized water, wherein Mn (COOH) 2 With CdCl 2 The molar ratio is 1:9, 3:7 or 5:5, and the reaction solution is obtained after stirring, dissolving and reacting for 2 hours at room temperature, wherein Cd in the reaction solution is obtainedCl 2 The concentration of (2) is 0.1mol/L, and the concentration of thiourea is 0.08mol/L;
s2, pouring the reaction solution obtained in the step S1 into a reaction kettle with a polytetrafluoroethylene lining, and performing hydrothermal reaction for 15h at 150 ℃;
s3, centrifugally separating, washing and drying the solid in the reaction product of the step S2 to obtain Mn with a leaf petal-shaped three-dimensional dendritic structure x Cd 1-x S photocatalyst.
2. Mn with leaf-petal-shaped three-dimensional dendritic structure according to claim 1 x Cd 1-x The preparation method of the S photocatalyst is characterized in that in the step S3, the centrifugal revolution is 1000r/min, the drying temperature is 60 ℃, and the drying time is 6-12 h.
3. Mn with leaf-petal-shaped three-dimensional dendritic structure prepared by the method of claim 1 or 2 x Cd 1-x S photocatalyst.
4. A Mn with a leaf-petal-shaped three-dimensional dendritic structure according to claim 3 x Cd 1-x The application of the S photocatalyst in photocatalytic hydrogen production.
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