CN114950491A - Preparation of nickel-molybdenum-cadmium trimetal nano material constructed by polyacid and photocatalytic application of nickel-molybdenum-cadmium trimetal nano material - Google Patents
Preparation of nickel-molybdenum-cadmium trimetal nano material constructed by polyacid and photocatalytic application of nickel-molybdenum-cadmium trimetal nano material Download PDFInfo
- Publication number
- CN114950491A CN114950491A CN202210231665.8A CN202210231665A CN114950491A CN 114950491 A CN114950491 A CN 114950491A CN 202210231665 A CN202210231665 A CN 202210231665A CN 114950491 A CN114950491 A CN 114950491A
- Authority
- CN
- China
- Prior art keywords
- polyacid
- nickel
- cadmium
- molybdenum
- trimetal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 35
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 27
- YRYCCFRWHYDMCT-UHFFFAOYSA-N [Ni].[Cd].[Mo] Chemical compound [Ni].[Cd].[Mo] YRYCCFRWHYDMCT-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000001257 hydrogen Substances 0.000 claims abstract description 31
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 claims abstract description 22
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000011941 photocatalyst Substances 0.000 claims abstract description 15
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 6
- 229910052724 xenon Inorganic materials 0.000 claims abstract description 6
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 5
- 239000002243 precursor Substances 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 12
- 229910003294 NiMo Inorganic materials 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- 241000080590 Niso Species 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 5
- 229940101006 anhydrous sodium sulfite Drugs 0.000 claims description 4
- 230000003197 catalytic effect Effects 0.000 claims description 4
- 238000000354 decomposition reaction Methods 0.000 claims description 4
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 4
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- 239000002905 metal composite material Substances 0.000 claims description 3
- 238000007146 photocatalysis Methods 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000002073 nanorod Substances 0.000 claims description 2
- 239000002135 nanosheet Substances 0.000 claims description 2
- 239000004065 semiconductor Substances 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 239000013335 mesoporous material Substances 0.000 claims 1
- DDTIGTPWGISMKL-UHFFFAOYSA-N molybdenum nickel Chemical compound [Ni].[Mo] DDTIGTPWGISMKL-UHFFFAOYSA-N 0.000 claims 1
- 239000011148 porous material Substances 0.000 claims 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 19
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 4
- 229910052759 nickel Inorganic materials 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 238000005054 agglomeration Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 abstract description 2
- 230000002194 synthesizing effect Effects 0.000 abstract description 2
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 abstract 1
- 238000003860 storage Methods 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 6
- 238000001000 micrograph Methods 0.000 description 4
- 229910052723 transition metal Inorganic materials 0.000 description 4
- 150000003624 transition metals Chemical class 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 229910052976 metal sulfide Inorganic materials 0.000 description 2
- 238000001907 polarising light microscopy Methods 0.000 description 2
- 229920006324 polyoxymethylene Polymers 0.000 description 2
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical class [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011684 sodium molybdate Substances 0.000 description 1
- 235000015393 sodium molybdate Nutrition 0.000 description 1
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000002123 temporal effect Effects 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
- B01J27/0515—Molybdenum with iron group metals or platinum group metals
-
- 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
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/133—Renewable energy sources, e.g. sunlight
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention relates to preparation and application of a polyacid-derived trimetallic sulfide in the field of photocatalytic hydrogen evolution. The invention aims to solve the problems of rare raw material storage, poor activity under visible light and high cost of the prior art for synthesizing the high-performance photocatalyst and solve the problem of MoS 2 The problem of agglomeration is easy to occur. The patent designs and develops a polymetallic sulfide material Ni derived from polymolybdic acid 3 S 2 ‑MoS 2 -CdS. The adopted method comprises the following steps: preparing two precursors by using Waugh type nickel molybdic acid, thiourea and cadmium nitrate as raw materials, preparing a nickel molybdenum cadmium trimetal nano material photocatalyst constructed by polyacid by a hydrothermal synthesis method, and finding that the photocatalyst has high hydrogen production rate and the average hydrogen production efficiency can reach 2873 mu mol g under the irradiation of a 500W xenon lamp after a photocatalytic hydrogen production test ‑1 ·h ‑1 . And for a period of 30 hoursAfter 5 times of photocatalytic tests, the photocatalytic activity of the photocatalyst is not obviously reduced, and the fact that the nickel-molybdenum-cadmium three-metal nano-material photocatalyst constructed by the polyacid has good stability is proved.
Description
Technical Field
The invention relates to the field of photocatalytic hydrogen evolution.
Background
Due to the rapid depletion of fossil fuels and the deterioration of global environment, it is very urgent to search for sustainable and clean energy sources to replace the depleted fossil fuels. Many researchers have focused on developing green, pollution-free clean energy sources such as wind and solar, but the application of these new energy sources is severely limited by their spatial limitations and temporal instability. The light decomposition of solar energy to produce hydrogen is a very interesting focus, and the light catalytic hydrogen production is a technology which can convert the solar energy into clean and renewable hydrogen energy.
POMs having transition metal oxyanion cluster of d 0 The electronic structure construction is similar to the properties of metal oxide semiconductors, and therefore is considered as the most promising photocatalytic hydrogen production photocatalyst. Polyacids exhibit a wide variety of compositions and structures, can be manipulated at the molecular level and can provide precise ratios of transition metals, most of which are active only under uv irradiation, and few and less active under visible light irradiation. Compared with single metal sulfide, the trimetal sulfide shows obvious advantages in the process of photocatalytic hydrogen production by virtue of unique trimetal synergistic effect. Therefore, the polyoxometallate is taken as a precursor to provide a strategy for synthesizing the high-dispersion trimetallic sulfide photocatalyst.
Disclosure of Invention
Based on the background, the invention aims to provide the preparation and the photocatalytic application of the nickel-molybdenum-cadmium trimetal nanomaterial constructed by polyacid, and the preparation method is simple and convenient and has low cost. The prepared nano material has higher hydrogen production rate and good stability
The purpose of the invention is realized as follows:
the preparation method of the nickel-molybdenum-cadmium three-metal nano material constructed by polyacid comprises the following steps:
(1) 0.47g of NiSO was weighed 4 Dissolved in 5mL of boiling water, and then 4.94g (NH) was weighed 4 ) 6 Mo 7 O 24 ·4H 2 O, dissolved in 20mL of distilled water and adjusted to pH 4.1 with 1M sulfuric acid solution, and the solution is heated to boiling and added to NiSO while hot 4 In solution, at this point, 0.75g K 2 S 2 O 8 Are added together. Cooling the solution to the chamberFiltering and washing to obtain grey powder, i.e. NiMo 9 Drying in an oven at 60 deg.C for 24 hr to obtain (NH) 4 ) 6 (NiMo 9 O 32 )·8H 2 And (4) O precursor.
(2) 0.384g Cd (NO) was weighed 3 ) 2 ·4H 2 Dissolving O in 10mL of ethylenediamine, stirring for 10min, then weighing 0.284g of thiourea, adding the thiourea into the solution, stirring for 30min, reacting for 24h at 160 ℃, and then cooling to obtain CdS. Washing the product with absolute ethyl alcohol and distilled water for multiple times, and drying at 60 ℃ for 24h to obtain the CdS.
(3) 0.0369g (NH) was weighed 4 ) 6 (NiMo 9 O 32 )·8H 2 Dissolving O and 0.06g thiourea in 15mL distilled water, stirring for 1h at room temperature, weighing 0.0095g CdS, adding the solution, stirring for 30min, transferring to 25mL polytetrafluoroethylene, keeping at 180 deg.C for 24h, cooling to obtain Ni 3 S 2 -MoS 2 -CdS ternary metal composite photocatalyst. The product was washed several times with water and dried at 60 ℃ for 24 h.
The application of the nickel-molybdenum-cadmium trimetal nano material constructed by the polyacid is mainly in the aspects of photocatalytic decomposition of water and hydrogen evolution.
The application method comprises the following steps: under the irradiation of a 500W xenon lamp, sodium sulfide and anhydrous sodium sulfite are used as sacrificial agents, a system for decomposing water by photocatalysis to produce hydrogen is used as a catalytic system with the highest hydrogen production, and the average hydrogen production efficiency is 2873 mu mol g -1 ·h -1 Therefore, the nickel-molybdenum-cadmium three-metal nano material constructed by the polyacid is a high-efficiency photocatalyst for photocatalytic water decomposition.
Compared with the prior art, the invention has the following characteristics:
the invention adopts Polyacid (POMs) as a molecular platform which can provide a plurality of transition metal sources at the same time, and well solves the problem that the growth process is difficult to control due to the inconsistent nucleation rate of each component caused by the introduction of the transition metal. Breaks through the defects of uneven mixing, mutual separation and no reaction of reaction raw materials in the traditional technical line for preparing the trimetallic sulfide by taking simple sodium molybdate and metal salt as main raw materialsThe technical bottlenecks of synchronization, different product shapes, easy agglomeration and the like are realized, so that the high-dispersion and uniformly-distributed trimetallic sulfide is directionally prepared. The average hydrogen production efficiency is 2873 mu mol g by using a 500W xenon lamp as a light source and sodium sulfide and anhydrous sodium sulfite as sacrificial agents -1 ·h -1 。
The invention can obtain a nickel-molybdenum-cadmium trimetal nano material constructed by polyacid.
Drawings
FIG. 1 shows a polyacid-structured Ni-Mo-Cd-trimetal nanomaterial prepared in example 1 of the present invention and MoS 2 (JCPDS Card No.37-1492)、Ni 3 S 2 (JCPDS Card No.44-1418) and CdS (JCPDS Card number 47-1179) XRD spectra.
FIG. 2 is a scanning electron microscope image of a polyacid-structured Ni-Mo-Cd-trimetal nanomaterial prepared in example 1 of the present invention.
FIG. 3 is a transmission electron microscope image of a polyacid-structured Ni-Mo-Cd-trimetal nanomaterial prepared in example 1 of the present invention.
FIG. 4 is a BET test chart of a polyacid-structured Ni-Mo-Cd-trimetal nanomaterial prepared in example 1 of the present invention.
FIG. 5 shows a polyacid-structured Ni-Mo-Cd trimetal nanomaterial prepared in example 1 of the present invention and Waugh-type Ni-molybdic acid and Ni 3 S 2 -MoS 2 The photocatalytic hydrogen production rate is compared with the hydrogen production rate.
Fig. 6 shows the photocatalytic cycle stability of a polyacid-structured nickel-molybdenum-cadmium trimetal nanomaterial prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and examples.
Embodiment 1, a polyacid-structured nickel-molybdenum-cadmium trimetal nanomaterial, comprising the following preparation steps:
(1) 0.47g of NiSO was weighed 4 Dissolved in 5mL of boiling water, and then 4.94g (NH) was weighed 4 ) 6 Mo 7 O 24 ·4H 2 O, dissolved in 20mL of distilled water and adjusted to pH 4.1 with 1M sulfuric acid solution, and the solution was addedHeating to boil, and adding into NiSO 4 In solution, at this point, 0.75g K 2 S 2 O 8 Are added together. After the solution is cooled to room temperature, carrying out suction filtration and washing to obtain gray powder, namely NiMo 9 Drying in an oven at 60 deg.C for 24 hr to obtain (NH) 4 ) 6 (NiMo 9 O 32 )·8H 2 And (4) O precursor.
(2) 0.384g Cd (NO) was weighed 3 ) 2 ·4H 2 Dissolving O in 10mL of ethylenediamine, stirring for 10min, then weighing 0.284g of thiourea, adding the thiourea into the solution, stirring for 30min, reacting for 24h at 160 ℃, and then cooling to obtain CdS. Washing the product with absolute ethyl alcohol and distilled water for multiple times, and drying at 60 ℃ for 24h to obtain the CdS.
(3) 0.0369g (NH) was weighed 4 ) 6 (NiMo 9 O 32 )·8H 2 Dissolving O and 0.06g thiourea in 15mL distilled water, stirring for 1h at room temperature, weighing 0.0095g CdS, adding the solution, stirring for 30min, transferring to 25mL polytetrafluoroethylene, keeping at 180 deg.C for 24h, cooling to obtain Ni 3 S 2 -MoS 2 -CdS ternary metal composite photocatalyst. The product was washed several times with water and dried at 60 ℃ for 24 h.
The invention is further described with reference to the following drawings and examples:
as shown in figure 1, the nickel molybdenum cadmium trimetal nano material and MoS constructed by polyacid 2 (JCPDS Card No. 37-1492)、Ni 3 S 2 (JCPDS Card No.44-1418) and CdS (JCPDS Card No.47-1179) XRD spectra. Nickel metal sulfide and MoS derived from polymolybdic acid 2 (JCPDS,No.37-1492)、Ni 3 S 2 (JCPDS, No.44-1418) and CdS (JCPDS Card No.47-1179) XRD have good matching, and diffraction peaks at 14.3 degrees, 32.6 degrees, 39.5 degrees and 58.3 degrees of 2 theta respectively correspond to MoS 2 (002), (100), (103) and (110) crystal planes (JCPDS, No. 37-1492). Diffraction peaks at 44.3 °, 37.7 °, 54.6 ° and 31.1 ° are Ni 3 S 2 (JCPDS, No.44-1418) with (202), (003), (122) and (110) crystal planes, and diffraction peaks at 24.8 °, 26.4 °, 28.1 ° and 47.7 ° and 51.8 ° assignedIn the (400), (033), (042), (037) and (028) crystal planes of CdS (JCPDS, No. 47-1179).
FIG. 2 shows a scanning electron microscope image of a polyacid-structured Ni-Mo-Cd trimetal nanomaterial. Ni 3 S 2 -MoS 2 the-CdS is formed by cross arrangement of nano sheets and nano rods. The cross arrangement of the flaky materials fully exposes active sites, which is beneficial to the entering of sacrificial agents and the effective transfer of electrons, and the addition of the rod-shaped CdS further improves the photocatalytic hydrogen production performance.
FIG. 3 shows a transmission electron microscope image of a polyacid-structured Ni-Mo-Cd trimetal nanomaterial. The lattice fringes at 0.29nm being Ni 3 S 2 The (110) crystal plane of (A), the lattice fringes having a lattice spacing of 0.62nm corresponding to MoS 2 The (002) crystal plane of (b) at 0.35nm and the lattice fringes correspond to the (400) crystal plane of CdS.
Fig. 4 is a BET test chart of a polyacid-structured nickel-molybdenum-cadmium trimetal nanomaterial, which shows that the material has a large specific surface area, and mesopores exist in the structure, so that the contact between the material and a sacrificial agent is facilitated, and the photocatalytic performance is improved.
FIG. 5 shows a polyacid-structured Ni-Mo-Cd trimetal nanomaterial and Waugh-type nickel molybdic acid and Ni 3 S 2 -MoS 2 The photocatalytic hydrogen production rate is compared with the hydrogen production rate. Sodium sulfide and anhydrous sodium sulfite are used as sacrificial agents, a system for producing hydrogen by decomposing water through photocatalysis is a catalytic system with the highest hydrogen production, and the average hydrogen production efficiency is 2873 mu mol g -1 ·h -1 Thus, the nickel-molybdenum-cadmium trimetal nano material constructed by polyacid is an efficient photocatalyst.
FIG. 6 shows the photocatalytic cycling stability of a polyacid-structured Ni-Mo-Cd trimetal nanomaterial. Ni after 30h, 5 cycle tests with 500W xenon lamp irradiation 3 S 2 -MoS 2 And Ni 3 S 2 -MoS 2 The photocatalytic hydrogen production rate of CdS is not obviously reduced, which shows that the CdS has good stability, and the prepared nickel-molybdenum-cadmium trimetal nano material constructed by polyacid can be used as very stable photocatalytic hydrogen productionA photocatalyst for hydrogen production.
Claims (5)
1. A nickel-molybdenum-cadmium tri-metal nano material constructed by polyacid is characterized in that photosensitive semiconductor CdS is introduced into a nickel-molybdenum bi-metal polyacid system, the appearance presents a structure of cross arrangement of nano sheets and nano rods, the nano material has a large specific surface area, and the surface area can reach 27.941m 2 ·g -1 And the pore size of the mesoporous material is 2-15 nanometers, so that the problem that photo-generated electrons and holes are easy to recombine is effectively solved.
2. A preparation method and a photocatalytic application of a nickel-molybdenum-cadmium trimetal nano material constructed by polyacid comprise the following steps:
(1) 0.47g of NiSO was weighed 4 Dissolved in 5mL of boiling water, and then 4.94g (NH) was weighed 4 ) 6 Mo 7 O 24 ·4H 2 O, dissolved in 20mL of distilled water and adjusted to pH 4.1 with 1M sulfuric acid solution, and the solution is heated to boiling and added to NiSO while hot 4 In solution, at this point, 0.75g K 2 S 2 O 8 Are added together. After the solution is cooled to room temperature, carrying out suction filtration and washing to obtain gray powder, namely NiMo 9 Drying in a 60 ℃ oven for 24h to obtain (NH) 4 ) 6 (NiMo 9 O 32 )·8H 2 And (4) O precursor.
(2) 0.384g Cd (NO) was weighed 3 ) 2 ·4H 2 Dissolving O in 10mL of ethylenediamine, stirring for 10min, then weighing 0.284g of thiourea, adding the thiourea into the solution, stirring for 30min, reacting for 24h at 160 ℃, and then cooling to obtain CdS. Washing the product with absolute ethyl alcohol and distilled water for many times, and drying at 60 ℃ for 24 hours to obtain the CdS.
(3) 0.0369g (NH) was weighed 4 ) 6 (NiMo 9 O 32 )·8H 2 Dissolving O and 0.06g thiourea in 15mL distilled water, stirring at room temperature for 1h, weighing 0.0095g CdS, adding the solution, stirring for 30min, transferring to 25mL polytetrafluoroethylene, keeping at 180 ℃ for 24h, cooling to obtain Ni 3 S 2 -MoS 2 -CdS ternary metal composite photocatalyst. The product was washed several times with water and dried at 60 ℃ for 24 h.
3. The application of the polyacid-structured nickel-molybdenum-cadmium trimetal nanomaterial in patent claim 2 is characterized in that the preparation of the polyacid-structured nickel-molybdenum-cadmium trimetal nanomaterial and the application of the polyacid-structured nickel-molybdenum-cadmium trimetal nanomaterial in photocatalytic water decomposition for hydrogen production.
4. The use according to claim 3, characterized in that the method of application is as follows: under the irradiation of a 500W xenon lamp, sodium sulfide and anhydrous sodium sulfite are used as sacrificial agents, a system for decomposing water by photocatalysis to produce hydrogen is used as a catalytic system with the highest hydrogen production, and the average hydrogen production efficiency is 2873 mu mol g -1 ·h -1 Thus, the nickel-molybdenum-cadmium trimetal nano material constructed by polyacid is an efficient photocatalyst.
5. Use according to claim 3, characterized in that: under the irradiation of a 500W xenon lamp, after 30 hours and 5 times of photocatalytic tests, the photocatalytic activity is not obviously reduced, and the nickel-molybdenum-cadmium trimetal nano material photocatalyst constructed by the polyacid is proved to have good stability.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210231665.8A CN114950491A (en) | 2022-03-09 | 2022-03-09 | Preparation of nickel-molybdenum-cadmium trimetal nano material constructed by polyacid and photocatalytic application of nickel-molybdenum-cadmium trimetal nano material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210231665.8A CN114950491A (en) | 2022-03-09 | 2022-03-09 | Preparation of nickel-molybdenum-cadmium trimetal nano material constructed by polyacid and photocatalytic application of nickel-molybdenum-cadmium trimetal nano material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114950491A true CN114950491A (en) | 2022-08-30 |
Family
ID=82975583
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210231665.8A Pending CN114950491A (en) | 2022-03-09 | 2022-03-09 | Preparation of nickel-molybdenum-cadmium trimetal nano material constructed by polyacid and photocatalytic application of nickel-molybdenum-cadmium trimetal nano material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114950491A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105664977A (en) * | 2016-02-03 | 2016-06-15 | 中国科学院化学研究所 | Molybdenum disulfide-cadmium sulfide nanometer composite material and preparing method and application thereof |
| WO2019150000A1 (en) * | 2018-02-02 | 2019-08-08 | Wmz - Nanosurfaces Oy | Nanocomposites for photocatalytic water splitting using visible light and method for synthesis thereof |
| CN110841661A (en) * | 2019-11-28 | 2020-02-28 | 福建农林大学 | Preparation method and application of 1T-2H molybdenum disulfide @ cadmium sulfide composite nanomaterial |
| CN113578353A (en) * | 2021-07-27 | 2021-11-02 | 哈尔滨理工大学 | Preparation of polymolybdic acid-derived nickel metal sulfide and photocatalytic application thereof |
-
2022
- 2022-03-09 CN CN202210231665.8A patent/CN114950491A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105664977A (en) * | 2016-02-03 | 2016-06-15 | 中国科学院化学研究所 | Molybdenum disulfide-cadmium sulfide nanometer composite material and preparing method and application thereof |
| WO2019150000A1 (en) * | 2018-02-02 | 2019-08-08 | Wmz - Nanosurfaces Oy | Nanocomposites for photocatalytic water splitting using visible light and method for synthesis thereof |
| CN110841661A (en) * | 2019-11-28 | 2020-02-28 | 福建农林大学 | Preparation method and application of 1T-2H molybdenum disulfide @ cadmium sulfide composite nanomaterial |
| CN113578353A (en) * | 2021-07-27 | 2021-11-02 | 哈尔滨理工大学 | Preparation of polymolybdic acid-derived nickel metal sulfide and photocatalytic application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2021184563A1 (en) | Preparation method for foamed nickel-based catalyst for hydrogen production by water electrolysis | |
| CN111420664B (en) | Preparation method of flaky cuprous oxide/cobaltous oxide nanocomposite and application of flaky cuprous oxide/cobaltous oxide nanocomposite in catalyzing ammonia borane hydrolysis hydrogen production | |
| CN109746011B (en) | MOF-based derived composite photocatalyst and preparation method thereof | |
| WO2021232751A1 (en) | Porous coo/cop nanotubes, preparation method therefor and use thereof | |
| CN112663088B (en) | Preparation method of cobalt diselenide/iron oxyhydroxide composite material with nanometer petal-shaped structure | |
| CN107519905B (en) | Vanadium carbide nano-sieve electrocatalytic material capable of being used in wide pH range and preparation method thereof | |
| CN112871186A (en) | Nickel diselenide/sulfur indium zinc composite photocatalyst and preparation method and application thereof | |
| CN113299485A (en) | Bimetallic (Ni, Co) Se2Preparation method of heterostructure and application of heterostructure in super capacitor | |
| CN113578353A (en) | Preparation of polymolybdic acid-derived nickel metal sulfide and photocatalytic application thereof | |
| CN111085276B (en) | Preparation method of echinoid cobalt diselenide nanoparticles, and product and application thereof | |
| CN110013855B (en) | High-efficiency cobalt nickel oxide/nickel hydroxide compound electrocatalyst and preparation method and application thereof | |
| CN114950491A (en) | Preparation of nickel-molybdenum-cadmium trimetal nano material constructed by polyacid and photocatalytic application of nickel-molybdenum-cadmium trimetal nano material | |
| CN113428847B (en) | Nickel-molybdenum-copper ternary metal phosphide, preparation method and application thereof | |
| CN116005173A (en) | Epitaxial growth noble metal catalyst by combining 'atomization blasting' method with lattice grafting strategy and preparation method thereof | |
| CN116065185A (en) | Preparation method of rapidly constructed nano cone supported nano sheet electrocatalyst | |
| CN113842925B (en) | CdS/NiS2Bulk photocatalyst and preparation method and application thereof | |
| CN113652698B (en) | Tungsten-doped nickel phosphide dual-functional catalytic material with crossed nano-sheet structure | |
| CN112295581B (en) | Electrocatalyst material and application thereof | |
| CN110560095B (en) | Flaky semimetal MoTe2Cu and flaky semi-metal MoTe2Preparation method of Cu/RGO | |
| CN109012683B (en) | Preparation method of cobalt molybdate hollow microsphere electrocatalyst | |
| CN114956177B (en) | Polyacid-derived cadmium-molybdenum bimetallic hexagonal prism nano material | |
| CN110624572A (en) | Flaky semimetal MoTe2And flaky semi-metal MoTe2Preparation method of/RGO | |
| CN100363263C (en) | Process for preparing CdO nano powder of high qulity active cell material | |
| CN117463373B (en) | Porous hollow tubular CoS 2 /NiS 2 Rapid preparation method and application of heterojunction | |
| CN115125576B (en) | Composite selenide electrocatalyst and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |