CN103566953A - 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 PDFInfo
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- CN103566953A CN103566953A CN201310614267.5A CN201310614267A CN103566953A CN 103566953 A CN103566953 A CN 103566953A CN 201310614267 A CN201310614267 A CN 201310614267A CN 103566953 A CN103566953 A CN 103566953A
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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
Technical field
The invention belongs to catalysis material technical field, specifically, relate to a kind of CdS:MoS that is applied to photolysis water hydrogen
2one-dimensional composite nano photochemical catalyst and its preparation method and application.
Background technology
Mankind's activity becomes increasingly conspicuous the environmental problem that energy resource consumption causes, and the resources such as petroleum gas only can maintain decades, and the clean new energy technology efficiently of development has been extremely urgent.Its room temperature deep reaction and can directly utilize solar energy as characteristics such as light source drivings is usingd in photocatalysis, becomes a kind of desirable clear energy sources production technology.Since Fujishima in 1972 and professor Honda utilize titanium dioxide electrodes can decomposition water under ultraviolet lighting to generate hydrogen and oxygen, photocatalysis technology has just caused various countries scientists' extensive concern.
Through the research of decades, this technology makes important progress aspect 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 suitable position of energy band is the research emphasis that promotes that photocatalysis technology further develops.Research shows, MoS
2can be used as good auxiliary agent in photolysis water hydrogen reaction, can increase substantially the hydrogen manufacturing performance of catalyst.The scientific research personnel of Dalian Chemical Physics Research Institute utilizes high temperature sintering technology to prepare CdS/MoS
2compound product 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 structure sexual intercourse.Utilize the stratiform MoS of atomic thickness
2the research that significantly improves the one-dimensional composite nano structured light 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 of 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 of modifying, 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 and join in there-necked flask, and add excessive ammonium sulfide solution, under magnetic agitation, 50-90 ℃ of reaction 1-12 h, naturally cools to room temperature, adds alcohol crystal 0.5-12 h, obtains MoS
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 agitation, the DDTC aqueous solution are slowly dropped in the cadmium nitrate aqueous solution, obtain CdS presoma Cd (S
2cNEt
2)
2;
(3) preparation of CdS nanometer rods: add ethylenediamine to the 70-80% of its volume in autoclave, then add wherein Cd (S
2cNEt
2)
2, it is reacted at 120-280 ℃ to 6-48 h, obtain CdS nanometer rods; For avoiding the excessive generation danger of pressure in course of reaction, reaction vessel should all not be full of.
(4) CdS:MoS
2polyalcohol pressurization preparation: in autoclave, add the ethylene glycol of its volume capacity 60-80%, then adding mass ratio is 2-12: 1 CdS nanometer rods and four thio ammonium molybdate, after sealing, at 180-220 ℃, react 5-12 h;
(5) catalyst of being prepared by step (4) is placed in tube furnace, at N
2the lower calcining 3-5 of protection h, 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 ℃.
The invention also discloses the application of above-mentioned one-dimensional composite nano photochemical catalyst aspect 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 that meets environmental protection and new forms of energy demand.
The preparation method of above-mentioned composite Nano photochemical catalyst, 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 and join in there-necked flask, and add 70.0 mL ammonium sulfide solutions.80 ℃ of reaction 1 h under magnetic agitation.Naturally cool to room temperature, add alcohol crystal 3 h and 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 agitation, the DDTC aqueous solution slowly dropped in the cadmium nitrate aqueous solution, obtain CdS presoma Cd (S
2cNEt
2)
2.
(3) preparation of CdS nanometer rods: add 35 mL ethylenediamines in 50 mL autoclaves, then add wherein 0.9872 g Cd (S
2cNEt
2)
2, it is reacted at 180 ℃ to 24 h and 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 that makes CdS and ATTM is 2-12: 1, after sealing, at 180-220 ℃, react 5-12 h.
(5) catalyst of step 4 preparation is placed in to tube furnace, at N
2at protection, 300-900 ℃, calcine 3-5 h, obtain CdS:MoS
2composite Nano photochemical catalyst.
The present invention has realized CdS:MoS by simple polyalcohol pressurization technology
2synthesizing of composite Nano photochemical catalyst.First in ethylenediamine system, synthesized size uniform, the CdS nanometer rods of pattern rule, then makes ATTM decomposition in situ on CdS obtain one-dimensional CdS by polyalcohol pressure reduction technology: MoS
2composite Nano photochemical catalyst.
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 modifying
2one-dimensional composite nano structure, in order significantly to improve, the photochemical catalyst of hydrogen generation efficiency is synthetic provides a kind of new approach, and preparation method is simple, the CdS:MoS of gained
2composite Nano photochemical catalyst has efficient photodissociation water hydrogen manufacturing performance, has further developed the application of semiconductor catalyst aspect photolysis water hydrogen, and CdS:MoS
2composite Nano photochemical catalyst has higher stability.
Accompanying drawing explanation
Fig. 1 is the CdS:MoS of embodiment 1 preparation
2the SEM picture of composite Nano photochemical catalyst;
Fig. 2 is the CdS:MoS of embodiment 1 preparation
2the TEM picture of composite Nano photochemical catalyst;
Fig. 3 is the CdS:MoS of embodiment 1 preparation
2the XRD spectra of composite Nano photochemical catalyst;
Fig. 4 is the CdS:MoS of embodiment 1 preparation
2hydrogen manufacturing kinetic curve under composite Nano photochemical catalyst simulated solar irradiation;
Fig. 5 is the CdS:MoS of embodiment 2 preparations
2the SEM picture of S composite Nano photochemical catalyst;
Fig. 6 is the CdS:MoS of embodiment 2 preparations
2the TEM picture of composite Nano photochemical catalyst;
Fig. 7 is CdS:MoS under embodiment 2 simulated solar irradiations
2composite Nano photochemical catalyst hydrogen manufacturing kinetic curve;
Fig. 8 is MoS
2load capacity and CdS:MoS
2the hydrogen manufacturing Rate Relationship curve of composite Nano photochemical catalyst;
Fig. 9 is CdS:MoS
2the calcining heat of composite Nano photochemical catalyst and hydrogen manufacturing Rate Relationship curve.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Embodiment 1
CdS:MoS
2the preparation of composite Nano photochemical catalyst
(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 and join in there-necked flask, and add 70.0 mL ammonium sulfide solutions.80 ℃ of reaction 1 h under magnetic agitation.Naturally cool to room temperature, add alcohol crystal 3 h and 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 agitation, the DDTC aqueous solution slowly dropped to Cd (NO
3)
2in the aqueous solution, obtain CdS presoma Cd (S
2cNEt
2)
2.
(3) preparation of CdS nanometer rods: add 35 mL ethylenediamines in 50 mL autoclaves, then add wherein 0.9872 g Cd (S
2cNEt
2)
2, it is reacted at 180 ℃ to 24 h and 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 making the mass ratio of CdS and ATTM is 6: 1, react 5 h after sealing at 180 ℃.
Fig. 1 is the CdS:MoS of embodiment 1 preparation
2the SEM picture of composite Nano photochemical catalyst, can find out synthetic CdS:MoS
2composite Nano photochemical catalyst is one-dimensional nano structure, and appearance and size is homogeneous comparatively.
Fig. 2 is the CdS:MoS of embodiment 1 preparation
2the TEM picture of composite Nano photochemical catalyst, due to MoS
2crystallization degree is lower, fails to observe obvious lattice fringe.
Fig. 3 is the CdS:MoS of embodiment 1 preparation
2the XRD spectra of composite Nano photochemical catalyst, due to the MoS obtaining under this condition
2crystallization degree is lower, particle diameter is less, does not occur obvious MoS
2characteristic diffraction peak.
CdS:MoS
2composite Nano photochemical catalyst sunshine hydrogen manufacturing performance
By the CdS:MoS of 0.05 g embodiment 1 gained
2composite Nano photochemical catalyst is dispersed in the 60 mL aqueous solution, then add 2.64 g sodium sulfites and 3.62 g vulcanized sodium, on LabSolar-III AG photocatalysis on-line analysis system, carry out photolysis water hydrogen experiment, with 300 W xenon lamps, as simulated solar radiant, product adopts gas-chromatography to detect online.
Fig. 4 is the CdS:MoS of embodiment 1 preparation
2composite Nano photochemical catalyst 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.
(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 and join in there-necked flask, and add 70.0 mL ammonium sulfide solutions.80 ℃ of reaction 1 h under magnetic agitation.Naturally cool to room temperature, add alcohol crystal 3 h and 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 agitation, the DDTC aqueous solution slowly dropped to Cd (NO
3)
2in the aqueous solution, obtain CdS presoma Cd (S
2cNEt
2)
2.
(3) preparation of CdS nanometer rods: add 35 mL ethylenediamines in 50 mL autoclaves, then add wherein 0.9872 g Cd (S
2cNEt
2)
2, it is reacted at 180 ℃ to 24 h and 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 making the mass ratio of CdS and ATTM is 6: 1, react 5 h after sealing at 180 ℃.
(5) catalyst of step 4 preparation is placed in to tube furnace, at N
2protection, calcine 3 h at 500 ℃, obtain CdS:MoS
2composite Nano photochemical catalyst.
Fig. 5 is the CdS:MoS of embodiment 2 preparations
2the SEM picture of composite Nano photochemical catalyst, can find out synthetic CdS:MoS
2composite Nano photochemical catalyst is 1-dimention nano line structure, and appearance and size is homogeneous comparatively.
Fig. 6 is the CdS:MoS of embodiment 2 preparations
2the TEM picture of composite Nano photochemical catalyst, can find out synthetic CdS:MoS
2composite Nano photochemical catalyst is 1-dimention nano line structure, and loads to the MoS on CdS
2for individual layer, interface is comparatively clear.
CdS:MoS
2composite Nano photochemical catalyst sunshine hydrogen manufacturing performance
By the CdS:MoS of 0.05 g embodiment 2 gained
2composite Nano photochemical catalyst is dispersed in the 60 mL aqueous solution, then add 2.64 g sodium sulfites and 3.62 g vulcanized sodium, on LabSolar-III AG photocatalysis on-line analysis system, carry out photolysis water hydrogen experiment, with 300W xenon lamp, as simulated solar radiant, product adopts gas-chromatography to detect online.
Fig. 7 is the CdS:MoS preparing under embodiment 2 simulated solar irradiations
2composite Nano photochemical catalyst 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
2composite Nano photochemical catalyst increases, and this is by MoS after calcining
2crystallization degree improve, due to Adsorption increases.
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 improves through calcining post crystallization degree, and Adsorption increases, and photolysis water hydrogen efficiency is also improved.
The above, be only preferred embodiment of the present invention, is not the present invention to be done to the restriction of other form, and any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the equivalent embodiment of equivalent variations.But every technical solution of the present invention content that do not depart from, any simple modification, equivalent variations and the remodeling above embodiment done according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (5)
1. an one-dimensional composite nano photochemical catalyst, is characterized in that: described catalyst is atomic layers thick MoS
2the one-dimensional CdS nanorod structure of modifying, expression formula is CdS:MoS
2.
2. a preparation method for one-dimensional composite nano photochemical catalyst described in claim 1, 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 and join in there-necked flask, and add excessive ammonium sulfide solution, under magnetic agitation, 50-90 ℃ of reaction 1-12 h, naturally cools to room temperature, adds alcohol crystal 0.5-12 h, obtains MoS
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 agitation, the DDTC aqueous solution are slowly dropped in the cadmium nitrate aqueous solution, obtain CdS presoma Cd (S
2cNEt
2)
2;
(3) preparation of CdS nanometer rods: add ethylenediamine to the 70-80% of its volume in autoclave, then add wherein Cd (S
2cNEt
2)
2, it is reacted at 120-280 ℃ to 6-48 h, obtain CdS nanometer rods;
(4) CdS:MoS
2polyalcohol pressurization preparation: in autoclave, add the ethylene glycol of its volume capacity 60-80%, then adding mass ratio is 2-12: 1 CdS nanometer rods and four thio ammonium molybdate, after sealing, at 180-220 ℃, react 5-12 h;
(5) catalyst of being prepared by step (4) is placed in tube furnace, at N
2the lower calcining 3-5 of protection h, obtains CdS:MoS
2one-dimensional composite nano photochemical catalyst.
3. the preparation method of one-dimensional composite nano photochemical catalyst according to claim 2, is characterized in that, the mass ratio of described CdS nanometer rods and four thio ammonium molybdate is 6: 1.
4. the preparation method of one-dimensional composite nano photochemical catalyst according to claim 2, is characterized in that, in step (5), catalyst calcination temperature is 300-900 ℃.
5. the application of above-mentioned one-dimensional composite nano photochemical catalyst aspect photolysis water hydrogen.
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