CN103566953B - One-dimensional nanometer photocatalyst as well as preparation method and application thereof - Google Patents

One-dimensional nanometer photocatalyst as well as preparation method and application thereof Download PDF

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CN103566953B
CN103566953B CN201310614267.5A CN201310614267A CN103566953B CN 103566953 B CN103566953 B CN 103566953B CN 201310614267 A CN201310614267 A CN 201310614267A CN 103566953 B CN103566953 B CN 103566953B
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CN103566953A (en
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安长华
李金全
王淑涛
张钦辉
张军
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China University of Petroleum East China
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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 a one-dimensional nanometer photocatalyst as well as a preparation method and application thereof. The photocatalyst adopts a one-dimensional CdS nanometer rod structure modified by atom layer thickness MoS2; the formula is CdS: MoS2. The simple polylol pressurizing technology is adopted to realize the synthesis of the CdS: MoS2 composite nanometer photocatalyst; firstly, CdS nanometer rods with uniform size and regular morphology are synthesized in an ethanediamine system; then the polylol pressurizing reduction technology is adopted to decompose ATTM in situ on CdS to obtain the one-dimensional CdS: MoS2 composite nanometer photocatalyst. The catalyst has the solar photocatalytic water hydrogen preparation performance, can largely improve the efficiency of hydrogen production by using sunlight, and is suitable for the field of new energy development.

Description

One-dimensional composite nano photochemical catalyst and its preparation method and application
Technical field
The invention belongs to catalysis material technical field, specifically, relate to a kind of CdS:MoS being applied to photolysis water hydrogen 2one-dimensional composite nano photochemical catalyst and its preparation method and application.
Background technology
The environmental problem that mankind's activity makes energy resource consumption cause becomes increasingly conspicuous, and the resources such as petroleum gas only can maintain decades, and the clean new energy technology efficiently of development has been extremely urgent.Photocatalysis is using its room temperature deep reaction and can directly utilize solar energy as characteristics such as light source drivings, becomes a kind of desirable clear energy sources production technology.Since Fujishima and Honda professor in 1972 utilizes titanium dioxide electrodes can since decomposition water generates hydrogen and oxygen under ultraviolet lighting, photocatalysis technology just causes the extensive concern of various countries scientist.
Through the research of decades, this technology makes important progress in photolysis water hydrogen, but efficient visible light catalysis product hydrogen is one of bottleneck of its development of restriction.Therefore the visible light-responded catalyst that lasting research allotment has appropriate band position is the research emphasis promoting that photocatalysis technology further develops.Research shows, MoS 2as auxiliary agent excellent in photolysis water hydrogen reaction, can increase substantially the hydrogen manufacturing performance of catalyst.The Dalian Chemical Physics Research Institute scientific research personnel CdS/MoS that utilized high temperature sintering technique to prepare 2compound produces hydrogen photochemical catalyst, but this preparation method's temperature is higher, is unfavorable for the structure regulating of catalyst and the further investigation of its architecture element.Utilize the stratiform MoS of atomic thickness 2the research significantly improving the one-dimensional composite nano structure photochemical catalyst of hydrogen generation efficiency has no report.
Summary of the invention
The object of the present invention is to provide a kind of one-dimensional composite nano photochemical catalyst and its preparation method and application, significantly improve the efficiency utilizing sunshine hydrogen manufacturing.
For solving the problems of the technologies described above, the present invention is achieved by the following technical solutions:
On the one hand, the invention provides a kind of one-dimensional composite nano photochemical catalyst, this photochemical catalyst is atomic layers thick MoS 2the one-dimensional CdS nanorod structure modified, molybdenum bisuphide auxiliary agent individual layer loads on cadmium sulfide, and expression formula is CdS:MoS 2.
On the other hand, the invention provides a kind of preparation method of above-mentioned one-dimensional composite nano photochemical catalyst, comprise the following steps:
(1) MoS 2the preparation of presoma four thio ammonium molybdate (ATTM): appropriate ammonium molybdate is dissolved in concentrated ammonia liquor and is mixed with saturated solution; Get this saturated solution of certain volume to join in there-necked flask, and add excessive ammonium sulfide solution, 50-90 DEG C of reaction 1-12 h, naturally cools to room temperature, adds alcohol crystal 0.5-12 h, namely obtain MoS under magnetic stirring 2presoma four thio ammonium molybdate;
(2) CdS presoma Cd (S 2cNEt 2) 2preparation: respectively cadmium nitrate and DDTC are dissolved in suitable quantity of water by the mol ratio of 1:2, then under magnetic stirring the DDTC aqueous solution are slowly dropped in the cadmium nitrate aqueous solution, namely obtain CdS presoma Cd (S 2cNEt 2) 2;
(3) preparation of CdS nanometer rods: add the 70-80% of ethylenediamine to its volume in autoclave, then add Cd (S wherein 2cNEt 2) 2, it is reacted 6-48 h at 120-280 DEG C, namely obtains CdS nanometer rods; For avoiding the excessive generation of pressure in course of reaction dangerous, reaction vessel should all not be full of.
(4) CdS:MoS 2polyalcohol pressurization preparation: the ethylene glycol adding its volume capacity 60-80% in autoclave, then adds CdS nanometer rods and four thio ammonium molybdate that mass ratio is 2-12: 1, reacts 5-12 h after sealing at 180-220 DEG C;
(5) catalyst prepared by step (4) is placed in tube furnace, at N 2protection lower calcining 3-5 h, namely obtains CdS:MoS 2one-dimensional composite nano photochemical catalyst.
Further, the mass ratio of described CdS nanometer rods and four thio ammonium molybdate is 6: 1.
Further, in step (5), catalyst calcination temperature is 300-900 DEG C.
The invention also discloses the application of above-mentioned one-dimensional composite nano photochemical catalyst in photolysis water hydrogen.The present invention can be used for the photolysis water hydrogen of new forms of energy manufacture view, is the novel photocatalysis material meeting environmental protection and new forms of energy demand.
The preparation method of above-mentioned compound nanometer photocatalyst, specifically comprises the following steps:
(1) MoS 2the preparation of presoma four thio ammonium molybdate (ATTM): 0.05 mol ammonium molybdate is dissolved in 300 mL concentrated ammonia liquors and is mixed with saturated solution; Get this saturated solution of 21.0 mL to join in there-necked flask, and add 70.0 mL ammonium sulfide solutions.80 DEG C of reaction 1 h under magnetic stirring.Naturally cool to room temperature, add alcohol crystal 3 h and namely obtain MoS 2precursor A TTM.
(2) CdS presoma Cd (S 2cNEt 2) 2preparation: respectively by 3.0805 g Cd (NO 3) 24H 2o and 4.8094 g DDTC (C 5h 10nS 2na 3H 2o) be dissolved in 40 mL and 30 mL water, then under magnetic stirring the DDTC aqueous solution slowly dropped in the cadmium nitrate aqueous solution, namely obtain CdS presoma Cd (S 2cNEt 2) 2.
(3) preparation of CdS nanometer rods: add 35 mL ethylenediamines in 50 mL autoclaves, then adds 0.9872 g Cd (S wherein 2cNEt 2) 2, it is reacted at 180 DEG C 24 h and namely obtains CdS nanometer rods.
(4) CdS:MoS 2polyalcohol pressurization preparation: 30-40 mL ethylene glycol joins the autoclave of capacity 50 mL, then adds CdS and ATTM, and the mass ratio making CdS and ATTM is 2-12: 1, reacts 5-12 h after sealing at 180-220 DEG C.
(5) catalyst prepared by step 4 is placed in tube furnace, at N 2calcine 3-5 h at protection, 300-900 DEG C, namely obtain CdS:MoS 2compound nanometer photocatalyst.
The present invention achieves CdS:MoS by simple polyalcohol condensation technique 2the synthesis of compound nanometer photocatalyst.First in ethylenediamine system, synthesized size uniform, the CdS nanometer rods of pattern rule, then made ATTM decomposition in situ on CdS obtain one-dimensional CdS by polyalcohol pressure reduction technology: MoS 2compound nanometer photocatalyst.
The present invention is to provide the 1-dimention nano semiconductor highly effective hydrogen yield photochemical catalyst that a kind of base metal is modified,
Can highly effective hydrogen yield when photolysis water hydrogen, this catalyst is the one dimension CdS semiconduct composite that atomic layers thick molybdenum bisuphide is modified.
Compared with prior art, advantage of the present invention and positive effect are:
The present invention has prepared atomic layers thick MoS by simple polyalcohol pressure reduction reaction 2the CdS:MoS modified 2one-dimensional composite nano structure, for the photochemical catalyst synthesis significantly improving hydrogen generation efficiency provides a kind of new approach, preparation method is simple, the CdS:MoS of gained 2compound nanometer photocatalyst has efficient photocatalytic water hydrogen manufacturing performance, has further developed the application of semiconductor catalyst in photolysis water hydrogen, and CdS:MoS 2compound nanometer photocatalyst has higher stability.
Accompanying drawing explanation
Fig. 1 is CdS:MoS prepared by embodiment 1 2the SEM picture of compound nanometer photocatalyst;
Fig. 2 is CdS:MoS prepared by embodiment 1 2the TEM picture of compound nanometer photocatalyst;
Fig. 3 is CdS:MoS prepared by embodiment 1 2the XRD spectra of compound nanometer photocatalyst;
Fig. 4 is CdS:MoS prepared by embodiment 1 2hydrogen manufacturing kinetic curve under compound nanometer photocatalyst simulated solar irradiation;
Fig. 5 is CdS:MoS prepared by embodiment 2 2the SEM picture of S compound nanometer photocatalyst;
Fig. 6 is CdS:MoS prepared by embodiment 2 2the TEM picture of compound nanometer photocatalyst;
Fig. 7 is CdS:MoS under embodiment 2 simulated solar irradiation 2compound nanometer photocatalyst hydrogen manufacturing kinetic curve;
Fig. 8 is MoS 2load capacity and CdS:MoS 2the hydrogen production rate relation curve of compound nanometer photocatalyst;
Fig. 9 is CdS:MoS 2the calcining heat of compound nanometer photocatalyst and hydrogen production rate relation curve.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Embodiment 1
CdS:MoS 2the preparation of compound nanometer photocatalyst
(1) MoS 2the preparation of presoma four thio ammonium molybdate (ATTM): 0.05 mol ammonium molybdate is dissolved in 300 mL concentrated ammonia liquors and is mixed with saturated solution; Get this saturated solution of 21.0 mL to join in there-necked flask, and add 70.0 mL ammonium sulfide solutions.80 DEG C of reaction 1 h under magnetic stirring.Naturally cool to room temperature, add alcohol crystal 3 h and namely obtain MoS 2precursor A TTM.
(2) CdS presoma Cd (S 2cNEt 2) 2preparation: respectively by 3.0805 g cadmium nitrate (Cd (NO 3) 24H 2o) and 4.8094 g DDTC (C 5h 10nS 2na 3H 2o) be dissolved in 40 mL and 30 mL water, then under magnetic stirring the DDTC aqueous solution slowly dropped to Cd (NO 3) 2in the aqueous solution, namely obtain CdS presoma Cd (S 2cNEt 2) 2.
(3) preparation of CdS nanometer rods: add 35 mL ethylenediamines in 50 mL autoclaves, then adds 0.9872 g Cd (S wherein 2cNEt 2) 2, it is reacted at 180 DEG C 24 h and namely obtains CdS nanometer rods.
(4) CdS:MoS 2polyalcohol pressurization preparation: 40 mL ethylene glycol join the autoclave of capacity 50 mL, then add CdS and ATTM, and the mass ratio making CdS and ATTM is 6: 1, reacts 5 h after sealing at 180 DEG C.
Fig. 1 is CdS:MoS prepared by embodiment 1 2the SEM picture of compound nanometer photocatalyst, can find out the CdS:MoS of synthesis 2compound nanometer photocatalyst is one-dimensional nano structure, and appearance and size is comparatively homogeneous.
Fig. 2 is CdS:MoS prepared by embodiment 1 2the TEM picture of compound nanometer photocatalyst, due to MoS 2crystallization degree is lower, fails to observe obvious lattice fringe.
Fig. 3 is CdS:MoS prepared by embodiment 1 2the XRD spectra of compound nanometer photocatalyst, due to the MoS obtained under this condition 2crystallization degree is lower, particle diameter is less, does not occur obvious MoS 2characteristic diffraction peak.
CdS:MoS 2compound nanometer photocatalyst sunshine hydrogen manufacturing performance
By the CdS:MoS of 0.05 g embodiment 1 gained 2compound nanometer photocatalyst is dispersed in the 60 mL aqueous solution, then 2.64 g sodium sulfites and 3.62 g vulcanized sodium are added, LabSolar-III AG photocatalysis on-line analysis system carries out photolysis water hydrogen experiment, with 300 W xenon lamps as simulated solar radiant, product adopts gas-chromatography to carry out on-line checkingi.
Fig. 4 is CdS:MoS prepared by embodiment 1 2compound nanometer photocatalyst is hydrogen manufacturing kinetic curve under simulated solar irradiation, and as seen from the figure, along with the prolongation of light application time, the output of hydrogen increases gradually, and average hydrogen-producing speed is 2.6 mL/h.
Embodiment 2
(1) MoS 2the preparation of presoma four thio ammonium molybdate (ATTM): 0.05 mol ammonium molybdate is dissolved in 300 mL concentrated ammonia liquors and is mixed with saturated solution; Get this saturated solution of 21.0 mL to join in there-necked flask, and add 70.0 mL ammonium sulfide solutions.80 DEG C of reaction 1 h under magnetic stirring.Naturally cool to room temperature, add alcohol crystal 3 h and namely obtain MoS 2precursor A TTM.
(2) CdS presoma Cd (S 2cNEt 2) 2preparation: respectively by 3.0805 g cadmium nitrate (Cd (NO 3) 24H 2o) and 4.8094 g DDTC (C 5h 10nS 2na 3H 2o) be dissolved in 40 mL and 30 mL water, then under magnetic stirring the DDTC aqueous solution slowly dropped to Cd (NO 3) 2in the aqueous solution, namely obtain CdS presoma Cd (S 2cNEt 2) 2.
(3) preparation of CdS nanometer rods: add 35 mL ethylenediamines in 50 mL autoclaves, then adds 0.9872 g Cd (S wherein 2cNEt 2) 2, it is reacted at 180 DEG C 24 h and namely obtains CdS nanometer rods.
(4) CdS:MoS 2polyalcohol pressurization preparation: 40 mL ethylene glycol join the autoclave of capacity 50 mL, then add CdS and ATTM, and the mass ratio making CdS and ATTM is 6: 1, reacts 5 h after sealing at 180 DEG C.
(5) catalyst prepared by step 4 is placed in tube furnace, at N 2protection, calcine 3 h at 500 DEG C, namely obtain CdS:MoS 2compound nanometer photocatalyst.
Fig. 5 is CdS:MoS prepared by embodiment 2 2the SEM picture of compound nanometer photocatalyst, can find out the CdS:MoS of synthesis 2compound nanometer photocatalyst is 1-dimention nano line structure, and appearance and size is comparatively homogeneous.
Fig. 6 is CdS:MoS prepared by embodiment 2 2the TEM picture of compound nanometer photocatalyst, can find out the CdS:MoS of synthesis 2compound nanometer photocatalyst is 1-dimention nano line structure, and loads to the MoS on CdS 2for individual layer, interface is comparatively clear.
CdS:MoS 2compound nanometer photocatalyst sunshine hydrogen manufacturing performance
By the CdS:MoS of 0.05 g embodiment 2 gained 2compound nanometer photocatalyst is dispersed in the 60 mL aqueous solution, then 2.64 g sodium sulfites and 3.62 g vulcanized sodium are added, LabSolar-III AG photocatalysis on-line analysis system carries out photolysis water hydrogen experiment, with 300W xenon lamp as simulated solar radiant, product adopts gas-chromatography to carry out on-line checkingi.
Fig. 7 is the CdS:MoS prepared under embodiment 2 simulated solar irradiation 2compound nanometer photocatalyst hydrogen manufacturing kinetic curve, as seen from the figure, along with the prolongation of light application time, the output of hydrogen increases gradually, and average hydrogen-producing speed reaches 3.6 mL/h, the CdS:MoS that hydrogen generation efficiency is not calcined 2compound nanometer photocatalyst increases, and this is by calcining rear MoS 2crystallization degree improve, Adsorption increase caused by.
Fig. 8 shows MoS 2when addition is 10%, hydrogen generation efficiency is the highest; Fig. 9 illustrates that calcining heat is 500 oduring C, catalyst hydrogen generation efficiency is better.
From the result of embodiment 1 and 2, embodiment 1 product is not calcined, therefore crystallization degree is low; Embodiment 2 is improved through calcining post crystallization degree, and Adsorption increases, and photolysis water hydrogen efficiency is also improved.
The above is only preferred embodiment of the present invention, and be not restriction the present invention being made to other form, any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the Equivalent embodiments of equivalent variations.But everyly do not depart from technical solution of the present invention content, any simple modification, equivalent variations and the remodeling done above embodiment according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.

Claims (2)

1. a preparation method for one-dimensional composite nano photochemical catalyst, is characterized in that, comprises the following steps:
(1) MoS 2the preparation of presoma four thio ammonium molybdate: appropriate ammonium molybdate is dissolved in concentrated ammonia liquor and is mixed with saturated solution; Get this saturated solution of certain volume to join in there-necked flask, and add excessive ammonium sulfide solution, 50-90 DEG C of reaction 1-12 h, naturally cools to room temperature, adds alcohol crystal 0.5-12 h, namely obtain MoS under magnetic stirring 2presoma four thio ammonium molybdate;
(2) CdS presoma Cd (S 2cNEt 2) 2preparation: respectively cadmium nitrate and DDTC are dissolved in suitable quantity of water by the mol ratio of 1:2, then under magnetic stirring the DDTC aqueous solution are slowly dropped in the cadmium nitrate aqueous solution, namely obtain CdS presoma Cd (S 2cNEt 2) 2;
(3) preparation of CdS nanometer rods: add the 70-80% of ethylenediamine to its volume in autoclave, then add Cd (S wherein 2cNEt 2) 2, it is reacted 6-48 h at 120-280 DEG C, namely obtains CdS nanometer rods;
(4) CdS:MoS 2polyalcohol pressurization preparation: the ethylene glycol adding its volume capacity 60-80% in autoclave, then adds CdS nanometer rods and four thio ammonium molybdate that mass ratio is 2-12: 1, reacts 5-12 h after sealing at 180-220 DEG C;
(5) catalyst prepared by step (4) is placed in tube furnace, at N 2protection lower calcining 3-5 h, namely obtains CdS:MoS 2one-dimensional composite nano photochemical catalyst, this catalyst is atomic layers thick MoS 2the one-dimensional CdS nanorod structure modified.
2. the preparation method of one-dimensional composite nano photochemical catalyst according to claim 1, it is characterized in that, the mass ratio of described CdS nanometer rods and four thio ammonium molybdate is 6: 1.
3 .according to claim 1, the preparation method of one-dimensional composite nano photochemical catalyst, is characterized in that, in step (5), catalyst calcination temperature is 300-900 DEG C.
4 .the application of one-dimensional composite nano photochemical catalyst in photolysis water hydrogen that in the claims 1-3, preparation method described in any one obtains.
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