CN103506142A - Molybdenum disulfide/silver phosphate composite visible light photocatalytic material and preparation method thereof - Google Patents
Molybdenum disulfide/silver phosphate composite visible light photocatalytic material and preparation method thereof Download PDFInfo
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- CN103506142A CN103506142A CN201310462452.7A CN201310462452A CN103506142A CN 103506142 A CN103506142 A CN 103506142A CN 201310462452 A CN201310462452 A CN 201310462452A CN 103506142 A CN103506142 A CN 103506142A
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Abstract
The invention relates to photocatalytic materials, and particularly relates to a visible-light response graphite-like alkene molybdenum disulfide/silver phosphate composite photocatalyst and a preparation method thereof. Modification treatment is performed on silver phosphate photocatalyst through utilizing graphite-like alkene molybdenum disulfide, so that the graphite-like alkene molybdenum disulfide/silver phosphate composite material is obtained, the composite material can greatly improve the absorption behavior of silver phosphate in visible regions, and the preparation method for the graphite-like alkene molybdenum disulfide/silver phosphate composite material is simple and practicable, the cost is low, the synthesis condition is wild, and large-scale popularization is facilitated; the prepared composite material has strong light absorption behavior in the visible regions.
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; lasting environmental pollution and energy shortage; caused the worry of people to global crisis; in order to realize the sustainable development of human society; develop and a kind ofly can be used for environmental improvement and can be used for again new technology prepared by clean energy resource; become a urgent and urgent task; photocatalysis technology is because it is in wide application prospects in field such as environmental protection, clean energy resource preparations (solar energy is converted into Hydrogen Energy); and paid much attention to, become a kind of technology that has application prospect.
The key of photocatalysis technology research is photochemical catalyst, for a long time, photochemical catalyst based on conductor oxidates such as titanium dioxide, zinc oxide relies on its good photocatalysis performance under UV-irradiation to be subject to researcher's attention, but its wider band gap has reduced its utilization rate to visible ray, has limited their commercial application; Although can improve the utilization rate of existing photochemical catalyst to visible ray by technology such as ion doping, modification are compound, increase rate is limited; Therefore, the efficient compound catalyst that development of new is visible light-responded, becomes the focus direction that current photocatalysis is studied.
Silver orthophosphate is as a kind of novel visible responsive photocatalyst, and under the irradiation of visible ray, having excellent photocatalysis performance can degradable organic pollutant, shows stronger Photocatalytic oxidation activity; By the modification to silver orthophosphate, improve the absorption characteristic that it goes at visible ray, be the effective way that further improves silver orthophosphate photochemical catalyst catalytic activity; Therefore, the invention provides the preparation method of kind Graphene molybdenum bisuphide/silver orthophosphate composite, its objective is that the load by simple substance silver strengthens silver orthophosphate in the absorption characteristic of visible region, this composite than pure silver orthophosphate in visible-range (wave-length coverage 400-800 nm) optical absorption characteristics be improved largely.
Summary of the invention
The object of this invention is to provide a kind of class Graphene molybdenum bisuphide/silver orthophosphate compounded visible light photocatalyst with low cost, efficient and preparation method thereof, realized 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 that realizes the object of the invention is: a kind of visible light-responded class Graphene molybdenum bisuphide/silver phosphate composite photocatalyst, and the class Graphene molybdenum bisuphide and the silver orthophosphate that by mass ratio, are 0.1:100 ~ 3:100 are composited; Preparation method comprises the following steps:
The first step, synthesizes class Graphene molybdenum bisuphide by hydro-thermal method; Described preparation method can be with reference to C. N. R. Rao, Angshuman Nag, and Inorganic Analogues of Graphene,
eur. J. Inorg. Chem.2010,4244 – 4250; Or
H.?S.?S.?Ramakrishna?Matte,?A.?Gomathi,?Arun?K.?Manna,?Dattatray?J.?Late,?Ranjan?Datta,
Swapan?K.?Pati,?and?C.?N.?R.?Rao,?MoS
2?and?WS
2?Analogues?of?Graphene,
?Angew.?Chem.?Int.?Ed.?2010,?49,?4059–4062。
Second step, is placed in the ultrasonic dispersion of the aqueous solution by class Graphene molybdenum bisuphide, obtains the dispersion liquid of class Graphene molybdenum bisuphide;
The 3rd step, adds silver nitrate solid particle in first step gained dispersion liquid, continues ultrasonicly fully to dissolve to silver nitrate, then standing;
The 4th step, under the condition of heating water bath and uniform stirring, dropwise joins the sodium radio-phosphate,P-32 solution having prepared in the solution of second step gained, is added dropwise to complete rear continuation shading and stirs a period of time;
The 5th step, washs the resulting product of three-step reaction be dried, and 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 orthophosphate photochemical catalyst, and obtain kind Graphene molybdenum bisuphide/silver orthophosphate composite, can increase substantially silver orthophosphate in the absorption characteristic of visible region, 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
Fig. 1 is the XRD figure of the obtained class Graphene of embodiment 1 molybdenum bisuphide/silver phosphate composite photocatalyst;
Fig. 2 is the DRS spectrogram of the obtained class Graphene of embodiment 1 molybdenum bisuphide/silver phosphate composite photocatalyst;
Fig. 3 is the photocurrent response figure of the obtained class Graphene of embodiment 1 molybdenum bisuphide/silver phosphate composite photocatalyst;
Fig. 4 is that the obtained class Graphene of embodiment 1 molybdenum bisuphide/silver phosphate composite photocatalyst is the rhodamine B photocatalytic degradation curve map of 10 mg/L to concentration under different visible light irradiation time.
The specific embodiment
Below in conjunction with accompanying drawing, the present invention is done to set forth in further detail.
Visible light-responded class Graphene molybdenum bisuphide/silver phosphate composite photocatalyst of the present invention, the molybdenum bisuphide and the silver orthophosphate that by mass ratio, are 0.1:100 ~ 3:100 are composited.
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 class Graphene molybdenum bisuphide that the aqueous solution is ultrasonic to be dispersed to evenly, obtains the dispersion liquid of 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;
The 3rd step, at 50 ~ 80 ℃ of heating water baths and under the condition of stirring, the sodium radio-phosphate,P-32 solution having prepared is dropwise joined in the solution of second step gained, be added dropwise to complete rear continuation shading stirring and make it mix abundant reaction, the mass ratio of the silver orthophosphate of generation and class Graphene molybdenum bisuphide is 100:3 ~ 100:0.1;
The 4th step, washs the resulting product of three-step reaction be dried, and can obtain described photochemical catalyst.
In described step 1, the time of ultrasonic dispersion is 20 ~ 50 minutes, and ultrasonic power is 90 w.
Ultrasonic power in described step 2 is 90 w.
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, is placed in the ultrasonic dispersion of the 20 ml aqueous solution 20 minutes by 0.3 mg class Graphene molybdenum bisuphide, and ultrasonic power is 90 w, obtains the dispersion liquid of class Graphene molybdenum bisuphide;
Second step, adds 340 mg silver nitrate solid particles in first step gained dispersion liquid, continues ultrasonicly fully to dissolve to silver nitrate, and ultrasonic power is 90 w;
The 3rd step, under the condition of 50 ℃ of heating water baths and uniform stirring, dropwise joins the sodium radio-phosphate,P-32 solution having prepared (containing 253 mg sodium phosphates, 20 ml deionized waters) in the solution of second step gained, is added dropwise to complete rear continuation shading and stirs 70 minutes;
The 4th step, washs the resulting product of three-step reaction be dried, and 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, is placed in the ultrasonic dispersion of the 20 ml aqueous solution 30 minutes by 1.5 mg class Graphene molybdenum bisuphide, and ultrasonic power is 90 w, obtains the dispersion liquid of class Graphene molybdenum bisuphide;
Second step, adds 340 mg silver nitrate solid particles in first step gained dispersion liquid, continues ultrasonicly fully to dissolve to silver nitrate, and ultrasonic power is 90 w;
The 3rd step, under the condition of 60 ℃ of heating water baths and uniform stirring, dropwise joins the sodium radio-phosphate,P-32 solution having prepared (containing 253 mg sodium phosphates, 20 ml deionized waters) in the solution of second step gained, is added dropwise to complete rear continuation shading and stirs 60 minutes;
The 4th step, washs the resulting product of three-step reaction be dried, and 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, is placed in the ultrasonic dispersion of the 20 ml aqueous solution 40 minutes by 3 mg class Graphene molybdenum bisuphide, and ultrasonic power is 90 w, obtains the dispersion liquid of class Graphene molybdenum bisuphide;
Second step, adds 340 mg silver nitrate solid particles in first step gained dispersion liquid, continues ultrasonicly fully to dissolve to silver nitrate, and ultrasonic power is 90 w;
The 3rd step, under the condition of 70 ℃ of heating water baths and uniform stirring, dropwise joins the sodium radio-phosphate,P-32 solution having prepared (containing 253 mg sodium phosphates, 20 ml deionized waters) in the solution of second step gained, is added dropwise to complete rear continuation shading and stirs 50 minutes;
The 4th step, washs the resulting product of three-step reaction be dried, and 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, is placed in the ultrasonic dispersion of the 20 ml aqueous solution 50 minutes by 9 mg class Graphene molybdenum bisuphide, and ultrasonic power is 90 w, obtains the dispersion liquid of class Graphene molybdenum bisuphide;
Second step, adds 340 mg silver nitrate solid particles in first step gained dispersion liquid, continues ultrasonicly fully to dissolve to silver nitrate, and ultrasonic power is 90 w;
The 3rd step, under the condition of 80 ℃ of heating water baths and uniform stirring, dropwise joins the sodium radio-phosphate,P-32 solution having prepared (containing 253 mg sodium phosphates, 20 ml deionized waters) in the solution of second step gained, is added dropwise to complete rear continuation shading and stirs 40 minutes;
The 4th step, washs the resulting product of three-step reaction be dried, and can obtain described photochemical catalyst.
Fig. 1 is the X-ray diffracting spectrum of the prepared class Graphene molybdenum bisuphide/silver phosphate composite visible light catalyst of the present invention, diffraction maximums all in figure are all coincide with silver orthophosphate phase, because class Graphene molybdenum bisuphide content is relatively less, and for the silver orthophosphate better with respect to crystallization, diffraction maximum is very strong, its XRD diffraction maximum cannot be observed in the drawings, Fig. 2 is the uv drs collection of illustrative plates of the prepared class Graphene molybdenum bisuphide/silver phosphate composite visible light catalyst of the present invention, from figure, can draw, composite photo-catalyst after doping class Graphene molybdenum bisuphide is than body silver orthophosphate, in the absorption of visible region (wave-length coverage 400-800 nm), obviously strengthens, equally, Fig. 3 is the photocurrent response collection of illustrative plates of the prepared class Graphene molybdenum bisuphide/silver phosphate composite visible light catalyst of the present invention, and than body silver orthophosphate, the photocurrent response of this composite photo-catalyst also obviously strengthens, Fig. 4 is that the prepared class Graphene molybdenum bisuphide/silver phosphate composite photocatalyst of the present invention is the rhodamine B photocatalytic degradation curve map of 10 mg/L to concentration under visible ray condition (wave-length coverage 400-800 nm), as can be seen from Figure 4, this composite photo-catalyst radiation of visible light after 4 minutes the degradation rate to rhodamine B reach 40%, radiation of visible light after 10 minutes the degradation rate to rhodamine B reach 90%, 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, under radiation of visible light, degraded the activity of rhodamine B of 10 mg/L at 4 minutes, within 10 minutes and 12 minutes, be respectively 15%, 45% and 70%, so, the activity of this composite photocatalyst after the class Graphene molybdenum bisuphide that adulterated promotes obviously.
Claims (5)
1. molybdenum bisuphide/silver orthophosphate composite visible light catalysis material, it is characterized in that: class Graphene molybdenum bisuphide and silver orthophosphate that described material is 0.1:100 ~ 3:100 by mass ratio are composited, under the visible ray condition of wave-length coverage 400-800 nm, it to concentration, is the rhodamine of 10 mg/L, radiation of visible light after 4 minutes the degradation rate to rhodamine B reach 40%, radiation of visible light after 10 minutes the degradation rate to rhodamine B reach 90%, continue radiation of visible light degradation rate increase few, radiation of visible light after 12 minutes rhodamine B degradation rate be 95%.
2. the preparation method of a kind of molybdenum bisuphide/silver orthophosphate composite visible light catalysis material as claimed in claim 1, is characterized in that comprising the steps:
(1) class Graphene molybdenum bisuphide is placed in to the aqueous solution is ultrasonic to be dispersed 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 ℃ of heating water baths and under the condition of stirring, the sodium radio-phosphate,P-32 solution having prepared is dropwise joined in the solution of second step gained, be added dropwise to complete rear continuation shading stirring and make it mix abundant reaction, the mass ratio of the silver orthophosphate of generation and class Graphene molybdenum bisuphide is 100:3 ~ 100:0.1;
(4) the resulting product of three-step reaction is washed and is dried, can obtain described photochemical catalyst.
3. the preparation method of a kind of molybdenum bisuphide/silver orthophosphate composite visible light catalysis material as claimed in claim 2, is characterized in that: in described step 1, the time of ultrasonic dispersion is 20 ~ 50 minutes, and ultrasonic power is 90 w.
4. the preparation method of a kind of molybdenum bisuphide/silver orthophosphate composite visible light catalysis material as claimed in claim 2, is characterized in that: the ultrasonic power in described step 2 is 90 w.
5. the preparation method of a kind of molybdenum bisuphide/silver orthophosphate composite visible light catalysis 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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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN104148093A (en) * | 2014-07-21 | 2014-11-19 | 河南师范大学 | Preparation method for Bi2WO6-MoS2 composite photocatalyst |
| CN104218114A (en) * | 2014-08-28 | 2014-12-17 | 太原理工大学 | Two-dimensional heterojunction solar cell and manufacturing 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 |
| 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 |
| CN107029761A (en) * | 2017-03-30 | 2017-08-11 | 常州大学 | A kind of preparation method of support type silver phosphate photocatalyst |
| 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 |
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| CN102631939A (en) * | 2012-03-28 | 2012-08-15 | 江苏大学 | Graphene/silver phosphate composite visible light photocatalyst and preparation method thereof |
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| CN102631939A (en) * | 2012-03-28 | 2012-08-15 | 江苏大学 | Graphene/silver phosphate composite visible light photocatalyst and preparation method thereof |
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Cited By (12)
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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 |
| CN104148093A (en) * | 2014-07-21 | 2014-11-19 | 河南师范大学 | Preparation method for Bi2WO6-MoS2 composite photocatalyst |
| CN104148093B (en) * | 2014-07-21 | 2017-02-15 | 河南师范大学 | Preparation method for Bi2WO6-MoS2 composite photocatalyst |
| CN104218114A (en) * | 2014-08-28 | 2014-12-17 | 太原理工大学 | Two-dimensional heterojunction solar cell and manufacturing 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 |
| 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 |
| CN107029761A (en) * | 2017-03-30 | 2017-08-11 | 常州大学 | A kind of preparation method of support type silver phosphate photocatalyst |
| 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 |
| CN114733539A (en) * | 2022-05-20 | 2022-07-12 | 遵义师范学院 | BP QDs and Ag-Ag3PO4 co-modified MoS2 composite material, and preparation method and application thereof |
| 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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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 |