CN103611550A - Preparation method of molybdenum disulfide-silver metavanadate composite nano photocatalyst - Google Patents
Preparation method of molybdenum disulfide-silver metavanadate composite nano photocatalyst Download PDFInfo
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- CN103611550A CN103611550A CN201310590160.1A CN201310590160A CN103611550A CN 103611550 A CN103611550 A CN 103611550A CN 201310590160 A CN201310590160 A CN 201310590160A CN 103611550 A CN103611550 A CN 103611550A
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Abstract
The invention discloses a preparation method of a molybdenum disulfide-silver metavanadate composite nano photocatalyst, which comprises the following steps: (1) synthesis of MoS2 nano flowers: carrying out hydrothermal synthesis on (NH4)2MO4, KSCN and hydroxylamine hydrochloride to obtain MoS2 nano flowers; (2) synthesis of AgVO3 nanorods: synthesizing the AgVO3 nanorods from AgNO3 and ammonium metavanadate; and (3) synthesis of MoS2-AgVO3 composite nano photocatalyst: carrying out mixing and ball milling on the MoS2 and AgVO3 in a mole ratio of 1:1-1:5. The method has the advantages of accessible raw materials, low price, simple preparation technique, controllable parameters and safe and environment-friendly production process, has important application in the fields of photochemistry, photocatalysis, gas sensitiveness, lithium electricity and the like, and is hopeful to be used for large-scale industrial production.
Description
Technical field
The present invention relates to field of nanometer material technology, particularly, is a kind of MoS
2-AgVO
3the preparation method of composite Nano photochemical catalyst.
Background technology
Transition metal vanadate is the functional material that a class is good, especially as semiconductor light-catalyst, has obtained research widely, is demonstrating its unique effect and wide application prospect aspect new forms of energy and the depollution of environment.Researcher finds that some vanadic acid ag materials also have suitable optical band gap, and good visible absorption and catalytic performance, also has the advantages such as nontoxic, good stability simultaneously, is the visible ray semiconductor catalyst of a class function admirable.Molybdenum bisuphide (MoS
2) there is the layer structure of similar graphite, belong to hexagonal crystal system, be a kind of outstanding two-dimensional nano material.The MoS with nanostructured
2in many performances, have been further upgraded, show highlightedly the following aspects: specific area is very big, adsorption capacity is stronger, and reactivity is high, the catalytic performance especially performance of catalytic hydrogenation desulfurization is stronger, can be used to prepare special catalysis material and air storage material.
Summary of the invention
The object of the present invention is to provide a kind of MoS
2-AgVO
3the preparation method of composite Nano photochemical catalyst, with low cost, technique is simple and productive rate is high.
Above-mentioned purpose is achieved by the following technical solution:
A kind of MoS
2-AgVO
3the preparation method of composite Nano photochemical catalyst, comprises the steps:
(1) MoS
2nano flower is synthetic: with (NH4)
2mO
4, KSCN and hydroxylamine hydrochloride be raw water thermal synthesis MoS
2nano flower, reaction temperature is 150 ℃～500 ℃, the reaction time is 16～48h;
Particularly, be by (NH4)
2mO
4, KSCN and hydroxylamine hydrochloride be according to the mol ratio of the 1:2:1-1:4:4 formation solution that is dissolved in the water, isothermal reaction, product obtains MoS after centrifugal, washing, vacuum drying
2nano flower; Described vacuum drying is at 80 ℃ of dry 10h.
AgVO
3synthesizing of nanometer rods: with AgNO
3(silver metavanadate) and ammonium metavanadate are the synthetic AgVO of raw material
3nanometer rods, hydro-thermal insulation is 90 ℃～240 ℃, temperature retention time is 12～48h;
Particularly, be by AgNO
3be dissolved in the water according to the mol ratio of 1:1-1:4 with ammonium metavanadate, form after solution, then isothermal reaction, obtains AgVO at 80 ℃ of dry 10h
3nanometer rods;
(3) MoS
2-AgVO
3synthesizing of composite Nano photochemical catalyst: by MoS
2nano flower and AgVO
3nanometer rods is placed in ball milling filling by the mol ratio of 1:1-1:5 and vacuumizes and logical argon gas or nitrogen protection, then carries out low speed ball milling with ball mill, and after product washing, vacuum drying obtains MoS
2-AgVO
3composite Nano photochemical catalyst.
Accompanying drawing explanation
Fig. 1 is the MoS that embodiment 1 makes
2(Fig. 1 a), AgVO
3the XRD spectra of (Fig. 1 b), the known synthetic MoS of Fig. 1 a
2all peaks consistent with standard diffraction pattern (PDF No.37-1492), illustrate that synthetic product is pure MoS
2; Fig. 1 b is AgVO
3xRD collection of illustrative plates, its all peaks are consistent with standard diffraction pattern (JCPDS:29-1154), illustrate that synthetic product is pure AgVO
3;
Fig. 2 is MoS
2, AgVO
3and embodiment 1 is that make and MoS
2-AgVO
3the field emission scanning electron microscope of composite Nano photochemical catalyst (SEM) photo, Fig. 2 a is Hydrothermal Synthesis MoS
2sEM figure, its pattern is average diameter 1-2 μ m nano flower; Fig. 2 b is Hydrothermal Synthesis AgVO
3sEM figure, its pattern is the nanometer rods that the about 500nm of diameter, length are about 1um; Fig. 2 c is the MoS that ball milling mixes
2-AgVO
3the SEM of composite nano materials, can clearly see MoS
2nano flower and AgVO
3nanometer rods mixes uniformly.AgVO
3itself be photochemical catalyst, MoS
2there is excellent absorption property, synthetic MoS
2-AgVO
3after composite, MoS
2contribute to strengthen photo-catalysis capability, the absorption property of photochemical catalyst; Can be applicable to the fields such as air-sensitive, electrochemistry and lithium electricity.
The specific embodiment
By the specific embodiment, further describe the present invention below, as known by the technical knowledge, the present invention also can describe by other the scheme that does not depart from the technology of the present invention feature, and therefore changes within the scope of the present invention all or that be equal in the scope of the invention are all included in the invention.
Reagent that the present invention adopts is all purchased from traditional Chinese medicines group.
Embodiment 1:
A kind of MoS
2-AgVO
3the preparation method of composite Nano photochemical catalyst, comprises the steps:
(1) 0.24g (NH4)
2mO
4, 0.32g KSCN and 0.28g NH
2oH HCl is dissolved in the deionized water of 60mL, after dissolving completely, continues to stir 30min, then mixed liquor is transferred in the stainless steel cauldron of 100ml, is placed in vacuum drying chamber in 180 ℃ of insulation reaction 24h, after reaction finishes, is cooled to room temperature; Product, after centrifugation, is used respectively deionized water and absolute ethyl alcohol cyclic washing, last under vacuum condition 80 ℃ of dry 10h obtain the product powder of grey black, i.e. MoS
2nano flower;
(2) 0.17g AgNO
3with 0.12g NH
4vO
3be dissolved in the deionized water of 60mL, after dissolving completely, continue to stir 30min, then mixed liquor is transferred in the stainless steel cauldron of 100ml, be placed in vacuum drying chamber in 160 ℃ of insulation 24h, be cooled to room temperature.Product, after centrifugation, is used respectively deionized water and absolute ethyl alcohol cyclic washing, and finally under vacuum condition, 80 ℃ of dry 10h obtain yellow product powder, i.e. AgVO
3nanometer rods;
(3) MoS
2nano flower and AgVO
3after the mixed in molar ratio of nanometer rods with 1:2, add in stainless steel jar mill, using stainless steel ball as ball-milling medium, ratio of grinding media to material is 10:1, with 200rmp ball milling 2h.Product absolute ethyl alcohol cyclic washing, last under vacuum condition 60 ℃ of dry 12h obtain the product powder of black, i.e. MoS
2-AgVO
3composite Nano photochemical catalyst.
Material and process conditions that embodiment 2 to 4 adopts are shown in Table 1:
Table 1
Raw material ratio involved in table 1 is mol ratio, and Shi℃， reaction time unit of reaction temperature unit is: h.
Embodiment 5
The degradation property of the MoS2-AgVO3 composite Nano photochemical catalyst obtaining, the present invention selects rhodamine B (Rh B) as photocatalytic degradation object.Respectively the sample in embodiment is carried out to Photocatalytic Degradation Property test, the catalyst of preparing with embodiment 1-4 is numbered respectively 1#, 2#, 3#, 4#, and the rhodamine B molecule under visible ray condition in degradation water is evaluated.Light source is the xenon lamp of 500W, and the Rh B solution of 100mL is put into beaker, adds the photochemical catalyst of 0.05g, and the ultrasonic mark 10min of lucifuge stirs 20min, makes Rh B reach adsorption equilibrium in photocatalyst surface.Turn on light to irradiate and carry out photocatalytic degradation reaction, after 3 hours, sample respectively 4mL, with centrifuge centrifugation catalyst granules, get supernatant, by the absorbance of UV-vis spectrophotometer monitoring Rh B, and then the change in concentration of following the tracks of Rh B in solution.According to first order reaction kinetic, ln (C/CO)-kt curve is carried out to linear fit and can calculate to obtain apparent reaction rate constant k((min-1)), by the size of k value, can judge the height of the photocatalytic activity of photochemical catalyst.Result shows (in Table 1), and MoS2-AgVO3 composite Nano photochemical catalyst has shown higher photocatalytic activity under visible ray condition.
The degradation rate of table 2 embodiment 1-4 gained composite catalyst to rhodamine B
Note: the corresponding embodiment 1-4 of sample 1#-4# gained compound.
Claims (3)
1. a preparation method for molybdenum bisuphide-silver metavanadate composite Nano photochemical catalyst, is characterized in that comprising the steps:
(1) MoS
2nano flower is synthetic: with (NH4)
2mO
4, KSCN and hydroxylamine hydrochloride be raw water thermal synthesis MoS
2nano flower, reaction temperature is 150 ℃～500 ℃, the reaction time is 16～48h;
(2) AgVO
3synthesizing of nanometer rods: with AgNO
3with ammonium metavanadate be the synthetic AgVO of raw material
3nanometer rods, hydro-thermal insulation is 90 ℃～240 ℃, temperature retention time is 12～48h;
(3) MoS
2-AgVO
3synthesizing of composite Nano photochemical catalyst: by MoS
2and AgVO
3by the mol ratio of 1:1-1:5, be placed in that ball mill vacuumizes and logical argon gas or nitrogen protection, carry out low speed ball milling, after products therefrom washing, vacuum drying obtains MoS
2-AgVO
3composite Nano photochemical catalyst.
2. the preparation method of a kind of molybdenum bisuphide-silver metavanadate composite Nano photochemical catalyst according to claim 1, is characterized in that in step (1), (NH4)
2mO
4, KSCN and hydroxylamine hydrochloride mol ratio be 1:2:1-1:4:4.
3. the preparation method of a kind of molybdenum bisuphide-silver metavanadate composite Nano photochemical catalyst according to claim 1, is characterized in that AgNO in step (2)
3with the mol ratio of ammonium metavanadate be 1:1-1:4.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105126844A (en) * | 2015-08-06 | 2015-12-09 | 江苏大学 | Molybdenum disulfide/silver vanadate visible light composite catalyst and preparation method thereof |
| CN105536684A (en) * | 2015-12-22 | 2016-05-04 | 镇江市高等专科学校 | Preparation method of molybdenum disulfide-silver sulfide composite nano-grade adsorption-photocatalyst |
| CN106521540A (en) * | 2016-10-25 | 2017-03-22 | 柳玉辉 | Method for preparing graphene-like flower-shaped molybdenum disulfide by co-deposition |
| 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 |
| CN112495420A (en) * | 2020-12-09 | 2021-03-16 | 北华大学 | Preparation method of nitrogen-rich graphite phase carbon nitride/silver metavanadate composite photocatalyst |
| CN115192606A (en) * | 2022-09-01 | 2022-10-18 | 天津师范大学 | Monoatomic nanoenzyme Pt @ MoS 2 And preparation method and application thereof |
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| US20030072941A1 (en) * | 1999-05-28 | 2003-04-17 | Novich Bruce E. | Sizing compositions, methods and apparatus for cleaning sized fiber glass strands, yarns and fabrics |
| CN102580736A (en) * | 2012-02-09 | 2012-07-18 | 江苏大学 | Grapheme / silver vanadium oxide nanometer composite visible light catalyst and preparation method thereof |
| CN102701281A (en) * | 2012-05-14 | 2012-10-03 | 无锡润鹏复合新材料有限公司 | Preparation method of flower-shaped hollow molybdenum disulfide microspheres |
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2013
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| US20030072941A1 (en) * | 1999-05-28 | 2003-04-17 | Novich Bruce E. | Sizing compositions, methods and apparatus for cleaning sized fiber glass strands, yarns and fabrics |
| CN102580736A (en) * | 2012-02-09 | 2012-07-18 | 江苏大学 | Grapheme / silver vanadium oxide nanometer composite visible light catalyst and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105126844A (en) * | 2015-08-06 | 2015-12-09 | 江苏大学 | Molybdenum disulfide/silver vanadate visible light composite catalyst and preparation method thereof |
| CN105536684A (en) * | 2015-12-22 | 2016-05-04 | 镇江市高等专科学校 | Preparation method of molybdenum disulfide-silver sulfide composite nano-grade adsorption-photocatalyst |
| CN106521540A (en) * | 2016-10-25 | 2017-03-22 | 柳玉辉 | Method for preparing graphene-like flower-shaped molybdenum disulfide by co-deposition |
| 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 |
| CN112495420A (en) * | 2020-12-09 | 2021-03-16 | 北华大学 | Preparation method of nitrogen-rich graphite phase carbon nitride/silver metavanadate composite photocatalyst |
| CN115192606A (en) * | 2022-09-01 | 2022-10-18 | 天津师范大学 | Monoatomic nanoenzyme Pt @ MoS 2 And preparation method and application thereof |
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|---|---|
| CN103611550B (en) | 2016-05-04 |
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