CN103611550B - A kind of preparation method of molybdenum bisuphide-silver metavanadate composite Nano photochemical catalyst - Google Patents
A kind of preparation method of molybdenum bisuphide-silver metavanadate composite Nano photochemical catalyst Download PDFInfo
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Abstract
The preparation method who the invention discloses a kind of molybdenum bisuphide-silver metavanadate composite Nano photochemical catalyst, concrete grammar is as follows: (1) MoS2Nano flower is synthetic: with (NH4)2MoO4, KSCN and hydroxylamine hydrochloride be raw water thermal synthesis MoS2Nano flower; (2) AgVO3Synthesizing of nanometer rods: with AgNO3With ammonium metavanadate be the synthetic AgVO of raw material3Nanometer rods; (3) MoS2-AgVO3Synthesizing of composite Nano photochemical catalyst: MoS2And AgVO3Press the mixed in molar ratio ball milling of 1:1-1:5. The inventive method raw material is easy to get, cheap, preparation technology is simple, parameter is easily controlled, production process safety and environmental protection, and have important application in the fields such as the photochemistry of rubbing, photocatalysis, air-sensitive, lithium electricity is expected to for large-scale industrial production.
Description
Technical field
The present invention relates to field of nanometer material technology, particularly, is a kind of MoS2-AgVO3CompoundThe preparation method of nano-photocatalyst.
Background technology
Transition metal vanadate is the functional material that a class is good, especially as partly leadingBody photochemical catalyst has obtained research widely, aspect new forms of energy and the depollution of environment, showsGo out its unique effect and wide application prospect. Researcher finds some vanadic acid silverMaterial also has suitable optical band gap, and good visible absorption and catalyticCan, also there is the advantages such as nontoxic, good stability simultaneously, be a class function admirable canSee optical semiconductor catalyst. Molybdenum bisuphide (MoS2) there is the layer structure of similar graphite,Belonging to hexagonal crystal system, is a kind of outstanding two-dimensional nano material. There is the MoS of nanostructured2In many performances, have been further upgraded, show highlightedly the following aspects:Specific area is very big, and adsorption capacity is stronger, and reactivity is high, and catalytic performance especiallyThe performance of catalytic hydrogenation desulfurization is stronger, can be used to prepare special catalysis material and air storage materialMaterial.
Summary of the invention
The object of the present invention is to provide a kind of MoS2-AgVO3Composite Nano photochemical catalystPreparation method, with low cost, technique is simple and productive rate is high.
Above-mentioned purpose is achieved by the following technical solution:
A kind of MoS2-AgVO3The preparation method of composite Nano photochemical catalyst, comprises following stepRapid:
(1)MoS2Nano flower is synthetic: with (NH4)2MoO4, KSCN and hydroxylamine hydrochloride be formerMaterial Hydrothermal Synthesis MoS2Nano flower, reaction temperature is 150 DEG C～500 DEG C, the reaction time is16～48h；
Particularly, be by (NH4)2MoO4, KSCN and hydroxylamine hydrochloride according toThe mol ratio of the 1:2:1-1:4:4 formation solution that is dissolved in the water, isothermal reaction, product warpAfter centrifugal, washing, vacuum drying, obtain MoS2Nano flower; Described vacuum drying be80 DEG C of dry 10h.
AgVO3Synthesizing of nanometer rods: with AgNO3(silver metavanadate) and ammonium metavanadate are formerThe synthetic AgVO of material3Nanometer rods, hydro-thermal insulation is 90 DEG C～240 DEG C, temperature retention time is 12～48h；
Particularly, be by AgNO3Dissolve according to the mol ratio of 1:1-1:4 with ammonium metavanadateYu Shuizhong, forms after solution, and then isothermal reaction, obtains AgVO at 80 DEG C of dry 10h3Nanometer rods;
(3)MoS2-AgVO3Synthesizing of composite Nano photochemical catalyst: by MoS2Nano flowerAnd AgVO3Nanometer rods is placed in ball milling filling by the mol ratio of 1:1-1:5 and vacuumizes and lead toArgon gas or nitrogen protection, then carry out low speed ball milling with ball mill, after product washing,Vacuum drying obtains MoS2-AgVO3Composite Nano photochemical catalyst.
Brief description of the drawings
Fig. 1 is the MoS that embodiment 1 makes2(Fig. 1 a), AgVO3(Fig. 1 XRD b)Spectrogram, the known synthetic MoS of Fig. 1 a2All peaks and standard diffraction pattern (PDFNo.37-1492) consistent, illustrate that synthetic product is pure MoS2; Fig. 1 b is AgVO3XRD collection of illustrative plates, its all peaks are consistent with standard diffraction pattern (JCPDS:29-1154),Illustrate that synthetic product is pure AgVO3；
Fig. 2 is MoS2、AgVO3And embodiment 1 is that make and MoS2-AgVO3CompoundField emission scanning electron microscope (SEM) photo of nano-photocatalyst, Fig. 2 a is that hydro-thermal is closedBecome MoS2SEM figure, its pattern is average diameter 1-2 μ m nano flower; Fig. 2 b isHydrothermal Synthesis AgVO3SEM figure, its pattern is that the about 500nm of diameter, length are aboutThe nanometer rods of 1um; Fig. 2 c is the MoS that ball milling mixes2-AgVO3Composite nano materialsSEM, can clearly see MoS2Nano flower and AgVO3Nanometer rods is blended in one uniformlyRise. AgVO3Itself be photochemical catalyst, MoS2There is excellent absorption property, syntheticMoS2-AgVO3After composite, MoS2Contribute to strengthen the photocatalysis energy of photochemical catalystPower, absorption property; Can be applicable to the fields such as air-sensitive, electrochemistry and lithium electricity.
Detailed description of the invention
Further describe the present invention by detailed description of the invention below, can by technology general knowledgeKnow, the present invention also can retouch by other the scheme that does not depart from the technology of the present invention featureState, therefore within the scope of the present invention all or be equal to all quilts of change in the scope of the inventionThe present invention comprises.
Reagent that the present invention adopts is all purchased from traditional Chinese medicines group.
Embodiment 1:
A kind of MoS2-AgVO3The preparation method of composite Nano photochemical catalyst, comprises following stepRapid:
(1)0.24g(NH4)2MoO4, 0.32gKSCN and 0.28gNH2OHHCl is moltenIn the deionized water of 60mL, after dissolving completely, continue to stir 30min, then will mixClose in the stainless steel cauldron that liquid is transferred to 100ml, be placed in vacuum drying chamber in180 DEG C of insulation reaction 24h, are cooled to room temperature after reaction finishes; Product is through centrifugalAfter separation, use respectively deionized water and absolute ethyl alcohol cyclic washing, finally at vacuum barThe lower 80 DEG C of dry 10h of part obtain the product powder of grey black, i.e. MoS2Nano flower;
(2)0.17gAgNO3And 0.12gNH4VO3Be dissolved in the deionized water of 60mL,After dissolving completely, continue to stir 30min, then mixed liquor is transferred to 100ml notIn rust steel reactor, be placed in vacuum drying chamber in 160 DEG C of insulation 24h, be cooled to chamberTemperature. Product, after centrifugation, is used respectively deionized water and absolute ethyl alcohol repeatedlyWashing, finally under vacuum condition, 80 DEG C of dry 10h obtain yellow product powder,Be AgVO3Nanometer rods;
(3)MoS2Nano flower and AgVO3After the mixed in molar ratio of nanometer rods with 1:2, addEnter 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, finally at vacuum barThe lower 60 DEG C of dry 12h of part obtain the product powder of black, i.e. MoS2-AgVO3Compound receivingRice 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 reaction temperature unit is DEG C,Reaction time unit is: h.
Embodiment 5
The degradation property of the MoS2-AgVO3 composite Nano photochemical catalyst obtaining, thisBrightly select rhodamine B (RhB) as photocatalytic degradation object. Respectively in embodimentSample carry out Photocatalytic Degradation Property test, the catalyst of preparing with embodiment 1-4Number respectively 1#, 2#, 3#, 4#, the rhodamine under visible ray condition in degradation waterB molecule is evaluated. Light source is the xenon lamp of 500W, and the RhB solution of 100mL is putEnter in beaker, add the photochemical catalyst of 0.05g, the ultrasonic mark 10min of lucifuge, stirs20min, makes RhB reach adsorption equilibrium in photocatalyst surface. Turn on light irradiate intoThe reaction of row photocatalytic degradation, sampled respectively 4mL after 3 hours, used centrifuge centrifugationCatalyst granules, gets supernatant, with the suction of UV-vis spectrophotometer monitoring RhBLuminosity, and then the change in concentration of following the tracks of RhB in solution. According to first-order kineticsRule is carried out linear fit to ln (C/C0)-kt curve can calculate to obtain apparent reaction ratesConstant k ((min-1)), can judge the light of photochemical catalyst and urge by the size of k valueChange active height. Result shows (in table 2), and MoS2-AgVO3 composite Nano light is urgedAgent 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,It is characterized in that comprising the steps:
(1)MoS2Nano flower is synthetic: with (NH4)2MoO4, KSCN and hydroxylamine hydrochloride be formerMaterial Hydrothermal Synthesis MoS2Nano flower, reaction temperature is 150 DEG C～500 DEG C, the reaction time is16～48h；
(2)AgVO3Synthesizing of nanometer rods: with AgNO3With ammonium metavanadate be that raw material is syntheticAgVO3Nanometer rods, hydro-thermal insulation is 90 DEG C～240 DEG C, temperature retention time is 12～48h;
(3)MoS2-AgVO3Synthesizing of composite Nano photochemical catalyst: by MoS2And AgVO3PressThe mol ratio of 1:1-1:5 is 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 MoS2-AgVO3CompoundNano-photocatalyst.
2. a kind of molybdenum bisuphide-silver metavanadate composite Nano according to claim 1The preparation method of photochemical catalyst, is characterized in that in step (1) (NH4)2MoO4、KSCNWith the mol ratio of hydroxylamine hydrochloride be 1:2:1,1:2:2 or 1:4:4.
3. a kind of molybdenum bisuphide-silver metavanadate composite Nano according to claim 1The preparation method of photochemical catalyst, is characterized in that AgNO in step (2)3And ammonium metavanadateMol ratio be 1:1-1:4.
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| 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 |
| CN106521540B (en) * | 2016-10-25 | 2018-10-26 | 东华理工大学 | A method of it is co-deposited and prepares the flower-shaped molybdenum disulfide material of class graphene |
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