CN105126844A - Molybdenum disulfide/silver vanadate visible light composite catalyst and preparation method thereof - Google Patents

Molybdenum disulfide/silver vanadate visible light composite catalyst and preparation method thereof Download PDF

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CN105126844A
CN105126844A CN201510478901.6A CN201510478901A CN105126844A CN 105126844 A CN105126844 A CN 105126844A CN 201510478901 A CN201510478901 A CN 201510478901A CN 105126844 A CN105126844 A CN 105126844A
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visible light
preparation
molybdenum bisuphide
silver
light composite
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许晖
朱婷婷
李华明
颜佳
徐远国
宋艳华
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Jiangsu University
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Jiangsu University
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Abstract

The present invention provides a molybdenum disulfide/silver vanadate visible light composite catalyst and a preparation method thereof, and belongs to the technical field of composite materials and photocatalysis in environmental governance, wherein MoS2 and Ag3VO4 are compounded according to a mass ratio of 1:99-10:90 to obtain the material, and MoS2 particles are uniformly dispersed on the Ag3VO4 surface to form a heterojunction structure. According to the preparation method, graphene-like molybdenum disulfide is placed in an aqueous solution to carry out ultrasonic dispersing to obtain a graphene-like molybdenum disulfide dispersion A; silver nitrate solid particles are added to the obtained dispersion A, and shading stirring is performed in the case of water bath temperature control to completely dissolve the silver nitrate so as to obtain a dispersion B; and a prepared sodium vanadate aqueous solution is slowly added to the obtained dispersion B in a dropwise manner, and shading stirring is continuously performed after the adding so as to obtain the product. According to the present invention, the composite photocatalyst provides a good degradation effect on methylene blue under visible light, the preparation process is performed at a room temperature, the energy consumption is low, the cost is low, the synthesis condition is the room temperature and is easy to achieve, and the method is suitable for large-scale preparation.

Description

A kind of molybdenum bisuphide/silver vanadate visible light composite photocatalyst and preparation method thereof
Technical field
The present invention relates to photochemical catalyst, refer in particular to a kind of molybdenum bisuphide/silver vanadate compounded visible light photocatalyst and preparation method thereof, belong to photocatalysis technology field in composite and environmental improvement.
Background technology
Along with developing rapidly of modern industry, global energy shortage and environment deterioration problem highlight day by day, the existence of serious threat to the mankind and the sustainable development of society.But in many environmental problems, toxicity is large, the removal of persistence organic pollutant is a difficult problem always.In view of the characteristic of its low energy consumption and green, photocatalysis technology degradable organic pollutant becomes an active research direction, under optical excitation, utilize the physical property of semiconductor that light energy conversion is become chemical energy, under relatively mild condition, degradable organic pollutant is inorganic molecules, and can not secondary pollution be brought, comparing with chemical method with traditional physical method has incomparable advantage, and the research wherein for visible light responsive photocatalytic material attracts wide attention especially.
Ag 3vO 4as a kind of novel visible responsive photocatalyst, under photolysis water hydrogen and visible ray, in degradable organic pollutant, there is excellent performance.Because electron recombination rate is high and photocatalytic activity is low, Ag 3vO 4the application of monomer is limited.Pass through Ag 3vO 4other photochemical catalysts that adulterate carry out modification, are the effective ways improving its visible light catalysis activity further.In this year, the Synthesis and applications of nano transition metal disulphide receives much concern.Molybdenum bisuphide is due to its intrinsic class Graphene layer structure, and the interaction of interlayer Van der Waals force, specific area is large, and having catalytic activity group, is a kind of good co-catalyst.Therefore, the invention provides a kind of MoS 2/ Ag 3vO 4composite photo-catalyst and preparation method thereof, its objective is and improve silver vanadate in the photocatalytic activity of visible region and stability by the load of elemental silver.
Summary of the invention
The present invention utilizes MoS 2application prospect widely in electricity and optics, provides a kind of visible-light response type MoS improving photocatalytic activity and specific area 2/ Ag 3vO 4composite photo-catalyst and preparation method thereof; The course of reaction of the method only needs at room temperature to carry out, and achieves the pattern of Effective Regulation silver vanadate in course of reaction, solve existing photochemical catalyst not high to visible ray utilization rate, to problems such as high concentrations of organic dye degradation efficiency are low.
The technical solution realizing the object of the invention is:
A kind of molybdenum bisuphide/silver vanadate visible light composite photocatalyst MoS 2/ Ag 3vO 4, be the MoS of 1:99 ~ 10:90 by mass ratio 2and Ag 3vO 4be composited; MoS 2evengranularly be dispersed in Ag 3vO 4surface forms heterojunction structure; Composite photo-catalyst is carried out photocatalytic degradation to 10mg/L methylene blue under visible light, and at front 12min to methylene blue fast degradation, after 18min, the degradation rate of this photochemical catalyst to methylene blue reaches 92%.
A preparation method for molybdenum bisuphide/silver vanadate visible light composite photocatalyst, comprises the steps:
Step 1, class Graphene molybdenum bisuphide is placed in aqueous solution ultrasonic disperse, obtains the dispersion liquid A of class Graphene molybdenum bisuphide;
Step 2, added in step 1 gained dispersion liquid A by silver nitrate solid particle, shading is stirred to silver nitrate and fully dissolves, and obtains dispersion liquid B;
Step 3, the sodium vanadate aqueous solution prepared dropwise slowly to be joined in the dispersion liquid B of step 2 gained, after being added dropwise to complete, obtain dispersion liquid C, continue shading dispersed with stirring liquid C, obtain product;
Step 4, product step 3 obtained leave standstill, and then centrifuge washing is dry, namely obtains photochemical catalyst MoS 2/ Ag 3vO 4.
In described step 1, in dispersion liquid A, the concentration of molybdenum bisuphide is 0.208 ~ 3.1mg/mL.
In described step 2, in dispersion liquid B, the concentration of silver nitrate is 51mg/mL.
In described step 3, sodium vanadate aqueous solution volume: dispersion liquid B volume is 4:5, sodium vanadate concentration of aqueous solution is 50mg/mL.
The ultrasonic disperse time of described step 1 is 30 ~ 40min.
The mixing time of described step 2 is 30 ~ 40min.
Mixing time in described step 3 is 240min.
The time of repose of described step 4 is 0.5 ~ 1h, and baking temperature is 35 ~ 50 DEG C, and drying time is 4 ~ 6h.
Step 1 ~ 3 are all at room temperature carried out.
Compared with prior art, its remarkable advantage is in the present invention:
(1) class Graphene molybdenum bisuphide is utilized to carry out modification to silver vanadate photochemical catalyst, and obtain a kind Graphene molybdenum bisuphide/silver vanadate composite, the formation of its heterojunction structure, is conducive to being separated of light induced electron and hole, improves photocatalytic activity; Can 92% be reached to the degraded of methylene blue in 18min.
(2) preparation method of molybdenum bisuphide of the present invention/silver vanadate composite is simple, and preparation process is all at room temperature carried out, and energy consumption is low, with low cost, easily realizes, and is conducive to extensive preparation.
Accompanying drawing explanation
Fig. 1 is MoS obtained by embodiment 1 2/ Ag 3vO 4the XRD figure of composite photo-catalyst;
Fig. 2 is MoS obtained by embodiment 1 2/ Ag 3vO 4the IR spectrogram of composite photo-catalyst;
Fig. 3 is MoS obtained by embodiment 1 2/ Ag 3vO 4the impedance diagram of composite photo-catalyst;
Fig. 4 is MoS obtained by embodiment 1 2/ Ag 3vO 4composite photo-catalyst is the photocatalytic degradation of methylene blue curve map of 10mg/L to concentration under different visible light irradiation time.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is set forth in further detail.
Embodiment 1:
Visible light-responded MoS of the present invention 2/ Ag 3vO 4the preparation method of composite photo-catalyst, specifically comprises the following steps:
The first step, is placed in 50mL aqueous solution ultrasonic disperse 30 minutes by 0.0104g class Graphene molybdenum bisuphide, obtains the dispersion liquid of class Graphene molybdenum bisuphide;
Second step, adds 2.55g silver nitrate solid particle in first step gained dispersion liquid, and in 25 DEG C of water-bath situations, 30min is stirred in shading, fully dissolves to silver nitrate;
3rd step, dropwise slowly joins the sodium radio-phosphate,P-32 solution prepared (containing 2g sodium vanadate, 40mL deionized water) in the solution of second step gained, is added dropwise to complete rear continuation shading and stirs 240min, obtain product;
4th step, leaves standstill 1h by the product that three-step reaction obtains, centrifugal, and washing, dry 6h at 50 DEG C, can obtain MoS 2/ Ag 3vO 4photochemical catalyst.
Embodiment 2:
Visible light-responded MoS of the present invention 2/ Ag 3vO 4close the preparation method of photochemical catalyst, specifically comprise the following steps:
The first step, is placed in 50mL aqueous solution ultrasonic disperse 40 minutes by 0.0431g class Graphene molybdenum bisuphide, obtains the dispersion liquid of class Graphene molybdenum bisuphide;
Second step, adds 2.55g silver nitrate solid particle in first step gained dispersion liquid, and in 25 DEG C of water-bath situations, 40min is stirred in shading, fully dissolves to silver nitrate;
3rd step, dropwise slowly joins the sodium radio-phosphate,P-32 solution prepared (containing 2g sodium vanadate, 40mL deionized water) in the solution of second step gained, is added dropwise to complete rear continuation shading and stirs 240min, obtain product;
4th step, leaves standstill 0.5h by the product that three-step reaction obtains, centrifugal, and washing, dry 6h at 35 DEG C, can obtain MoS 2/ Ag 3vO 4photochemical catalyst.
Embodiment 3:
Visible light-responded MoS of the present invention 2/ Ag 3vO 4close the preparation method of photochemical catalyst, specifically comprise the following steps:
The first step, is placed in 50mL aqueous solution ultrasonic disperse 30 minutes by 0.0778g class Graphene molybdenum bisuphide, obtains the dispersion liquid of class Graphene molybdenum bisuphide;
Second step, adds 2.55g silver nitrate solid particle in first step gained dispersion liquid, and in 25 DEG C of water-bath situations, 30min is stirred in shading, fully dissolves to silver nitrate;
3rd step, dropwise slowly joins the sodium radio-phosphate,P-32 solution prepared (containing 2g sodium vanadate, 40mL deionized water) in the solution of second step gained, is added dropwise to complete rear continuation shading and stirs 240min, obtain product;
4th step, leaves standstill 1h by the product that three-step reaction obtains, centrifugal, and washing, dry 4h at 50 DEG C, can obtain MoS 2/ Ag 3vO 4photochemical catalyst.
Embodiment 4:
Visible light-responded MoS of the present invention 2/ Ag 3vO 4close the preparation method of photochemical catalyst, specifically comprise the following steps:
The first step, is placed in 50mL aqueous solution ultrasonic disperse 30 minutes by 0.115g class Graphene molybdenum bisuphide, obtains the dispersion liquid of class Graphene molybdenum bisuphide;
Second step, adds 2.55g silver nitrate solid particle in first step gained dispersion liquid, and in 25 DEG C of water-bath situations, 30min is stirred in shading, fully dissolves to silver nitrate;
3rd step, dropwise slowly joins the sodium radio-phosphate,P-32 solution prepared (containing 2g sodium vanadate, 40mL deionized water) in the solution of second step gained, is added dropwise to complete rear continuation shading and stirs 240min, obtain product;
4th step, leaves standstill 1h by the product that three-step reaction obtains, centrifugal, and washing, dry 4h at 50 DEG C, can obtain MoS 2/ Ag 3vO 4photochemical catalyst.
The MoS of Fig. 1 prepared by embodiment 1 2/ Ag 3vO 4the X-ray diffracting spectrum of composite visible light catalyst, diffraction maximums all in figure is all corresponding with silver vanadate standard card, because class Graphene molybdenum disulfide content is relatively less, and the silver vanadate very strong relative to the good diffraction maximum of crystallization, its X-ray diffraction peak cannot be observed in the drawings.
The infared spectrum of the graphite mould molybdenum bisuphide of Fig. 2 prepared by embodiment 1, silver vanadate, graphite mould molybdenum bisuphide/silver vanadate composite visible light catalyst.As can be seen from the figure, the characteristic peak representing graphite type carbon nitride and silver carbonate can find at composite visible light catalyst, this demonstrates graphite mould molybdenum bisuphide and silver vanadate is successfully combined with each other.
The MoS of Fig. 3 prepared by embodiment 1 2/ Ag 3vO 4the electrochemical impedance collection of illustrative plates of composite visible light catalyst, compared to silver vanadate monomer, MoS 2/ Ag 3vO 4there is relatively little semicircle.Therefore, interface charge transfer smoothly occurs in MoS 2/ Ag 3vO 4composite surface, facilitates the separative efficiency that photo-generate electron-hole is right.
The MoS of Fig. 4 prepared by embodiment 1 2/ Ag 3vO 4composite photo-catalyst is the photocatalytic degradation of methylene blue curve map of 10mg/L to concentration under different visible light irradiation time.As can be seen from the figure, this composite photo-catalyst is at front 12min to methylene blue energy fast degradation, and after 18min, the degradation rate of this photochemical catalyst to methylene blue reaches 92%.Contrast therewith, silver vanadate under visible light conditions to concentration be the degradation rate of the methylene blue of 10mg/L greatly about 25%, as can be seen here, the composite photo-catalyst synthesized by this example improves the photocatalysis performance of silver vanadate significantly.
Described embodiment is preferred embodiment of the present invention; but the present invention is not limited to above-mentioned embodiment; when not deviating from flesh and blood of the present invention, any apparent improvement that those skilled in the art can make, replacement or modification all belong to protection scope of the present invention.

Claims (10)

1. molybdenum bisuphide/silver vanadate visible light composite photocatalyst MoS 2/ Ag 3vO 4, it is characterized in that, described material is the MoS of 1:99 ~ 10:90 by mass ratio 2and Ag 3vO 4be composited; MoS 2evengranularly be dispersed in Ag 3vO 4surface forms heterojunction structure; This composite photo-catalyst is carried out photocatalytic degradation to 10mg/L methylene blue under visible light, and at front 12min to methylene blue fast degradation, after 18min, the degradation rate of this photochemical catalyst to methylene blue reaches 92%.
2. the preparation method of a kind of molybdenum bisuphide/silver vanadate visible light composite photocatalyst according to claim 1, is characterized in that, comprise the steps:
Step 1, class Graphene molybdenum bisuphide is placed in aqueous solution ultrasonic disperse, obtains the dispersion liquid A of class Graphene molybdenum bisuphide;
Step 2, added in step 1 gained dispersion liquid A by silver nitrate solid particle, shading is stirred to silver nitrate and fully dissolves, and obtains dispersion liquid B;
Step 3, the sodium vanadate aqueous solution prepared dropwise slowly to be joined in the dispersion liquid B of step 2 gained, after being added dropwise to complete, obtain dispersion liquid C, continue shading dispersed with stirring liquid C, obtain product;
Step 4, product step 3 obtained leave standstill, and then centrifuge washing is dry, namely obtains photochemical catalyst MoS 2/ Ag 3vO 4.
3. the preparation method of a kind of molybdenum bisuphide/silver vanadate visible light composite photocatalyst according to claim 2, is characterized in that, in step 1, in dispersion liquid A, the concentration of molybdenum bisuphide is 0.208 ~ 3.1mg/mL.
4. the preparation method of a kind of molybdenum bisuphide/silver vanadate visible light composite photocatalyst according to claim 2, is characterized in that, in step 2, in dispersion liquid B, the concentration of silver nitrate is 51mg/mL.
5. the preparation method of a kind of molybdenum bisuphide/silver vanadate visible light composite photocatalyst according to claim 2, is characterized in that, in step 3, sodium vanadate aqueous solution volume: dispersion liquid B volume is 4:5, sodium vanadate concentration of aqueous solution is 50mg/mL.
6. the preparation method of a kind of molybdenum bisuphide/silver vanadate visible light composite photocatalyst according to claim 2, is characterized in that, the ultrasonic disperse time of step 1 is 30 ~ 40min.
7. the preparation method of a kind of molybdenum bisuphide/silver vanadate visible light composite photocatalyst according to claim 2, is characterized in that, the mixing time of step 2 is 30 ~ 40min.
8. the preparation method of a kind of molybdenum bisuphide/silver vanadate visible light composite photocatalyst according to claim 2, is characterized in that, the mixing time in step 3 is 240min.
9. the preparation method of a kind of molybdenum bisuphide/silver vanadate visible light composite photocatalyst according to claim 2, is characterized in that, the time of repose of step 4 is 0.5 ~ 1h; Baking temperature is 35 ~ 50 DEG C, and drying time is 4 ~ 6h.
10. the preparation method of a kind of molybdenum bisuphide/silver vanadate visible light composite photocatalyst according to claim 2, it is characterized in that, step 1 ~ 3 are all at room temperature carried out.
CN201510478901.6A 2015-08-06 2015-08-06 Molybdenum disulfide/silver vanadate visible light composite catalyst and preparation method thereof Pending CN105126844A (en)

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CN108325494A (en) * 2018-02-08 2018-07-27 浙江睿升环保科技有限公司 A kind of high-performance Ag3VO4Compound difunctional catalysis materials of/BiOI and its preparation method and application
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CN112191258A (en) * 2020-11-10 2021-01-08 西安工程大学 Ternary plasma photocatalyst fiber for treating printing and dyeing wastewater and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN107837810A (en) * 2017-09-22 2018-03-27 江苏大学 A kind of Preparation method and use of heterojunction composite photocatalyst
CN108325494A (en) * 2018-02-08 2018-07-27 浙江睿升环保科技有限公司 A kind of high-performance Ag3VO4Compound difunctional catalysis materials of/BiOI and its preparation method and application
CN108262054A (en) * 2018-03-06 2018-07-10 内蒙古大学 A kind of preparation method of silver vanadate/nitride porous carbon heterojunction composite photocatalyst
CN108786873A (en) * 2018-07-05 2018-11-13 河南师范大学 A kind of MoS2/Ag2CO3The synthesis and application of heterojunction photocatalysis material
CN111744503A (en) * 2020-07-29 2020-10-09 自然资源部第一海洋研究所 Z-shaped heterojunction MoS2/Bi2WO6Composite photocatalyst and preparation method and application thereof
CN111774075A (en) * 2020-07-29 2020-10-16 自然资源部第一海洋研究所 BiOI/MoS2Heterojunction composite photocatalyst and preparation method and application thereof
CN112191258A (en) * 2020-11-10 2021-01-08 西安工程大学 Ternary plasma photocatalyst fiber for treating printing and dyeing wastewater and preparation method thereof
CN112191258B (en) * 2020-11-10 2022-12-09 西安工程大学 Ternary plasma photocatalyst fiber for treating printing and dyeing wastewater and preparation method thereof

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Application publication date: 20151209