CN109277107B - Transition metal phosphide/red phosphorus photocatalytic material, preparation method and application - Google Patents
Transition metal phosphide/red phosphorus photocatalytic material, preparation method and application Download PDFInfo
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- CN109277107B CN109277107B CN201811105021.4A CN201811105021A CN109277107B CN 109277107 B CN109277107 B CN 109277107B CN 201811105021 A CN201811105021 A CN 201811105021A CN 109277107 B CN109277107 B CN 109277107B
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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
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/185—Phosphorus; Compounds thereof with iron group metals or platinum group metals
- B01J27/1853—Phosphorus; Compounds thereof with iron group metals or platinum group metals with iron, cobalt or nickel
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- 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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- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
- C01B2203/1047—Group VIII metal catalysts
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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
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
- C01B2203/1047—Group VIII metal catalysts
- C01B2203/1052—Nickel or cobalt catalysts
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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
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
- C01B2203/1047—Group VIII metal catalysts
- C01B2203/1052—Nickel or cobalt catalysts
- C01B2203/1058—Nickel catalysts
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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
Abstract
The invention discloses a transition metal phosphide/red phosphorus photocatalytic material, a preparation method and application thereof, wherein the photocatalytic material comprises nanometer red phosphorus and transition metal phosphide growing on the surface of the nanometer red phosphorus; dispersing nano red phosphorus in a transition metal precursor solution, reacting at 100-200 ℃ for 20-60 min, and then carrying out suction filtration on a product to obtain the transition metal phosphide/red phosphorus photocatalytic material, wherein the prepared transition metal phosphide/red phosphorus photocatalytic material is applied to hydrogen production by photolysis of water. The invention skillfully utilizes red phosphorus as a phosphorus source of the transition metal phosphide, and can obtain the transition metal phosphide/red phosphorus nano-composite photocatalytic material by regulating and controlling the reaction degree between the transition metal phosphide and the red phosphorus, the transition metal phosphide and the red phosphorus in the composite material have good contact, the specific surface area of the product is high, more active sites can be provided for the photocatalytic reaction, and the composite material has good electron hole separation performance and hydrogen production performance by photolysis of water.
Description
Technical Field
The invention belongs to the technical field of photocatalytic materials, and particularly relates to a transition metal phosphide/red phosphorus photocatalytic material, a preparation method and application.
Background
Transition Metal Phosphides (TMPs) refer to compounds formed by Transition metal elements (Ni, Co, Fe, Mn, Mo, W, Cu, etc.) and phosphorus elements, have excellent light, heat, acid-base stability and semimetal characteristics, are novel catalytic materials appearing after Transition metal carbides, nitrides and sulfides, and are research hotspots in the fields of photoelectric hydrogen production, catalytic hydrogenation, dehydrogenation, and the like.
At present, Fu Wen Pu, Du Ping Wu et al will treat Ni2P、Co2P、CoP、FeP、Cu3P and CdS, g-C3N4The transition metal phosphide can greatly improve the catalytic activity of a semiconductor, and the hydrogen evolution performance of the transition metal phosphide can be comparable to that of noble metal platinum, so that the transition metal phosphide is paid much attention to the application in the field of photocatalysis. However, in general, when preparing the transition metal phosphide, it is necessary to add a phosphate (such as NaH) to the transition metal ion precursor solution2PO2，NH4H2PO4Etc.), while the preparation of phosphide is carried out by adopting a high-temperature calcination method under the protection of inert gas, the preparation process has harsh conditions and low yield; in addition, most of transition metal phosphide/semiconductor composite systems adopt a mechanical composite method, and the contact between the two is not ideal enough, so that the separation of carriers is not facilitated, and the improvement of the photocatalytic performance is further influenced. Therefore, the invention provides a novel photocatalytic material and a preparation method thereof, and provides a feasible way for improving the photocatalytic activity of red phosphorus.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention provides a transition metal phosphide/red phosphorus photocatalytic material, a preparation method and application thereof, provides a novel photocatalytic material with good performance of photolyzing water to prepare hydrogen, and provides a feasible way for improving the photocatalytic activity of red phosphorus.
In order to achieve the purpose, the invention adopts the following technical scheme:
a transition metal phosphide/red phosphorus photocatalytic material comprises nanometer red phosphorus and transition metal phosphide growing on the surface of the nanometer red phosphorus.
The invention also discloses a preparation method of the transition metal phosphide/red phosphorus photocatalytic material, which comprises the steps of dispersing nano red phosphorus in a transition metal precursor solution, reacting at 100-200 ℃ for 20-60 min, and filtering the product to obtain the transition metal phosphide/red phosphorus photocatalytic material.
Furthermore, the concentration of the transition metal precursor solution is 0.02-0.10 mol/L, and the concentration of the nano red phosphorus is 25-65 g/L.
Further, dispersing the nano red phosphorus in the transition metal precursor solution, stirring for 30-210 min, reacting for 20-60 min at 100-200 ℃ by using a microwave-assisted method, carrying out suction filtration and washing on a product, and drying at 50-70 ℃ to obtain the transition metal phosphide/red phosphorus nanocomposite.
Further, a transition metal soluble salt is dissolved in a solvent to obtain a transition metal precursor solution, wherein the transition metal soluble salt is nitrate or acetate or chloride, and the solvent is a mixed solution of water and ethanol, water and glycol or water and glycerol.
Furthermore, the volume ratio of the water to the ethanol, the water to the glycol or the water to the glycerol is 1: 1-9.
The invention also discloses application of the transition metal phosphide/red phosphorus photocatalytic material in hydrogen production by photolysis of water.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention skillfully utilizes red phosphorus as a phosphorus source of the transition metal phosphide, and can obtain the transition metal phosphide/red phosphorus nano-composite photocatalytic material by regulating and controlling the reaction degree between the transition metal phosphide and the red phosphorus, the transition metal phosphide and the red phosphorus in the composite material have good contact, the specific surface area of the product is high, more active sites can be provided for the photocatalytic reaction, and the composite material has good electron hole separation performance and hydrogen production performance by photolysis of water.
(2) The preparation process of the invention does not need to separately add phosphate and the like, and the preparation method is simple and has low cost; the in-situ growth of the invention is beneficial to establishing a good carrier transmission channel, the separation of the photo-generated electrons and the holes is fast, simultaneously, the interface stability is good, and the compound has good hydrogen production performance by photolysis of water.
Drawings
FIG. 1 is a TEM image of an iron phosphide/red phosphorus sample obtained in example 1.
FIG. 2 is a TEM image of a cobalt phosphide/red phosphorus sample obtained in example 2.
FIG. 3 is a TEM image of a nickel phosphide/red phosphorus sample obtained in example 3, (b) is a partial enlarged view of the I-th part in FIG. (a), and (c) is a partial enlarged view of the II-th part in FIG. (a).
Fig. 4 is an XRD pattern of the samples of example 1 to example 3.
Fig. 5 is a UV-Vis spectrum of the samples of examples 1 to 3.
FIG. 6 is a photolytic hydrogen production spectrum for the sample of example 1.
FIG. 7 is a photolytic hydrogen production spectrum for the sample of example 2.
FIG. 8 is a photolytic hydrogen production spectrum for the sample of example 3.
The invention is described in detail below with reference to the drawings and the detailed description.
Detailed Description
The invention provides a novel photocatalytic material, which enriches the research range of a phosphorus-based photocatalytic material and has important reference significance for the development of an element photocatalyst. The invention discloses a transition metal phosphide/red phosphorus photocatalytic material, which comprises nanometer red phosphorus and transition metal phosphide growing on the surface of the nanometer red phosphorus.
The preparation method of the transition metal phosphide/red phosphorus photocatalytic material comprises the following steps:
step 1: dissolving a transition metal soluble salt in a solvent to obtain a transition metal precursor solution, wherein the transition metal soluble salt is nitrate or acetate or chloride, and the solvent is a mixed solution of water and ethanol, water and glycol or water and glycerol; wherein the volume ratio of water to ethanol, water to glycol or water to glycerol is 1: 1-9.
Step 2: dispersing nano red phosphorus in a transition metal precursor solution, stirring for 30-210 min, reacting at 100-200 ℃ for 20-60 min, carrying out suction filtration and washing on a product, and drying at 50-70 ℃ to obtain a transition metal/red phosphorus nanocomposite; preferably, the solution is transferred to a microwave synthesis tank, and the transition metal phosphide is grown in situ on the surface of the nano red phosphorus by a microwave-assisted method.
Wherein the concentration of the transition metal precursor solution is 0.02-0.10 mol/L, and the concentration of the nano red phosphorus is 25-65 g/L.
The prepared transition metal phosphide/red phosphorus photocatalytic material can be used for hydrogen production by photolysis of water.
The nano red phosphorus in the invention can be prepared by the following method:
under the condition of room temperature, commercially available red phosphorus is put into water to be ground, is sieved by a 120-mesh screen and is dried to obtain micron-sized red phosphorus particles, the micron-sized red phosphorus particles are dispersed in a reaction liquid consisting of water, ethylene glycol and NaOH, are stirred and are then transferred into a hydrothermal synthesis reaction tank with a polytetrafluoroethylene lining, are sealed and are put into an air-blast drying box, are kept at 200 ℃ for 24 hours, are naturally cooled to room temperature after the reaction is finished, and are repeatedly washed by distilled water and absolute ethyl alcohol, centrifuged and dried at 80 ℃ to finally obtain the nano red phosphorus powder. The nano red phosphorus can also be obtained by other existing methods.
The following embodiments of the present invention are provided, and it should be noted that the present invention is not limited to the following embodiments, and all equivalent changes based on the technical solutions of the present invention are within the protection scope of the present invention.
Example 1
Preparing nano red phosphorus: under the condition of room temperature, putting commercially available red phosphorus into water for grinding, sieving by using a 120-mesh sieve, drying to obtain micron-sized red phosphorus particles, weighing 3.0g of red phosphorus particles, dispersing the micron-sized red phosphorus particles into a reaction solution consisting of 55mL of water, 5mL of ethylene glycol and 0.12g of NaOH, stirring for 30min, transferring to a 100mL hydrothermal synthesis reaction tank with a polytetrafluoroethylene lining, sealing, putting into an air-blast drying box, heating to 200 ℃ at the speed of 5 ℃/min, keeping the temperature for 24h, naturally cooling to the room temperature after the reaction is finished, repeatedly washing the product by using distilled water and absolute ethyl alcohol, centrifuging at the speed of 12000rmp/min, and drying at the temperature of 80 ℃ to finally obtain the nano red phosphorus powder.
Preparing a transition metal/red phosphorus nanocomposite material: FeCl is added3·6H2Dissolving O in a mixed solution of 25mL of water and 25mL of glycol, adding the nano red phosphorus after uniform dissolution, and continuously stirring for 210min, wherein the concentration of the transition metal precursor solution is 0.05mol/L, and the concentrations of the nano red phosphorus are 40g/L respectively. And then transferring the reaction liquid to a microwave synthesis tank, heating to 200 ℃ in a microwave reaction system, preserving the temperature for 60min, naturally cooling to room temperature after the reaction is finished, filtering the product by using a 200nm filter membrane, repeatedly washing by using distilled water and ethanol, and drying the solid product at 60 ℃ to obtain the iron phosphide/red phosphorus composite material.
As shown in FIG. 1, the white circle portion is iron phosphide (Fe)2P) particles, wherein RP represents nano red phosphorus, and iron phosphide particles are in good contact with the surface of the red phosphorus; FIG. 4 contains the X-ray powder diffraction pattern of the obtained product, and FIG. 5 shows the ultraviolet-visible absorption spectrum of the obtained sample, and the response performance of the sample in the visible light region can be enhanced by the generated iron phosphide. As can be seen from the attached FIG. 6, the hydrogen production rate by photolysis of water by iron phosphide/red phosphorus is improved by 2.15 times compared with that of a pure red phosphorus sample under visible light.
Example 2
This example differs from example 1 in that: the concentration of the transition metal precursor solution is 0.02mol/L, and the concentration of the nano red phosphorus is 25 g/L.
Compared with the appearance of the iron phosphide/red phosphorus composite material obtained in the embodiment 1, the hydrogen production rate by photolysis of water is improved by 1.95 times compared with that of a pure red phosphorus sample.
Example 3
This example differs from example 1 in that: the concentration of the transition metal precursor solution is 0.10mol/L, and the concentration of the nano red phosphorus is 65 g/L.
Compared with the appearance of the iron phosphide/red phosphorus composite material obtained in the example 1, the hydrogen production rate by photolysis of water is improved by 1.78 times compared with that of a pure red phosphorus sample.
Example 4
Adding Co (NO) at room temperature3)2·6H2O is dispersed in 10mL of water and 40mL of glycerinAnd (3) dissolving the mixed solvent of alcohol uniformly, adding nano red phosphorus, and continuously stirring for 120min, wherein the concentration of the transition metal precursor solution is 0.07mol/L, and the concentration of the nano red phosphorus is 65g/L respectively. And then transferring the reaction liquid to a microwave synthesis tank, heating to 170 ℃ in a microwave reaction system, preserving the temperature for 45min, naturally cooling to room temperature after the reaction is finished, filtering the product by using a 200nm filter membrane, repeatedly washing by using distilled water and ethanol, and drying the solid product at 50 ℃ to obtain the cobalt phosphide/red phosphorus composite material. As can be seen from FIG. 2, a large amount of rod-like cobalt phosphide (Co) uniformly contacted with red phosphorus is uniformly distributed on the surface of red phosphorus2P). FIG. 4 contains the X-ray powder diffraction pattern of the obtained product, and FIG. 5 shows the ultraviolet-visible absorption spectrum of the obtained sample, and the visible generated cobalt phosphide can also enhance the response performance of the sample in the visible light region. As can be seen from FIG. 7, the hydrogen production rate by photolysis of water of the cobalt phosphide/red phosphorus sample is improved by 2.44 times compared with that of the pure red phosphorus sample under visible light.
Example 5
At room temperature, adding NiCl2·6H2Dispersing O in a mixed solvent of 5mL of water and 45mL of ethanol, adding the nano red phosphorus after the O is dissolved uniformly, and continuing stirring for 30min, wherein the concentration of the transition metal precursor solution is 0.10mol/L, and the concentration of the nano red phosphorus is 50 g/L. And then, carrying out suction filtration on the product by using a 200nm filter membrane, repeatedly washing the product by using distilled water and ethanol, and drying the solid product at 70 ℃ to obtain the red-black nickel phosphide/red phosphorus nanocomposite. As shown in FIG. 3, the white circle portion is nickel phosphide (Ni)2P), nickel phosphide particles were distributed on the surface of red phosphorus, and the enlarged view of the lattice spacing thereof corresponded to the dotted line box regions I and II, whereby it could be seen that the exposed crystal face thereof corresponded to the 111 crystal face. FIG. 4 contains the X-ray powder diffraction pattern of the obtained product, and FIG. 5 shows the ultraviolet-visible absorption spectrum of the obtained sample, and the response performance of the sample in the visible light region can be enhanced by the generated cobalt phosphide. As can be seen from FIG. 8, the hydrogen production rate by photolysis of water of the composite sample is improved by 1.89 times compared with that of the pure red phosphorus sample under visible light.
Claims (6)
1. The application of a transition metal phosphide/red phosphorus photocatalytic material in hydrogen production by photolysis of water is characterized in that the photocatalytic material comprises nano red phosphorus and transition metal phosphide growing on the surface of the nano red phosphorus; the transition metal phosphide is iron phosphide or cobalt phosphide or nickel phosphide.
2. The use of the transition metal phosphide/red-phosphorus photocatalytic material as defined in claim 1 in the photolysis of water to produce hydrogen, wherein said transition metal phosphide/red-phosphorus photocatalytic material is prepared by the following method: dispersing the nano red phosphorus in a transition metal precursor solution, reacting at 100-200 ℃ for 20-60 min, and filtering the product to obtain the transition metal phosphide/red phosphorus photocatalytic material.
3. The application of the transition metal phosphide/red phosphorus photocatalytic material in hydrogen production by photolysis of water according to claim 2, wherein the concentration of the transition metal precursor solution is 0.02-0.10 mol/L, and the concentration of nano red phosphorus is 25-65 g/L.
4. The application of the transition metal phosphide/red phosphorus photocatalytic material in hydrogen production by photolysis of water according to claim 2, wherein the preparation method specifically comprises the following steps: dispersing nano red phosphorus in a transition metal precursor solution, stirring for 30-210 min, reacting for 20-60 min at 100-200 ℃ by using a microwave-assisted method, carrying out suction filtration and washing on a product, and drying at 50-70 ℃ to obtain the transition metal phosphide/red phosphorus nanocomposite.
5. The application of the transition metal phosphide/red phosphorus photocatalytic material in the photolysis of water to produce hydrogen as claimed in claim 2, wherein a transition metal precursor solution is obtained by dissolving a transition metal soluble salt in a solvent, wherein the transition metal soluble salt is a nitrate, an acetate or a chloride salt, and the solvent is a mixed solution of water and ethanol, water and ethylene glycol or water and glycerol.
6. The application of the transition metal phosphide/red phosphorus photocatalytic material in hydrogen production by photolysis of water as claimed in claim 5, wherein the volume ratio of water to ethanol, water to ethylene glycol or water to glycerol is 1: 1-9.
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| CN110773208B (en) * | 2019-10-25 | 2021-09-21 | 华南理工大学 | FexP/Cd0.5Zn0.5S photocatalyst and preparation method and application thereof |
| CN110756203B (en) * | 2019-10-25 | 2021-09-21 | 华南理工大学 | Ni2P/Mn0.3Cd0.7S photocatalytic water splitting composite catalyst and preparation method and application thereof |
| CN111036249A (en) * | 2019-12-23 | 2020-04-21 | 华南理工大学 | FexP/Mn0.3Cd0.7S composite photocatalyst and preparation method and application thereof |
| CN112275305A (en) * | 2020-09-17 | 2021-01-29 | 昆明理工大学 | High-efficiency hydrogen evolution catalyst and preparation method thereof |
| CN112619571B (en) * | 2020-11-18 | 2022-06-14 | 东南大学 | Method for regulating and controlling relative exposure strength of crystal face of transition metal phosphide |
| CN112607716B (en) * | 2020-11-30 | 2022-08-12 | 天津大学 | Preparation method of nickel phosphide nanosheet and nickel phosphide nanosheet prepared by same |
| CN113663703B (en) * | 2021-07-19 | 2023-08-01 | 苏州科技大学 | High-selectivity solar-driven carbon dioxide conversion composite material and preparation thereof |
| CN114950502B (en) * | 2022-06-21 | 2024-01-16 | 青岛大学 | Preparation method of nano rod-shaped red phosphorus photocatalyst with photocatalytic hydrogen evolution activity and stability |
| CN115283002B (en) * | 2022-08-25 | 2023-07-14 | 西安交通大学 | Preparation method and application of carbon nitride-nickel phosphide-crystalline red phosphorus composite photocatalyst |
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