CN103506142B - A kind of Molybdenum disulfide/silver phosphate composite visible light photocatalytic material and preparation method thereof - Google Patents
A kind of Molybdenum disulfide/silver phosphate composite visible light photocatalytic material and preparation method thereof Download PDFInfo
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- CN103506142B CN103506142B CN201310462452.7A CN201310462452A CN103506142B CN 103506142 B CN103506142 B CN 103506142B CN 201310462452 A CN201310462452 A CN 201310462452A CN 103506142 B CN103506142 B CN 103506142B
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Abstract
The present invention relates to catalysis material, refer in particular to a kind of visible light-responded class Graphene molybdenum bisuphide/silver phosphate composite photocatalyst and preparation method thereof.The present invention utilizes class Graphene molybdenum bisuphide to carry out modification to silver phosphate photocatalyst, and obtain a kind Graphene molybdenum bisuphide/silver orthophosphate composite, the absorption characteristic of silver orthophosphate at visible region can be increased substantially, secondly the preparation method of class Graphene molybdenum bisuphide/silver orthophosphate composite of the present invention is simple, cost is low, synthesis condition is gentle, is conducive to large-scale promotion; The composite of preparation has stronger optical absorption characteristics at visible region.
Description
Technical field
The present invention relates to catalysis material, refer in particular to a kind of visible light-responded class Graphene molybdenum bisuphide/silver phosphate composite photocatalyst and preparation method thereof, belong to photocatalysis technology field in composite and environmental improvement.
Background technology
From last century the seventies; the environmental pollution continued and energy shortage; cause the worry of people to global crisis; in order to realize the sustainable development of human society; develop a kind of new technology that not only can be used for environmental improvement but also can be used for prepared by clean energy resource; become a urgent and urgent task; photocatalysis technology is because of its application prospect wide in fields such as environmental protection, clean energy resourcies preparation (solar energy is converted into Hydrogen Energy); and paid much attention to, become a kind of technology having application prospect.
The key of photocatalysis technology research is photochemical catalyst, for a long time, photochemical catalyst based on the conductor oxidate such as titanium dioxide, zinc oxide relies on its good photocatalysis performance under UV-irradiation to receive the attention of researcher, but its wider band gap reduces its utilization rate to visible ray, limits their commercial application; Although can improve the utilization rate of existing photochemical catalyst to visible ray by the technology such as ion doping, modification compound, increase rate is limited; Therefore, the efficient compound catalyst that development of new is visible light-responded, becomes the focus direction of current photocatalysis research.
Silver orthophosphate is as a kind of novel visible responsive photocatalyst, and under the irradiation of visible ray, have excellent photocatalysis performance can degradable organic pollutant, shows stronger Photocatalytic oxidation activity; By the modification to silver orthophosphate, improving the absorption characteristic that it goes at visible ray, is the effective way improving silver phosphate photocatalyst catalytic activity further; Therefore, the invention provides the preparation method of a kind Graphene molybdenum bisuphide/silver orthophosphate composite, its objective is and strengthen the absorption characteristic of silver orthophosphate at visible region by the load of elemental silver, this composite is improved largely compared to pure silver orthophosphate (wave-length coverage 400-800nm) optical absorption characteristics in visible-range.
Summary of the invention
The object of this invention is to provide a kind of with low cost, efficient class Graphene Molybdenum disulfide/silver phosphate composite visible light photochemical catalyst and preparation method thereof, achieve the Effective Regulation of silver orthophosphate pattern in water-heat process, 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 visible light-responded class Graphene molybdenum bisuphide/silver phosphate composite photocatalyst, is that the class Graphene molybdenum bisuphide of 0.1:100 ~ 3:100 and silver orthophosphate are composited by mass ratio; Preparation method comprises the following steps:
The first step, by water heat transfer class Graphene molybdenum bisuphide; Described preparation method can with reference to C.N.R.Rao, AngshumanNag, InorganicAnaloguesofGraphene,
eur.J.Inorg.Chem.2010,4244 – 4250; Or
H.S.S.RamakrishnaMatte,A.Gomathi,ArunK.Manna,DattatrayJ.Late,RanjanDatta,
SwapanK.Pati,andC.N.R.Rao,MoS
2andWS
2AnaloguesofGraphene,
Angew.Chem.Int.Ed.2010,49,4059–4062。
Second step, is placed in aqueous solution ultrasonic disperse by class Graphene molybdenum bisuphide, obtains the dispersion liquid of class Graphene molybdenum bisuphide;
3rd step, adds silver nitrate solid particle in first step gained dispersion liquid, continues ultrasonicly fully to dissolve to silver nitrate, then leaves standstill;
4th step, under the condition of uniform stirring, dropwise joins the sodium radio-phosphate,P-32 solution prepared in the solution of second step gained at heating water bath, is added dropwise to complete rear continuation shading and stirs a period of time;
5th step, the product obtained by three-step reaction washing is also dry, can obtain described photochemical catalyst.
The present invention compared with prior art, its remarkable advantage: utilize class Graphene molybdenum bisuphide to carry out modification to silver phosphate photocatalyst, and obtain a kind Graphene molybdenum bisuphide/silver orthophosphate composite, the absorption characteristic of silver orthophosphate at visible region can be increased substantially, secondly the preparation method of class Graphene molybdenum bisuphide/silver orthophosphate composite of the present invention is simple, cost is low, and synthesis condition is gentle, is conducive to large-scale promotion.The composite of preparation has stronger optical absorption characteristics at visible region.
Accompanying drawing explanation
The XRD figure of Fig. 1 class Graphene molybdenum bisuphide/silver phosphate composite photocatalyst obtained by embodiment 1;
The DRS spectrogram of Fig. 2 class Graphene molybdenum bisuphide/silver phosphate composite photocatalyst obtained by embodiment 1;
The photocurrent response figure of Fig. 3 class Graphene molybdenum bisuphide/silver phosphate composite photocatalyst obtained by embodiment 1;
Fig. 4 class Graphene molybdenum bisuphide/silver phosphate composite photocatalyst obtained by embodiment 1 is the rhodamine B photocatalytic degradation 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.
Visible light-responded class Graphene molybdenum bisuphide/silver phosphate composite photocatalyst of the present invention is that the molybdenum bisuphide of 0.1:100 ~ 3:100 and silver orthophosphate are composited by mass ratio.
The preparation method of visible light-responded class Graphene molybdenum bisuphide/silver phosphate composite photocatalyst of the present invention, specifically comprises the following steps:
The first step, is placed in aqueous solution ultrasonic disperse to evenly, obtains the dispersion liquid of class Graphene molybdenum bisuphide by class Graphene molybdenum bisuphide;
Second step, adds silver nitrate solid particle in step 1 gained dispersion liquid, continues ultrasonicly fully to dissolve to silver nitrate;
3rd step, at 50 ~ 80 DEG C of heating water baths and stir condition under, the sodium radio-phosphate,P-32 solution prepared dropwise is joined in the solution of second step gained, being added dropwise to complete rear continuation shading stirring makes it mix abundant reaction, and the silver orthophosphate of generation and the mass ratio of class Graphene molybdenum bisuphide are 100:3 ~ 100:0.1;
4th step, the product obtained by three-step reaction washing is also dry, can obtain described photochemical catalyst.
In described step 1, the time of ultrasonic disperse is 20 ~ 50 minutes, and ultrasonic power is 90w.
Ultrasonic power in described step 2 is 90w.
Shading mixing time in described step 3 is 40 ~ 70 minutes.
Below in conjunction with embodiment, the present invention is described in further details.
Embodiment 1: the preparation method of visible light-responded class Graphene molybdenum bisuphide/silver phosphate composite photocatalyst of the present invention, specifically comprises the following steps:
The first step, 0.3mg class Graphene molybdenum bisuphide is placed in 20ml aqueous solution ultrasonic disperse 20 minutes, and ultrasonic power is 90w, obtains the dispersion liquid of class Graphene molybdenum bisuphide;
Second step, adds 340mg silver nitrate solid particle in first step gained dispersion liquid, continues ultrasonicly fully to dissolve to silver nitrate, and ultrasonic power is 90w;
3rd step, under the condition of uniform stirring at 50 DEG C of heating water baths, dropwise joins the sodium radio-phosphate,P-32 solution prepared (containing 253mg sodium phosphate, 20ml deionized water) in the solution of second step gained, is added dropwise to complete rear continuation shading and stirs 70 minutes;
4th step, the product obtained by three-step reaction washing is also dry, can obtain described photochemical catalyst.
Embodiment 2: the preparation method of visible light-responded class Graphene molybdenum bisuphide/silver phosphate composite photocatalyst of the present invention, specifically comprises the following steps:
The first step, 1.5mg class Graphene molybdenum bisuphide is placed in 20ml aqueous solution ultrasonic disperse 30 minutes, and ultrasonic power is 90w, obtains the dispersion liquid of class Graphene molybdenum bisuphide;
Second step, adds 340mg silver nitrate solid particle in first step gained dispersion liquid, continues ultrasonicly fully to dissolve to silver nitrate, and ultrasonic power is 90w;
3rd step, under the condition of uniform stirring at 60 DEG C of heating water baths, dropwise joins the sodium radio-phosphate,P-32 solution prepared (containing 253mg sodium phosphate, 20ml deionized water) in the solution of second step gained, is added dropwise to complete rear continuation shading and stirs 60 minutes;
4th step, the product obtained by three-step reaction washing is also dry, can obtain described photochemical catalyst.
Embodiment 3: the preparation method of visible light-responded class Graphene molybdenum bisuphide/silver phosphate composite photocatalyst of the present invention, specifically comprises the following steps:
The first step, 3mg class Graphene molybdenum bisuphide is placed in 20ml aqueous solution ultrasonic disperse 40 minutes, and ultrasonic power is 90w, obtains the dispersion liquid of class Graphene molybdenum bisuphide;
Second step, adds 340mg silver nitrate solid particle in first step gained dispersion liquid, continues ultrasonicly fully to dissolve to silver nitrate, and ultrasonic power is 90w;
3rd step, at 70 DEG C of heating water baths and under the condition of uniform stirring, the sodium radio-phosphate,P-32 solution prepared (containing 253mg sodium phosphate, 20ml deionized water) is dropwise joined in the solution of second step gained, is added dropwise to complete rear continuation shading and stirs 50 minutes;
4th step, the product obtained by three-step reaction washing is also dry, can obtain described photochemical catalyst.
Embodiment 4: the preparation method of visible light-responded class Graphene molybdenum bisuphide/silver phosphate composite photocatalyst of the present invention, specifically comprises the following steps:
The first step, 9mg class Graphene molybdenum bisuphide is placed in 20ml aqueous solution ultrasonic disperse 50 minutes, and ultrasonic power is 90w, obtains the dispersion liquid of class Graphene molybdenum bisuphide;
Second step, adds 340mg silver nitrate solid particle in first step gained dispersion liquid, continues ultrasonicly fully to dissolve to silver nitrate, and ultrasonic power is 90w;
3rd step, at 80 DEG C of heating water baths and under the condition of uniform stirring, the sodium radio-phosphate,P-32 solution prepared (containing 253mg sodium phosphate, 20ml deionized water) is dropwise joined in the solution of second step gained, is added dropwise to complete rear continuation shading and stirs 40 minutes;
4th step, the product obtained by three-step reaction washing is also dry, can obtain described photochemical catalyst.
The X-ray diffracting spectrum of the class Graphene Molybdenum disulfide/silver phosphate composite visible light catalyst of Fig. 1 prepared by the present invention, diffraction maximums all in figure all matches with silver orthophosphate thing, because class Graphene molybdenum disulfide content is relatively less, and for the silver orthophosphate better relative to crystallization, diffraction maximum is very strong, its XRD diffraction maximum cannot be observed in the drawings, the uv drs collection of illustrative plates of the class Graphene Molybdenum disulfide/silver phosphate composite visible light catalyst of Fig. 2 prepared by the present invention, can draw from figure, composite photo-catalyst after doping class Graphene molybdenum bisuphide, compared to body silver orthophosphate, obviously strengthens in the absorption of visible region (wave-length coverage 400-800nm), equally, the photocurrent response collection of illustrative plates of the class Graphene Molybdenum disulfide/silver phosphate composite visible light catalyst of Fig. 3 prepared by the present invention, compared to body silver orthophosphate, the photocurrent response of this composite photo-catalyst also obviously strengthens, the class Graphene molybdenum bisuphide/silver phosphate composite photocatalyst of Fig. 4 prepared by the present invention is the rhodamine B photocatalytic degradation curve map of 10mg/L to concentration under visible light conditions (wave-length coverage 400-800nm), as can be seen from Figure 4, this composite photo-catalyst reaches 40% to the degradation rate of rhodamine B at radiation of visible light after 4 minutes, after 10 minutes, 90% is reached to the degradation rate of rhodamine B at radiation of visible light, continuing radiation of visible light degradation rate increases few, radiation of visible light after 12 minutes rhodamine B degradation rate be 95%, for body silver orthophosphate, degraded the activity of rhodamine B of 10mg/L at 4 minutes under radiation of visible light, within 10 minutes and 12 minutes, be respectively 15%, 45% and 70%, so, the activity of this composite photocatalyst after being doped with class Graphene molybdenum bisuphide promotes obviously.
Claims (5)
1. a Molybdenum disulfide/silver phosphate composite visible light photocatalytic material, it is characterized in that: described material is that the class Graphene molybdenum bisuphide of 0.1:100 ~ 3:100 and silver orthophosphate are composited by mass ratio, under the visible light conditions of wave-length coverage 400-800nm, be the rhodamine B of 10mg/L to concentration, after 4 minutes, 40% is reached to the degradation rate of rhodamine B at radiation of visible light, after 10 minutes, 90% is reached to the degradation rate of rhodamine B at radiation of visible light, continuing radiation of visible light degradation rate increases few, radiation of visible light after 12 minutes rhodamine B degradation rate be 95%.
2. the preparation method of a kind of Molybdenum disulfide/silver phosphate composite visible light photocatalytic material as claimed in claim 1, is characterized in that comprising the steps:
(1) class Graphene molybdenum bisuphide is placed in aqueous solution ultrasonic disperse to evenly, obtains the dispersion liquid of class Graphene molybdenum bisuphide;
(2) silver nitrate solid particle is added in step (1) gained dispersion liquid, continue ultrasonicly fully to dissolve to silver nitrate;
(3) at 50 ~ 80 DEG C of heating water baths and stir condition under, the sodium radio-phosphate,P-32 solution prepared dropwise is joined in the solution of (2) step gained, being added dropwise to complete rear continuation shading stirring makes it mix abundant reaction, and the silver orthophosphate of generation and the mass ratio of class Graphene molybdenum bisuphide are 100:3 ~ 100:0.1;
(4) (3) step is reacted the product washing obtained also dry, described photochemical catalyst can be obtained.
3. the preparation method of a kind of Molybdenum disulfide/silver phosphate composite visible light photocatalytic material as claimed in claim 2, is characterized in that: in described step (1), the time of ultrasonic disperse is 20 ~ 50 minutes, and ultrasonic power is 90w.
4. the preparation method of a kind of Molybdenum disulfide/silver phosphate composite visible light photocatalytic material as claimed in claim 2, is characterized in that: the ultrasonic power in described step (2) is 90w.
5. the preparation method of a kind of Molybdenum disulfide/silver phosphate composite visible light photocatalytic material as claimed in claim 2, is characterized in that: the shading mixing time in described step (3) is 40 ~ 70 minutes.
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| CN103551173A (en) * | 2013-11-06 | 2014-02-05 | 上海电力学院 | Silver phosphate/molybdenum disulfide compound visible-light-driven photocatalyst and preparation method thereof |
| CN104148093B (en) * | 2014-07-21 | 2017-02-15 | 河南师范大学 | Preparation method for Bi2WO6-MoS2 composite photocatalyst |
| CN104218114B (en) * | 2014-08-28 | 2016-05-18 | 太原理工大学 | A kind of two-dimensional hetero-junction solar cell and preparation method thereof |
| CN105126844A (en) * | 2015-08-06 | 2015-12-09 | 江苏大学 | Molybdenum disulfide/silver vanadate visible light composite catalyst and preparation method thereof |
| CN107029761A (en) * | 2017-03-30 | 2017-08-11 | 常州大学 | A kind of preparation method of support type silver phosphate photocatalyst |
| CN106964382A (en) * | 2017-03-30 | 2017-07-21 | 常州大学 | A kind of preparation method of the silver-colored photochemical catalyst of zinc sulphide compound phosphoric acid |
| CN106994360A (en) * | 2017-04-05 | 2017-08-01 | 江苏大学 | A kind of preparation method of Z configurations visible light catalytic decomposition water composite |
| CN108525686A (en) * | 2018-03-22 | 2018-09-14 | 江苏大学 | A kind of selenizing molybdenum compounded visible light photocatalyst of silver orthophosphate/bis- and preparation method and application |
| CN108855164A (en) * | 2018-06-19 | 2018-11-23 | 广东工业大学 | A kind of carbon cloth load MoS2/Ag3PO4The preparation method of composite photocatalyst material |
| CN114733539B (en) * | 2022-05-20 | 2024-03-01 | 遵义师范学院 | BP QDs and Ag-Ag3PO4 co-modified MoS2 composite material and preparation method and application thereof |
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| CN102698774A (en) * | 2012-06-08 | 2012-10-03 | 浙江大学 | Hydrothermal preparation method for single-layer MoS2 and graphene composite nano material |
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| CN102698774A (en) * | 2012-06-08 | 2012-10-03 | 浙江大学 | Hydrothermal preparation method for single-layer MoS2 and graphene composite nano material |
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Effective date of registration: 20181219 Address after: Room 401, 4th floor, 22 Yaojia Road, Taizhou New Energy Industrial Park, Jiangsu Province Patentee after: Taizhou Haixin Energy Research Institute Co., Ltd. Address before: No. 301, Xuefu Road, Jingkou District, Zhenjiang, Jiangsu Province Patentee before: Jiangsu University |