CN111377479A - Application of nickel-doped molybdenum sulfide material in self-powered piezoelectricity-enhanced hydrogen production - Google Patents
Application of nickel-doped molybdenum sulfide material in self-powered piezoelectricity-enhanced hydrogen production Download PDFInfo
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- CN111377479A CN111377479A CN202010200288.2A CN202010200288A CN111377479A CN 111377479 A CN111377479 A CN 111377479A CN 202010200288 A CN202010200288 A CN 202010200288A CN 111377479 A CN111377479 A CN 111377479A
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 92
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 92
- 239000000463 material Substances 0.000 title claims abstract description 90
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 88
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 53
- JBANFLSTOJPTFW-UHFFFAOYSA-N azane;boron Chemical compound [B].N JBANFLSTOJPTFW-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910001453 nickel ion Inorganic materials 0.000 claims abstract description 7
- PTISTKLWEJDJID-UHFFFAOYSA-N sulfanylidenemolybdenum Chemical compound [Mo]=S PTISTKLWEJDJID-UHFFFAOYSA-N 0.000 claims abstract 2
- 239000000243 solution Substances 0.000 claims description 94
- 238000006243 chemical reaction Methods 0.000 claims description 50
- 238000009210 therapy by ultrasound Methods 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 239000008367 deionised water Substances 0.000 claims description 27
- 229910021641 deionized water Inorganic materials 0.000 claims description 27
- 229910052961 molybdenite Inorganic materials 0.000 claims description 27
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 27
- 239000004065 semiconductor Substances 0.000 claims description 24
- 239000011259 mixed solution Substances 0.000 claims description 18
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 18
- 230000001699 photocatalysis Effects 0.000 claims description 17
- 239000012779 reinforcing material Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims description 9
- 235000015393 sodium molybdate Nutrition 0.000 claims description 9
- 239000011684 sodium molybdate Substances 0.000 claims description 9
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 9
- 238000007789 sealing Methods 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 4
- 230000004044 response Effects 0.000 claims description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 3
- 230000001678 irradiating effect Effects 0.000 claims description 3
- 238000003756 stirring Methods 0.000 abstract description 3
- 239000011232 storage material Substances 0.000 abstract description 3
- 239000000446 fuel Substances 0.000 abstract description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 16
- 238000000034 method Methods 0.000 description 8
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 7
- 238000013032 photocatalytic reaction Methods 0.000 description 7
- 238000001291 vacuum drying Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 5
- 229910000085 borane Inorganic materials 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000004627 transmission electron microscopy Methods 0.000 description 3
- 229910003203 NH3BH3 Inorganic materials 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000004678 hydrides Chemical class 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000006303 photolysis reaction Methods 0.000 description 2
- 230000015843 photosynthesis, light reaction Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000001917 fluorescence detection Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000003574 free electron Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- -1 hydrogen Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- MRDDPVFURQTAIS-UHFFFAOYSA-N molybdenum;sulfanylidenenickel Chemical compound [Ni].[Mo]=S MRDDPVFURQTAIS-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 238000003797 solvolysis reaction Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
-
- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
-
- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
- B01J19/128—Infra-red light
-
- 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
-
- B01J35/39—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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- 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
- C01B3/06—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents
- C01B3/065—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents from a hydride
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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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 provides an application of a nickel-doped molybdenum sulfide material in self-powered piezoelectricity-enhanced hydrogen production. The nickel-doped molybdenum sulfide material (Ni-MoS)2) Comprising molybdenum sulphide MoS responsive to near-infrared light2The material and the divalent nickel ions doped in the molybdenum sulfide and on the surface of the molybdenum sulfide. The nickel-doped molybdenum sulfide material provided by the invention can effectively utilize the mechanical energy (such as vibration, noise, ultrasonic wave, stirring and other energy) in the nature, and the hydrogen content is up to 19.6 wt%Ammonia borane is used as a hydrogen storage material to prepare hydrogen energy at normal temperature and normal pressure, and self-powered piezoelectric enhanced hydrogen production is realized. And the hydrogen fuel can be used along with the preparation, thus solving the problem that the hydrogen is difficult to store. The preparation method of the nickel-doped molybdenum sulfide material provided by the invention is simple and feasible, and is green and environment-friendly.
Description
Technical Field
The invention relates to an application of a nickel-doped molybdenum sulfide material in self-powered piezoelectrically enhanced hydrogen production, in particular to an application of a nickel-doped molybdenum sulfide material in photocatalytic self-powered piezoelectrically enhanced hydrogen production, and belongs to the field of new energy.
Background
With the rapid development of human society, people's demand for energy is increasing day by day, and the exhaustion of fossil fuel causes energy shortage. Hydrogen energy is widely concerned by people because of its advantages of high combustion value, no secondary pollution and the like. However, hydrogen is easy to explode, and the cost of compressing hydrogen is high, so how to safely, effectively and economically prepare hydrogen and use hydrogen is a technical problem to be solved by hydrogen energy and hydrogen economy. Ammonia borane (NH)3BH3) The hydrogen storage material is a main hydrogen storage material, has the hydrogen content of 19.6 wt%, is solid at normal temperature and normal pressure, has higher stability, is safe and nontoxic, and is easy to carry. Thus, NH in contrast to gaseous or liquid hydrogen3BH3Is considered a more efficient and safer way of storing hydrogen energy. However, NH3BH3Hydrogen is released very slowly under natural conditions. In order to rapidly release hydrogen, catalysts containing noble metals, such as platinum, palladium, rhodium, gold, etc., have been developed. However, noble metals are expensive and low in abundance, so their applications are very limited. There is a need to develop a new technology that is safe, economical, environmentally friendly, and capable of releasing hydrogen gas efficiently.
Disclosure of Invention
The invention aims to provide application of a nickel-doped molybdenum sulfide material in self-powered piezoelectricity-enhanced hydrogen production, so as to overcome the defects in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a nickel-doped molybdenum sulfide piezoelectric reinforcing material (Ni-MoS)2) The application of the material in self-energized piezoelectric enhanced hydrogen production under infrared light irradiation.
Further, the nickel-doped molybdenum sulfide material comprises molybdenum sulfide MoS which is responsive to near infrared light2The material and the divalent nickel ions doped in the molybdenum sulfide and on the surface of the molybdenum sulfide.
Further, the mass of the divalent nickel ions is 10.0 wt% -35.0 wt% of the mass of the molybdenum sulfide material.
Further, the forbidden band width of the nickel-doped molybdenum sulfide material is 0.7eV-1.3 eV.
Further, the nickel is doped with molybdenum sulfide MoS2The response range of the semiconductor material to infrared light is 780-1550 nm.
Furthermore, under the condition that the temperature is 20-30 ℃, ultrasonic wave and near infrared light irradiation are simultaneously applied to a hydrogen production reaction system which is mainly formed by mixing a nickel-doped molybdenum sulfide material and ammonia borane aqueous solution, so that the preparation of hydrogen is realized.
Furthermore, the power of the ultrasonic wave is 20-30 KHz.
Further, the nickel-doped molybdenum sulfide material is prepared by a hydrothermal method, and the preparation method comprises the following steps:
(1) dissolving sodium molybdate in deionized water, and carrying out ultrasonic treatment for 30-60mins until the solution A is prepared; dissolving thiourea in deionized water, and carrying out ultrasonic treatment for 30-60mins until the solution B is uniformly mixed to obtain a solution B;
(3) dissolving nickel chloride hexahydrate in deionized water, and carrying out ultrasonic treatment for 30-60mins until the mixture is uniformly mixed to obtain a solution C;
(4) dropwise adding the solution B and the solution C into the solution A, and carrying out ultrasonic treatment for 30-60mins until the solution B and the solution C are uniformly mixed to obtain a mixed solution D;
(5) transferring the mixed solution D into a high-pressure reaction kettle, and reacting for 20-30h at the temperature of 150-.
Further, the concentration of the solution A is 0.1 mol/L-1.0 mol/L.
Further, the concentration of the solution B is 1.0 mol/L-5.0 mol/L.
Further, the concentration of the solution C is 0.1 mol/L-1.0 mol/L.
The embodiment of the invention also provides a self-powered piezoelectric enhanced photocatalytic hydrogen production method, which comprises the following steps:
doping ammonia borane and nickel with sulfurMolybdenum oxide piezoelectric reinforced material (Ni-MoS)2Semiconductor material) and applying mechanical energy and near infrared light to irradiate the hydrogen production reaction system at the same time, so that the hydrogen production reaction system reacts to generate hydrogen. Further, the mechanical energy may be generated by vibration, noise, ultrasonic waves, stirring, etc. applied to the hydrogen production reaction system.
The embodiment of the invention also provides a self-powered piezoelectric enhanced photocatalytic hydrogen production method, which comprises the following steps:
(1) putting ammonia borane aqueous solution into a photocatalytic hydrogen production reactor, and adding a nickel-doped molybdenum sulfide piezoelectric reinforcing material (Ni-MoS) into the ammonia borane aqueous solution2Semiconductor material) to form a hydrogen production reaction system, and then sealing the reactor;
(2) adjusting the temperature of the reactor to 1-5 ℃, then pumping the system to vacuum, and adjusting the temperature in the reactor to 20-30 ℃ after the reactor reaches a vacuum state;
(3) and applying ultrasonic waves to a hydrogen production reaction system in the reactor, and irradiating the hydrogen production reaction system with near infrared light to react in the hydrogen production reaction system and generate hydrogen.
Further, the photocatalytic hydrogen production reactor is shaded, so that ultraviolet light and visible light are prevented from entering a hydrogen production reaction system.
Further, the wavelength of the near infrared light is 850 nm.
Further, vacuum resin is used for sealing treatment.
Compared with the prior art, the invention has the advantages that: the nickel-doped molybdenum sulfide material provided by the invention has an enhanced piezoelectric effect, can effectively utilize mechanical energy (such as energy prepared by vibration, noise, ultrasonic waves, stirring and the like) in the nature to generate hydrogen energy, provides a new channel for preparing a hydrogen energy source, expands the practical application of a hydrogen production technology, and solves the problem that hydrogen is difficult to store as the prepared hydrogen is used along with preparation. The method for preparing the nickel-doped molybdenum sulfide material is simple and easy to implement, and is environment-friendly.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 shows a MoS provided by the present invention2And Ni-MoS2XRD pattern of the sample;
FIG. 2a is a MoS provided by the present invention2Transmission electron microscopy characterization of the samples, FIG. 2b is the Ni-MoS provided by the invention2A transmission electron microscope characterization map of the sample;
FIG. 3 shows a MoS provided by the present invention2And Ni-MoS2A solid state fluorescence reflectance map of the sample;
FIG. 4 shows Ni-MoS according to the present invention2A hydrogen yield curve chart when the sample is used for preparing hydrogen;
FIG. 5 is a reaction mechanism diagram of the photocatalytic hydrogen production reaction provided by the present invention.
Detailed Description
In view of the deficiencies in the prior art, the inventors of the present invention have made extensive studies and extensive practices to provide technical solutions of the present invention. The technical solution, its implementation and principles, etc. will be further explained as follows.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a nickel-doped molybdenum sulfide piezoelectric reinforcing material (Ni-MoS)2) The application of the material in self-energized piezoelectric enhanced hydrogen production under infrared light irradiation.
Further, the nickel-doped molybdenum sulfide material comprises molybdenum sulfide MoS which is responsive to near infrared light2The material and the divalent nickel ions doped in the molybdenum sulfide and on the surface of the molybdenum sulfide.
Further, the mass of the divalent nickel ions is 10.0 wt% -35.0 wt% of the mass of the molybdenum sulfide material.
Further, the forbidden band width of the nickel-doped molybdenum sulfide material is 0.7eV-1.3 eV.
Further, the nickel is doped with molybdenum sulfide MoS2The response range of the semiconductor material to infrared light is 780-1550 nm.
Furthermore, under the condition that the temperature is 20-30 ℃, ultrasonic wave and near infrared light irradiation are simultaneously applied to a hydrogen production reaction system which is mainly formed by mixing a nickel-doped molybdenum sulfide material and ammonia borane aqueous solution, so that the preparation of hydrogen is realized.
Furthermore, the power of the ultrasonic wave is 20-30 KHz.
Further, the nickel-doped molybdenum sulfide material is prepared by a hydrothermal method, and the preparation method comprises the following steps:
(1) dissolving sodium molybdate in deionized water, and carrying out ultrasonic treatment for 30-60mins until the solution A is prepared;
(2) dissolving thiourea in deionized water, and carrying out ultrasonic treatment for 30-60mins until the solution B is prepared;
(3) dissolving nickel chloride hexahydrate in deionized water, and carrying out ultrasonic treatment for 30-60mins until the mixture is uniformly mixed to obtain a solution C;
(4) dropwise adding the solution B and the solution C into the solution A, and carrying out ultrasonic treatment for 30-60mins until the solution B and the solution C are uniformly mixed to obtain a mixed solution D;
(5) transferring the mixed solution D into a high-pressure reaction kettle, and reacting for 20-30h at the temperature of 150-.
Further, the concentration of the solution A is 0.1-1.0 mol/L; the concentration of the solution B is 1.0-5.0 mol/L; the concentration of the solution C is 0.1 mol/L-1.0 mol/L.
The embodiment of the invention also provides a self-powered piezoelectric enhanced photocatalytic hydrogen production method, which comprises the following steps:
(1) putting ammonia borane aqueous solution into a photocatalytic hydrogen production reactor, and adding a nickel-doped molybdenum sulfide piezoelectric reinforcing material (Ni-MoS) into the ammonia borane aqueous solution2Semiconductor material) formedA hydrogen production reaction system, followed by sealing the reactor;
(2) adjusting the temperature of the reactor to 1-5 ℃, then pumping the system to vacuum, and adjusting the temperature in the reactor to 20-30 ℃ after the reactor reaches a vacuum state;
(3) and applying ultrasonic waves to a hydrogen production reaction system in the reactor, and irradiating the hydrogen production reaction system with near infrared light to react in the hydrogen production reaction system and generate hydrogen.
Further, the photocatalytic hydrogen production reactor is shaded, so that ultraviolet light and visible light are prevented from entering a hydrogen production reaction system.
Further, the wavelength of the near infrared light is 850 nm.
Further, vacuum resin is used for sealing treatment.
The reaction mechanism of the photocatalytic hydrogen production provided by the invention is that NH is carried out in the presence of a proper catalyst3BH3Hydrogen may be released by solvolysis or thermal decomposition, as follows:
NH3BH3(aq)+2H2O(l)＝NH4 +(aq)+BO2 -(aq)+3H2(g) (as shown in FIG. 5)
In the present invention, molybdenum sulfide itself is a semiconductor material that can respond to near infrared light and has a piezoelectric effect. The catalyst has three catalytic paths, the first is the thermal catalysis of the catalyst, which reduces the reaction potential of ammonia borane and water and accelerates the reaction rate. The second one is photocatalysis in response to 850nm near infrared light, electron transition occurs when the material is radiated by 850nm near infrared light, and photo-generated electrons react with protons h + in water to generate hydrogen. Since the electronegativity of H in the system is higher than that of B, H attracts free electrons to form hydride H-. Photoproduction of holes with hydride H-The combination produces hydrogen. The third is that the catalyst generates piezoelectric effect in ultrasonic oscillation, self-establishing electric field is formed inside the material to make the electron move directionally, and the generated electron and proton H in water+The reaction takes place to produce hydrogen, the resulting cavities are dissociated from the hydrogenSeed H-The combination produces hydrogen. After the nickel is doped into the molybdenum sulfide, the forbidden band width of the material is narrowed from the aspect of photocatalysis, the theoretical absorption boundary of the material is widened, and the utilization efficiency of light is improved. And the defects of the material are increased after doping, so that the recombination of electrons and holes is reduced, and the photocatalytic efficiency of the material is improved. From the aspect of piezoelectric catalysis, the surface defects of the material are increased, so that the entropy and the chaos of the material are increased, and the bulk defects of the material are increased, so that the symmetry of the material is reduced. The reduction of symmetry enhances the piezoelectric effect of the material, effectively inhibits the recombination of electrons and holes, and improves the piezoelectric catalysis efficiency of the material. In conclusion, the nickel doping improves the photocatalytic hydrogen production activity of molybdenum sulfide.
In one embodiment, the nickel-doped molybdenum sulfide material Ni-MoS prepared by the method is used2The semiconductor material is applied to automobiles, converts vibration energy in the automobile driving process into electric energy, and then hydrogen is prepared through photocatalytic reaction and is used as automobile fuel to realize self-energy supply hydrogen production.
The technical solution of the present invention is further explained below with reference to several examples.
Example 1
Piezoelectric reinforced material nickel-doped molybdenum sulfide material Ni-MoS2Preparation of semiconductor material, wherein the mass of Ni is MoS 210% of the mass of (a).
(1) 2.42g (0.01mol) of sodium molybdate (NaMoO)4.2H2O) is dissolved in 30mL deionized water, and is subjected to ultrasonic treatment for 30mins until the solution A is prepared after uniform mixing;
(2) 3.05g (0.04mol) of thiourea [ (NH)2)2CS]Dissolving in 30mL of deionized water, and carrying out ultrasonic treatment for 30mins until the solution B is uniformly mixed to obtain a solution B;
(3) 0.357g (0.0015mol) of nickel chloride hexahydrate is dissolved in deionized water, and ultrasonic treatment is carried out for 60mins until the solution C is prepared after uniform mixing;
(4) dropwise adding the solution B and the solution C into the solution A, and carrying out ultrasonic treatment for 60mins until the solution B and the solution C are uniformly mixed to obtain a mixed solution D;
(5) the mixed solution D is processed to be 100mL in constant volume and then is transferredReacting in a high-pressure reaction kettle at 200 ℃ for 24 hours, cooling, filtering, and drying in a vacuum drying oven at 60 ℃ for 6 hours to obtain the self-energized piezoelectric reinforcing material Ni-MoS2A semiconductor material.
The piezoelectric reinforcing material Ni-MoS prepared in the example 1 is doped with molybdenum sulfide material Ni-MoS2Semiconductor material and molybdenum sulfide MoS2XRD detection is carried out on the material, and the detection result is shown in figure 1.
The hydrogen production reaction is as follows:
(1) providing 100mL of NH at a concentration of 0.05mol/L3BH3Putting the solution into a photocatalytic hydrogen production reactor, and adding a self-energized piezoelectric reinforcing material (0.01 gNi-MoS) into the solution2Semiconductor material) covered with a quartz glass plate and sealed with the reactor;
(2) connecting the reactor photolysis water hydrogen production system in the step (1) with a low-temperature constant-temperature tank, sealing, controlling the temperature of the low-temperature constant-temperature tank to be 1 ℃, pumping the system to be vacuum, and controlling the temperature of the system to be 25 ℃ through the low-temperature constant-temperature tank after the system reaches a vacuum state;
(3) the reactor is placed in an ultrasonic cleaner, the ultrasonic is started, a near infrared light source with the wavelength of 850nm is placed 10cm above the reactor, the light source enters the reactor through a quartz glass plate to perform photocatalytic reaction, the photolysis water hydrogen production system is adjusted to be in a system circulation state to perform an experiment, and the hydrogen yield of each hour is detected by a gas chromatograph every other hour.
Example 2
Piezoelectric reinforced material nickel-doped molybdenum sulfide material Ni-MoS2Preparation of semiconductor material, wherein the mass of Ni is MoS 215 percent of the mass of
(1) 2.42g (0.01mol) of sodium molybdate (NaMoO)4.2H2O) is dissolved in 30mL deionized water, and is subjected to ultrasonic treatment for 30mins until the solution A is prepared after uniform mixing;
(2) 3.05g (0.04mol) of thiourea [ (NH)2)2CS]Dissolving in 30mL of deionized water, and carrying out ultrasonic treatment for 30mins until the solution B is uniformly mixed to obtain a solution B;
(3) 0.5355g (0.0022mol) of nickel chloride hexahydrate is dissolved in deionized water, and ultrasonic treatment is carried out for 60mins until the mixture is uniformly mixed to prepare solution C;
(4) dropwise adding the solution B and the solution C into the solution A, and carrying out ultrasonic treatment for 60mins until the solution B and the solution C are uniformly mixed to obtain a mixed solution D;
(5) the mixed solution D is processed to 100mL in constant volume and then transferred to a high-pressure reaction kettle, the reaction is carried out for 24 hours under the condition of controlling the temperature to be 200 ℃, and the self-energized piezoelectric reinforcing material Ni-MoS is prepared after the reaction is finished, cooled, filtered and placed in a vacuum drying oven to be dried for 6 hours under the condition of 60 DEG C2A semiconductor material.
The piezoelectric reinforcing material Ni-MoS prepared in the example 2 is doped with molybdenum sulfide material Ni-MoS2Semiconductor material and molybdenum sulfide MoS2The material was characterized by transmission electron microscopy and the results are shown in FIG. 2. Wherein, FIG. 2a shows a MoS provided by the present invention2Transmission electron microscopy characterization of the samples, FIG. 2b is the Ni-MoS provided by the invention2A transmission electron microscope characterization map of the sample;
the hydrogen production reaction was the same as the photocatalytic reaction procedure in example 1.
Example 3
Piezoelectric reinforced material nickel-doped molybdenum sulfide material Ni-MoS2Preparation of semiconductor material, wherein the mass of Ni is MoS 220% of the mass of (a).
(1) 2.42g (0.01mol) of sodium molybdate (NaMoO)4.2H2O) is dissolved in 30mL deionized water, and is subjected to ultrasonic treatment for 30mins until the solution A is prepared after uniform mixing;
(2) 3.05g (0.04mol) of thiourea [ (NH)2)2CS]Dissolving in 30mL of deionized water, and carrying out ultrasonic treatment for 30mins until the solution B is uniformly mixed to obtain a solution B;
(3) dissolving 0.714g (0.0030mol) of nickel chloride hexahydrate in deionized water, and carrying out ultrasonic treatment for 60mins until the mixture is uniformly mixed to obtain a solution C;
(4) dropwise adding the solution B and the solution C into the solution A, and carrying out ultrasonic treatment for 60mins until the solution B and the solution C are uniformly mixed to obtain a mixed solution D;
(5) the mixed solution D is processed to 100mL with constant volume and transferred into a high-pressure reaction kettle, and the temperature is controlled to be 200 DEG CThe mixture is reacted for 24 hours under the condition of one-piece reaction, and after the reaction is finished, the mixture is cooled, filtered and placed in a vacuum drying oven to be dried for 6 hours at the temperature of 60 ℃ to prepare the self-powered piezoelectric reinforcing material Ni-MoS2A semiconductor material.
The piezoelectric reinforcing material prepared in example 3 is doped with nickel molybdenum sulfide material Ni-MoS2Semiconductor material and molybdenum sulfide MoS2The material is subjected to solid fluorescence detection, the MoS2And Ni-MoS2Solid state fluorescence reflectance of the sample is shown in fig. 3.
The hydrogen production reaction was the same as the photocatalytic reaction procedure in example 1.
Example 4
Piezoelectric reinforced material nickel-doped molybdenum sulfide material Ni-MoS2Preparation of semiconductor material, wherein the mass of Ni is MoS 225% of the mass of (a).
(1) 2.42g (0.01mol) of sodium molybdate (NaMoO)4.2H2O) is dissolved in 30mL deionized water, and is subjected to ultrasonic treatment for 30mins until the solution A is prepared after uniform mixing;
(2) 3.05g (0.04mol) of thiourea [ (NH)2)2CS]Dissolving in 30mL of deionized water, and carrying out ultrasonic treatment for 30mins until the solution B is uniformly mixed to obtain a solution B;
(3) 0.893g (0.0038mol) of nickel chloride hexahydrate is dissolved in deionized water, and ultrasonic treatment is carried out for 60mins until the solution C is prepared after uniform mixing;
(4) dropwise adding the solution B and the solution C into the solution A, and carrying out ultrasonic treatment for 60mins until the solution B and the solution C are uniformly mixed to obtain a mixed solution D;
(5) the mixed solution D is processed to 100mL in constant volume and then transferred to a high-pressure reaction kettle, the reaction is carried out for 24 hours under the condition of controlling the temperature to be 200 ℃, and the self-energized piezoelectric reinforcing material Ni-MoS is prepared after the reaction is finished, cooled, filtered and placed in a vacuum drying oven to be dried for 6 hours under the condition of 60 DEG C2A semiconductor material.
The hydrogen production reaction was the same as the photocatalytic reaction procedure in example 1.
Example 5
Piezoelectric reinforced material nickel-doped molybdenum sulfide material Ni-MoS2Preparation of semiconductor material, wherein the mass of Ni is MoS 230% of the mass of (a).
(1) 2.42g (0.01mol) of sodium molybdate (NaMoO)4.2H2O) is dissolved in 30mL deionized water, and is subjected to ultrasonic treatment for 30mins until the solution A is prepared after uniform mixing;
(2) 3.05g (0.04mol) of thiourea [ (NH)2)2CS]Dissolving in 30mL of deionized water, and carrying out ultrasonic treatment for 30mins until the solution B is uniformly mixed to obtain a solution B;
(3) dissolving 1.07g (0.0045mol) of nickel chloride hexahydrate in deionized water, and carrying out ultrasonic treatment for 60mins until the mixture is uniformly mixed to obtain a solution C;
(4) dropwise adding the solution B and the solution C into the solution A, and carrying out ultrasonic treatment for 60mins until the solution B and the solution C are uniformly mixed to obtain a mixed solution D;
(5) the mixed solution D is processed to 100mL in constant volume and then transferred to a high-pressure reaction kettle, the reaction is carried out for 24 hours under the condition of controlling the temperature to be 200 ℃, and the self-energized piezoelectric reinforcing material Ni-MoS is prepared after the reaction is finished, cooled, filtered and placed in a vacuum drying oven to be dried for 6 hours under the condition of 60 DEG C2A semiconductor material.
The hydrogen production reaction was the same as the photocatalytic reaction procedure in example 1.
Example 6
Piezoelectric reinforced material nickel-doped molybdenum sulfide material Ni-MoS2Preparation of semiconductor material, wherein the mass of Ni is MoS 235% of the mass of (a).
(1) 2.42g (0.01mol) of sodium molybdate (NaMoO)4.2H2O) is dissolved in 30mL deionized water, and is subjected to ultrasonic treatment for 30mins until the solution A is prepared after uniform mixing;
(2) 3.05g (0.04mol) of thiourea [ (NH)2)2CS]Dissolving in 30mL of deionized water, and carrying out ultrasonic treatment for 30mins until the solution B is uniformly mixed to obtain a solution B;
(3) dissolving 1.31g (0.0055mol) of nickel chloride hexahydrate in deionized water, and carrying out ultrasonic treatment for 60mins until the mixture is uniformly mixed to obtain a solution C;
(4) dropwise adding the solution B and the solution C into the solution A, and carrying out ultrasonic treatment for 60mins until the solution B and the solution C are uniformly mixed to obtain a mixed solution D;
(5) the mixed solution D is processed to 100mL by constant volume and then transferred into a high-pressure reaction kettle,the temperature is controlled to be 200 ℃ for 24 hours, and the self-energized piezoelectric reinforcing material Ni-MoS is prepared after the reaction is finished, cooling, suction filtration and drying in a vacuum drying oven at 60 ℃ for 6 hours2A semiconductor material.
The hydrogen production reaction was the same as the photocatalytic reaction procedure in example 1.
It should be understood that the above-mentioned embodiments are merely illustrative of the technical concepts and features of the present invention, which are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and therefore, the protection scope of the present invention is not limited thereby. All equivalent changes and modifications made according to the spirit of the present invention should be covered in the protection scope of the present invention.
Claims (10)
1. Nickel-doped molybdenum sulfide piezoelectric reinforced material (Ni-MoS)2) The application of the material in self-energized piezoelectric enhanced hydrogen production under infrared light irradiation.
2. Use according to claim 1, characterized in that: the nickel-doped molybdenum sulfide material comprises molybdenum sulfide MoS which responds to near infrared light2The material and the divalent nickel ions doped in the molybdenum sulfide and on the surface of the molybdenum sulfide.
3. Use according to claim 2, characterized in that: the mass of the divalent nickel ions is 10.0 wt% -35.0 wt% of the mass of the molybdenum sulfide material.
4. Use according to claim 2, characterized in that: the forbidden band width of the nickel-doped molybdenum sulfide material is 0.7eV-1.3 eV.
5. Use according to claim 2, characterized in that: the nickel-doped molybdenum sulfide MoS2The response range of the semiconductor material to infrared light is 780-1550 nm.
6. Use according to claim 2, characterized in that it comprises: under the condition that the temperature is 20-30 ℃, ultrasonic wave and near infrared light irradiation are simultaneously applied to a hydrogen production reaction system which is mainly formed by mixing a nickel-doped molybdenum sulfide material and ammonia borane aqueous solution, so that the preparation of hydrogen is realized.
7. Use according to claim 6, characterized in that: the power of the ultrasonic wave is 20-30 KHz.
8. Use according to claim 1, wherein the nickel-doped molybdenum sulphide material is prepared by a hydrothermal method, and the preparation method comprises the following steps:
(1) dissolving sodium molybdate in deionized water, and carrying out ultrasonic treatment for 30-60mins until the solution A is prepared;
(2) dissolving thiourea in deionized water, and carrying out ultrasonic treatment for 30-60mins until the solution B is prepared;
(3) dissolving nickel chloride hexahydrate in deionized water, and carrying out ultrasonic treatment for 30-60mins until the mixture is uniformly mixed to obtain a solution C;
(4) dropwise adding the solution B and the solution C into the solution A, and carrying out ultrasonic treatment for 30-60mins until the solution B and the solution C are uniformly mixed to obtain a mixed solution D;
(5) transferring the mixed solution D into a high-pressure reaction kettle, and reacting for 20-30h at the temperature of 150-.
9. Use according to claim 8, characterized in that: the concentration of the solution A is 0.1-1.0 mol/L; the concentration of the solution B is 1.0-5.0 mol/L; the concentration of the solution C is 0.1 mol/L-1.0 mol/L.
10. A self-powered piezoelectric enhanced photocatalytic hydrogen production method is characterized by comprising the following steps:
(1) putting ammonia borane aqueous solution into a photocatalytic hydrogen production reactor, and adding a nickel-doped molybdenum sulfide piezoelectric reinforcing material (Ni-MoS) into the ammonia borane aqueous solution2) Forming a hydrogen production reaction system, and then sealing the reactor;
(2) adjusting the temperature of the reactor to 1-5 ℃, then pumping the system to vacuum, and adjusting the temperature in the reactor to 20-30 ℃ after the reactor reaches a vacuum state;
(3) and applying ultrasonic waves to a hydrogen production reaction system in the reactor, and irradiating the hydrogen production reaction system with near infrared light to react in the hydrogen production reaction system and generate hydrogen.
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