CN114471640A - Controllable preparation of composite crystal three-dimensional dendritic red phosphorus elementary substance photocatalyst and application of composite crystal three-dimensional dendritic red phosphorus elementary substance photocatalyst in water decomposition hydrogen production - Google Patents
Controllable preparation of composite crystal three-dimensional dendritic red phosphorus elementary substance photocatalyst and application of composite crystal three-dimensional dendritic red phosphorus elementary substance photocatalyst in water decomposition hydrogen production Download PDFInfo
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- CN114471640A CN114471640A CN202111669723.7A CN202111669723A CN114471640A CN 114471640 A CN114471640 A CN 114471640A CN 202111669723 A CN202111669723 A CN 202111669723A CN 114471640 A CN114471640 A CN 114471640A
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 42
- 239000013078 crystal Substances 0.000 title claims abstract description 37
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 34
- 239000001257 hydrogen Substances 0.000 title claims abstract description 34
- 239000000126 substance Substances 0.000 title claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 239000002131 composite material Substances 0.000 title claims abstract description 16
- 238000000354 decomposition reaction Methods 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 title abstract description 27
- 229910052751 metal Inorganic materials 0.000 claims abstract description 12
- 239000002184 metal Substances 0.000 claims abstract description 12
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 11
- 239000000835 fiber Substances 0.000 claims abstract description 7
- 239000002073 nanorod Substances 0.000 claims abstract description 7
- 239000002070 nanowire Substances 0.000 claims abstract description 7
- 230000001699 photocatalysis Effects 0.000 claims description 24
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 3
- 239000003708 ampul Substances 0.000 claims description 3
- 239000006227 byproduct Substances 0.000 claims description 3
- 230000003247 decreasing effect Effects 0.000 claims description 3
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000003837 high-temperature calcination Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 2
- 239000003054 catalyst Substances 0.000 abstract description 4
- 229910052797 bismuth Inorganic materials 0.000 abstract description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 13
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000003756 stirring Methods 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
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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
- 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
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
-
- B01J35/23—
-
- B01J35/39—
-
- 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
-
- 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 controllable preparation of the composite crystal three-dimensional dendritic red phosphorus single-substance photocatalyst and the application of water decomposition to hydrogen production belong to the technical field of catalysts. By adopting a controllable preparation process of Chemical Vapor Deposition (CVD), amorphous Red Phosphorus (RP) is taken as a precursor, and a three-dimensional dendritic red phosphorus elementary substance photocatalyst (DRP) with a composite crystal structure is successfully prepared in the presence of a metal bismuth (Bi) cocatalyst. The DRP photocatalyst consists of an RP nano-wire (main stem) with a Hittorf crystal form and an RP nano-rod (branch) with a fiber crystal form, so that a heterojunction structure with a composite crystal form is constructed, and separation and transfer of photo-generated charges are facilitated. The DRP elementary substance photocatalyst shows excellent hydrogen production performance by visible light water decomposition (1027 mu mol h)‑1 g‑1) And stability.
Description
Technical Field
The invention relates to a three-dimensional dendritic red phosphorus elementary substance photocatalyst (DRP) with a composite crystal structure, which has excellent photocatalytic water decomposition hydrogen production performance. Firstly, purifying commercial Red Phosphorus (RP) by a hydrothermal method; a preparation process of Chemical Vapor Deposition (CVD) is adopted, purified amorphous RP is used as a P source, metal bismuth (Bi) is used as a cocatalyst, and a series of DRP elementary substance photocatalysts are prepared by regulating and controlling the mass ratio of RP to Bi. Among them, DRP (Bi: RP ═ 1:2) exhibits the highest visible light photocatalytic hydrogen production performance and stability.
Background
The hydrogen energy has the advantages of high energy density, safety, environmental protection, recycling and the like, and is considered to be a green new energy source which can replace the traditional fossil fuel. The photocatalytic water splitting technology is an ideal strategy for preparing hydrogen energy, and the core and key of the technology is the research and development of efficient photocatalysts. Although many photocatalysts with excellent performance have been developed, most photocatalytic materials have excessively complicated systems and compositions. Therefore, the development of a simple and efficient photocatalyst may be a better strategy.
The RP is the simplest novel simple substance photocatalyst, has the advantages of adjustable energy level structure, wide visible light response range, low price, easy obtainment and the like, and has good application prospect in the field of hydrogen production by photocatalytic water decomposition. Researches show that the regulation and control of the morphology and the crystal structure are one of important strategies for improving the hydrogen production activity of RP photocatalysis. For example, RPs of various morphologies have been developed, such as nanoparticles (phys. chem. phys.,2016,18,3921), nanorods (nanoscales, 2014,6,14163), nanosheets (mater. lett.,2019,236,542), nanowires (angelw. chem. int.ed.,2009,48,3616), and nanobelts (appl. catal.b,2019,247,100), which further enhance the applicability of the RP in the field of photocatalysis; hu et al prepared RP of fiber crystal form by CVD method, and the hydrogen production efficiency reaches 684 mu mol h-1g-1The record of the hydrogen production activity of the current elemental semiconductor photocatalyst is the highest record (Angew. chem. int. Ed.2019,55,9580).
Based on the basic strategy of regulating and controlling the morphology and the crystal structure and inspired by Ren et al mechanism (Science,1998,282,1105) of inducing the growth of Carbon Nanotubes (CNT) on the surface of Ni by using a CVD method, the invention adopts a strategy of regulating and controlling the morphology and the crystal structure of RP by using metal Bi as a cocatalyst so as to further improve the photocatalytic water decomposition hydrogen production activity. The invention prepares the three-dimensional dendritic DRP elementary substance photocatalyst with a composite crystal structure by taking purified commercial RP as a P source and adopting a CVD method in the presence of a metal Bi cocatalyst. By adjusting the mass ratio of metal Bi to the RP precursor (Bi: RP is 1:0.5, 1:1, 1:2 and 1:4), the effective regulation and control of the shape and the crystal structure of the DRP are realized. Research shows that when the current driver mass ratio Bi to RP is 1 to 2, the prepared DRP single substance photocatalyst has the highest hydrogen production activity. The invention discloses a preparation method of the DRP photocatalyst.
Disclosure of Invention
The invention adopts a CVD method and takes metal Bi as a cocatalyst to successfully prepare the DRP elementary substance photocatalyst. The dendritic structure of the catalyst consists of an RP nanowire (main stem) with a Hittorf crystal form and an RP nanorod (branch) with a fiber crystal form, so that a heterojunction structure with a composite crystal form is constructed, separation and migration of photo-generated charges are effectively promoted, and the activity of hydrogen generated by photocatalytic decomposition of water is further improved.
The composite crystal form three-dimensional dendritic red phosphorus elementary substance photocatalyst is characterized by comprising two crystal form red phosphorus elementary substances, wherein the DRP elementary substance photocatalyst is a DRP elementary substance photocatalyst, the structure shape is a dendritic structure, the main trunk of the corresponding dendritic structure is an RP nanowire in a Hittorf crystal form, and the branch is an RP nanorod in a fiber crystal form.
The preparation method of the composite crystal form three-dimensional dendritic red phosphorus elementary substance photocatalyst is characterized by comprising the following steps of:
(1) purifying the commercial RP by a hydrothermal method to remove impurities on the surface of the RP;
(2) preparing a DRP photocatalyst by adopting a CVD method: uniformly mixing purified RP and metal Bi powder, tabletting, putting into a quartz ampoule bottle, vacuumizing, and sealing with acetylene flame; and (3) calcining the mixture at high temperature in a tubular furnace, and after the temperature is gradually reduced to room temperature, sequentially carrying out ultrasonic treatment, centrifugation and washing on the prepared sample to remove surface by-products and metal Bi, thereby finally obtaining the pure DRP elementary substance photocatalyst.
In the step (2), the mass ratio of Bi to RP is 1:1 to 1:4, preferably 1: 2.
High temperature calcination refers to: at 5 ℃ for min-1The temperature is increased to 580 ℃ at the speed rate, and the temperature is kept for 2 hours; then 0.1 DEG C
min-1The temperature is reduced to 300 ℃; finally at 1 deg.C for min-1The rate of (2) is decreased to room temperature.
The application of the composite crystal form three-dimensional dendritic red phosphorus single substance photocatalyst is used for photocatalytic water decomposition hydrogen production, the DRP photocatalyst is dispersed in distilled water containing methanol, Pt is added as a cocatalyst, and visible light is used as a light source to perform photocatalytic water decomposition hydrogen production.
The specific operation steps of the evaluation of the photocatalytic water splitting hydrogen production performance of the prepared DRP photocatalyst are as follows: 50mg of DRP photocatalyst was dispersed in 100mL of distilled water containing 10 vol% methanol, and 1 wt% Pt was added as a co-catalyst. The photocatalytic hydrogen evolution experiment adopts a y-shaped reaction tank connected with a cooling system and a closed gas circulation/discharge system, adopts a 300W xenon lamp provided with an L40 filter as a visible light source, and adopts a GC7900 gas chromatograph to detect the content of hydrogen generated by the photocatalytic reaction.
The invention has the advantages of cheap and easily obtained raw materials, simple and convenient preparation process flow, controllable product appearance and crystal form, and good photocatalytic hydrogen production activity under the irradiation of visible light. Wherein, DRP (Bi: RP is 1:2) has the highest hydrogen production activity which reaches 1027 mu mol h-1g-113 times that of commercial RP. The catalyst shows good photocatalytic hydrogen production stability after being subjected to a photocatalytic hydrogen production activity test for 20 continuous hours.
Drawings
As shown in fig. 1, the XRD spectrum of the prepared sample is shown. Curves (a), (b), (c), (d), (e), and (f) are, in order, commercially amorphous RP, RP nanowires in a Hittorf crystal form (Bi: RP ═ 1:0.5), DRP (Bi: RP ═ 1:1), DRP (Bi: RP ═ 1:2), DRP (Bi: RP ═ 1:4), and RP nanorods in a fiber crystal form (without Bi).
As shown in fig. 2, the SEM spectrum of the prepared sample is shown. Wherein curves (a), (b), (c), (d), (e), and (f) are commercially amorphous RP, Hittorf crystal form RP nanowires (Bi: RP ═ 1:0.5), DRP (Bi: RP ═ 1:1), DRP (Bi: RP ═ 1:2), DRP (Bi: RP ═ 1:4), and fiber crystal form RP nanorods (without Bi participating), respectively.
As shown in fig. 3, the hydrogen production activity of the prepared sample by photocatalytic water decomposition under visible light is shown. The prepared DRP photocatalyst shows excellent photocatalytic hydrogen production performance, wherein the photocatalytic hydrogen production activity of DRP (Bi: RP is 1:2) reaches 1027 mu mol h-1g-113 times that of commercial RP.
As shown in fig. 4, it is a photocatalytic hydrogen production stability test chart of DRP (Bi: RP ═ 1:2) photocatalyst. After the photocatalytic hydrogen production activity test is carried out for 20 continuous hours, the hydrogen production activity is found not to be obviously reduced, and the catalyst has good photocatalytic hydrogen production stability.
Detailed Description
The invention is illustrated in more detail by the following examples, the resulting DRP photocatalyst being illustrated by the accompanying drawings.
Example 1: purification of commercial RP. Weighing 2g of commercial RP, placing the RP into a beaker, adding 60mL of distilled water, and magnetically stirring for 1 hour; putting the solution into a polytetrafluoroethylene-lined high-pressure reaction kettle (100mL), and heating in an oven at 200 ℃ for 12 hours; centrifuging, washing and drying to obtain the purified RP.
Example 2: preparation of DRP photocatalyst (CVD method). Weighing 200mg of purified commercial RP, respectively and uniformly mixing with metal Bi (50, 100, 200 and 400mg) with different masses, tabletting, respectively placing into different quartz ampoules, vacuumizing and sealing by acetylene flame; placing quartz ampoule bottle into tube furnace, and heating at 5 deg.C for min-1The temperature is increased to 580 ℃ at the speed rate, and the temperature is kept for 2 hours; then at 0.1 deg.C for min-1The temperature is reduced to 300 ℃; finally at 1 deg.C for min-1The rate of (2) is decreased to room temperature. The sample was removed and washed with carbon disulfide (CS)2) Washing with distilled water for several times to remove by-products; carrying out ultrasonic treatment on the sample aqueous solution for 2h, and standing for 1h to remove black precipitates (metal Bi); centrifuging and drying to obtain the final product DRP photocatalyst.
The raw materials used by the invention are cheap and easy to obtain, the preparation process is simple, and the effective regulation and control of the crystal form and the morphology of the product can be realized. The prepared DRP (Bi: RP ═ 1:2) has the most excellent hydrogen production activity by decomposing water under visible light.
Claims (6)
1. The composite crystal form three-dimensional dendritic red phosphorus elementary substance photocatalyst is characterized by being a DRP elementary substance photocatalyst for short, two crystal form red phosphorus elementary substances are contained in the DRP elementary substance photocatalyst, the structure shape is a dendritic structure, the main trunk of the corresponding dendritic structure is an RP nano-wire with a Hittorf crystal form, and the branch is an RP nano-rod with a fiber crystal form.
2. The preparation method of the composite crystal form three-dimensional dendritic red phosphorus elementary substance photocatalyst according to claim 1, characterized by comprising the following steps:
(1) purifying the commercial RP by a hydrothermal method to remove impurities on the surface of the RP;
(2) preparing a DRP photocatalyst by adopting a CVD method: uniformly mixing purified RP and metal Bi powder, tabletting, putting into a quartz ampoule bottle, vacuumizing, and sealing with acetylene flame; calcining the mixture at high temperature in a tubular furnace, and after the temperature is gradually reduced to room temperature, sequentially carrying out ultrasonic treatment, centrifugation and washing on the prepared sample to remove surface byproducts and metal Bi, thereby finally obtaining the pure DRP elementary substance photocatalyst.
In the step (2), the mass ratio of Bi to RP is 1:1 to 1: 4.
3. The method of claim 2, wherein the mass ratio of Bi to RP is 1: 2.
4. The method of claim 2, wherein the high temperature calcination refers to: at 5 ℃ for min-1The temperature is increased to 580 ℃ at the speed rate, and the temperature is kept for 2 hours; then at 0.1 deg.C for min-1The temperature is reduced to 300 ℃; finally at 1 deg.C for min-1The rate of (2) is decreased to room temperature.
5. The application of the composite crystal form three-dimensional dendritic red phosphorus elementary substance photocatalyst disclosed by claim 1 in photocatalytic water decomposition to produce hydrogen.
6. The use of claim 5, wherein the DRP photocatalyst is dispersed in distilled water containing methanol, Pt is added as a promoter, and visible light is used as a light source to carry out photocatalytic water splitting to produce hydrogen.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105642321A (en) * | 2015-12-31 | 2016-06-08 | 青岛科技大学 | Nano red phosphorus/graphene composite photocatalyst and preparation method thereof |
| CN112774703A (en) * | 2021-02-01 | 2021-05-11 | 北京工业大学 | Elemental red phosphorus-loaded titanium dioxide composite catalyst for efficient photocatalytic decomposition of water to produce hydrogen |
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- 2021-12-31 CN CN202111669723.7A patent/CN114471640B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105642321A (en) * | 2015-12-31 | 2016-06-08 | 青岛科技大学 | Nano red phosphorus/graphene composite photocatalyst and preparation method thereof |
| CN112774703A (en) * | 2021-02-01 | 2021-05-11 | 北京工业大学 | Elemental red phosphorus-loaded titanium dioxide composite catalyst for efficient photocatalytic decomposition of water to produce hydrogen |
Non-Patent Citations (1)
| Title |
|---|
| YANG LIU，ET AL: ""Liquid bismuth initiated growth of phosphorus microbelts with efficient charge polarization for photocatalysis"", 《APPLIED CATALYSIS B: ENVIRONMENTAL》, pages 100 - 106 * |
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