CN114471640B - Controllable preparation of compound crystal form three-dimensional dendritic red phosphorus single-substance photocatalyst and application of compound crystal form three-dimensional dendritic red phosphorus single-substance photocatalyst in hydrogen production by water splitting - Google Patents
Controllable preparation of compound crystal form three-dimensional dendritic red phosphorus single-substance photocatalyst and application of compound crystal form three-dimensional dendritic red phosphorus single-substance photocatalyst in hydrogen production by water splitting Download PDFInfo
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 43
- 239000013078 crystal Substances 0.000 title claims abstract description 39
- 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 29
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 150000001875 compounds Chemical class 0.000 title claims description 7
- 239000002131 composite material 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 25
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 102000020897 Formins Human genes 0.000 claims description 8
- 108091022623 Formins Proteins 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 5
- 239000003708 ampul Substances 0.000 claims description 4
- 238000000354 decomposition reaction Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 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
- 239000006227 byproduct Substances 0.000 claims description 3
- 238000001816 cooling Methods 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 8
- 239000002243 precursor Substances 0.000 abstract description 3
- 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
- 238000000926 separation method Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development 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
- 239000000047 product Substances 0.000 description 2
- 238000000746 purification Methods 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
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 230000001276 controlling effect Effects 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
- 238000011049 filling Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000002803 fossil fuel Substances 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
- 150000002739 metals Chemical class 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000005303 weighing 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
Classifications
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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
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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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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- Engineering & Computer Science (AREA)
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Abstract
The controllable preparation of composite crystal form three-dimensional dendritic red phosphorus single-substance photocatalyst and the application of water-splitting 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 used as a precursor, and a three-dimensional dendritic red phosphorus simple substance photocatalyst (DRP) with a composite crystal structure is successfully prepared under the participation of a metallic bismuth (Bi) cocatalyst. The DRP photocatalyst consists of RP nanowires ("trunks") of Hittorf crystal forms and RP nanorods ("branches") of fiber crystal forms, so that a heterojunction structure with a composite crystal form is constructed, and separation and transfer of photo-generated charges are facilitated. The DRP simple substance photocatalyst shows excellent hydrogen production performance by visible light water splitting (1027 mu mol h) ‑1 g ‑1 ) And stability.
Description
Technical Field
The invention relates to a three-dimensional dendritic red phosphorus simple substance photocatalyst (DRP) with a composite crystal structure, which has excellent photocatalytic water splitting hydrogen production performance. Firstly, purifying commercial Red Phosphorus (RP) by a hydrothermal method; a preparation process of Chemical Vapor Deposition (CVD) is adopted, the amorphous RP after purification is used as a P source, the metal bismuth (Bi) is used as a cocatalyst, and a series of DRP simple substance photocatalysts are prepared by regulating and controlling the mass ratio of the RP to the 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 regarded as a green new energy source capable of replacing the traditional fossil fuel. Photocatalytic water splitting technology is an ideal strategy for preparing hydrogen energy, and the core and key point of the technology are the development of efficient photocatalysts. Although many excellent performance photocatalysts have been developed, the systems and compositions of most photocatalytic materials are overly complex. Thus, the development of a simple and efficient photocatalyst may be a better strategy.
RP is the simplest novel simple substance photocatalyst, has the advantages of adjustable energy level structure, wider visible light response range, low price, easy obtainment and the like, and has good application prospect in the field of photocatalytic water splitting hydrogen production. Research shows that the regulation and control of morphology and crystal structure is one of important strategies for improving RP photocatalytic hydrogen production activity. For example, a variety of different morphologies of RP have been developed, such as nanoparticles (Phys. Chem. Phys.,2016,18,3921), nanorods (nanoscales, 2014,6,14163), nanoplatelets (mater. Lett.,2019,236,542), nanowires (angel. Chem. Int. Ed.,2009,48,3616), and micro-ribbons (appl. Catalyst. B,2019,247,100), which further enhance the applicability of RP in the field of photocatalysis; hu et al prepared fiber crystalline form RP by CVD method with hydrogen production efficiency of 684 mu mol h -1 g -1 Is the highest record of the hydrogen generating activity of the simple substance semiconductor photocatalyst at present (Angew.chem.int.ed.2019, 55,9580).
Based on the basic strategy of morphology and crystal structure regulation and control, and inspired by a mechanism (Science, 1998,282,1105) of utilizing a CVD method to induce the growth of Carbon Nanotubes (CNTs) on the Ni surface by Ren et al, the invention adopts metal Bi as a cocatalyst and regulates the morphology and crystal structure of RP so as to further improve the photocatalytic water decomposition hydrogen production activity of the RP. The invention prepares the three-dimensional dendritic DRP simple substance photocatalyst with a composite crystal structure by taking purified commercial RP as a P source and adopting a CVD method under the participation of a metal Bi catalyst promoter. By adjusting the mass ratio of the metal Bi to the RP precursor (Bi: RP=1:0.5, 1:1, 1:2, 1:4), the effective regulation and control of the morphology and crystal structure of the DRP is realized. The research shows that when the mass ratio of the precursor Bi to RP=1:2, the prepared DRP simple 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 simple substance photocatalyst. The dendritic structure of the catalyst consists of RP nanowires ("trunks") of Hittorf crystal forms and RP nanorods ("branches") of fiber crystal forms, 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 photo-catalytic decomposition of water into hydrogen is improved.
The composite crystal form three-dimensional dendritic red phosphorus single-substance photocatalyst is characterized in that the composite crystal form three-dimensional dendritic red phosphorus single-substance photocatalyst is called DRP single-substance photocatalyst for short, the DRP single-substance photocatalyst contains two crystal forms of red phosphorus single-substance, the structural shape is a dendritic structure, the trunk of the corresponding dendritic structure is a RP nanowire of Hittorf crystal form, and the branches are RP nanorods of fiber crystal form.
The preparation method of the compound crystal form three-dimensional dendritic red phosphorus single-substance photocatalyst is characterized by comprising the following steps of:
(1) Purifying commercial RP by adopting a hydrothermal method to remove impurities on the surface of the commercial RP;
(2) The DRP photocatalyst is prepared by adopting a CVD method: mixing the purified RP and metal Bi powder uniformly, tabletting, placing into a quartz ampoule bottle, vacuumizing and sealing by acetylene flame; and (3) calcining the sample in a tube furnace at a high temperature, gradually cooling to room temperature, and sequentially performing ultrasonic treatment, centrifugation and washing on the prepared sample to remove the surface byproducts and the metal Bi of the sample, thereby obtaining the pure DRP simple substance photocatalyst.
The mass ratio of Bi to RP in the step (2) is=1:1 to 1:4, preferably 1:2.
High temperature calcination refers to: at 5 ℃ for min -1 Heating to 580 ℃ at a rate of 2h; then at 0.1 DEG C
min -1 Is cooled to 300 ℃; finally, the temperature is 1 ℃ for min -1 The rate of (2) is reduced to room temperature.
The application of the composite crystal three-dimensional dendritic red phosphorus simple substance photocatalyst is used for producing hydrogen by photocatalytic water decomposition, the DRP photocatalyst is dispersed in distilled water containing methanol, pt is added as a cocatalyst, and visible light is adopted as a light source to produce hydrogen by photocatalytic water decomposition.
The specific operation steps of the evaluation of the photocatalytic water splitting hydrogen production performance of the DRP photocatalyst prepared by the invention are as follows: 50mg of DRP photocatalyst was dispersed in 100mL of distilled water containing 10vol% methanol, and 1wt% Pt was added as a promoter. The photocatalysis hydrogen evolution experiment adopts a y-type reaction tank connected with a cooling system and a closed gas circulation/discharge system, adopts a 300W xenon lamp with an L40 filter as a visible light source, and detects the content of hydrogen generated by photocatalysis reaction by using a GC7900 gas chromatograph.
The invention has the advantages of cheap and easily obtained raw materials, simple and convenient preparation process flow, controllable product morphology and crystal form, and good photocatalytic hydrogen production activity under the irradiation of visible light. Wherein DRP (Bi: RP=1:2) has the highest hydrogen production activity, reaching 1027 mu mol h -1 g -1 Is 13 times larger than commercial RP. The catalyst is subjected to a photocatalytic hydrogen production activity test for 20 continuous hours, and the catalyst shows good photocatalytic hydrogen production stability.
Drawings
As shown in fig. 1, the XRD spectrum of the prepared sample was as follows. Curves (a), (b), (c), (d), (e), (f) are RP nanowires of commercial amorphous RP, hitdorf crystal form (Bi: rp=1:0.5), DRP (Bi: rp=1:1), DRP (Bi: rp=1:2), DRP (Bi: rp=1:4), RP nanorods of fiber crystal form (without Bi participation).
As shown in fig. 2, SEM spectra of the prepared samples were obtained. Curves (a), (b), (c), (d), (e), (f) are RP nanowires of commercial amorphous RP, hitdorf crystal forms (Bi: rp=1:0.5), DRP (Bi: rp=1:1), DRP (Bi: rp=1:2), DRP (Bi: rp=1:4), RP nanorods of fiber crystal forms (without Bi participation), respectively.
As shown in FIG. 3, a graph of the activity of visible light photocatalytic water splitting to produce hydrogen for the prepared samples is shown. The prepared DRP photocatalysts all show excellent photocatalytic hydrogen production performance, wherein the photocatalytic hydrogen production activity of DRP (Bi: RP=1:2) reaches 1027 mu mol h -1 g -1 Is 13 times larger than commercial RP.
As shown in fig. 4, a graph for testing the photocatalytic hydrogen production stability of DRP (Bi: rp=1:2) photocatalyst is shown. After the photocatalytic hydrogen production activity test is carried out for 20 continuous hours, the hydrogen production activity of the catalyst is found to be not obviously reduced, which indicates that the catalyst has good photocatalytic hydrogen production stability.
Detailed Description
Specific examples are set forth below to illustrate the invention in more detail, and the DRP photocatalyst produced is illustrated in the accompanying drawings.
Example 1: purification of commercial RP. 2g of commercial RP was weighed into a beaker, 60mL of distilled water was added and magnetically stirred for 1 hour; filling the solution into a polytetrafluoroethylene-lined high-pressure reaction kettle (100 mL), and heating in an oven at 200 ℃ for 12h; centrifuging, washing and drying to obtain the purified RP.
Example 2: preparation of DRP photocatalyst (CVD method). Weighing 200mg of purified commercial RP, uniformly mixing with Bi (50, 100, 200 and 400 mg) metals with different masses respectively, tabletting, respectively placing into different quartz ampoule bottles, vacuumizing and sealing with acetylene flame; placing the quartz ampoule bottle into a tube furnace at 5 ℃ for min -1 Heating to 580 ℃ at a rate of 2h; then the mixture is treated for 0.1 ℃ for min -1 Is cooled to 300 ℃; finally, the temperature is 1 ℃ for min -1 The rate of (2) is reduced to room temperature. The sample was taken out and treated with carbon disulphide (CS 2 ) Washing with distilled water for several times to remove byproducts; carrying out ultrasonic treatment on the aqueous solution of the sample for 2 hours, and standing for 1 hour to remove black precipitate (metal Bi); and centrifuging and drying to obtain the final product DRP photocatalyst.
The raw materials used in 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 (5)
1. The composite crystal form three-dimensional dendritic red phosphorus single-substance photocatalyst is characterized in that the composite crystal form three-dimensional dendritic red phosphorus single-substance photocatalyst is a DRP single-substance photocatalyst for short, is a heterojunction structure of a composite crystal form, and contains two crystal forms of red phosphorus single-substance, wherein the structural shape is a dendritic structure, the corresponding dendritic structure is an RP nanowire with a trunk of Hittorf crystal form, and branches into an RP nanorod of a fiber crystal form.
2. The preparation method of the compound crystal form three-dimensional dendritic red phosphorus single-substance photocatalyst as claimed in claim 1, which is characterized by comprising the following steps:
(1) Purifying commercial RP by adopting a hydrothermal method to remove impurities on the surface of the commercial RP;
(2) The DRP photocatalyst is prepared by adopting a CVD method: mixing the purified RP and metal Bi powder uniformly, tabletting, placing into a quartz ampoule bottle, vacuumizing and sealing by acetylene flame; calcining the sample in a tube furnace at a high temperature, gradually cooling to room temperature, sequentially performing ultrasonic treatment, centrifugation and washing on the prepared sample to remove the surface byproducts and the metal Bi, and finally obtaining the pure DRP simple substance photocatalyst;
the mass ratio of Bi to RP in the step (2) is=1:1-1:4;
high temperature calcination refers to: at 5 ℃ for min -1 Heating to 580 ℃ at a rate of 2h; then the mixture is treated for 0.1 ℃ for min -1 Is cooled to 300 ℃; finally, the temperature is 1 ℃ for min -1 The rate of (2) is reduced to room temperature.
3. The method according to claim 2, wherein the mass ratio of Bi to RP is 1:2.
4. The application of the compound crystal form three-dimensional dendritic red phosphorus simple substance photocatalyst in the hydrogen production by photocatalytic water splitting.
5. The method according to claim 4, wherein 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 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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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 |
|---|
| "Liquid bismuth initiated growth of phosphorus microbelts with efficient charge polarization for photocatalysis";Yang Liu，et al;《Applied Catalysis B: Environmental》;第100-106页 * |
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