CN106975511A - A kind of MoS2/C60/g‑C3N4Composite photo-catalyst and preparation method thereof - Google Patents

A kind of MoS2/C60/g‑C3N4Composite photo-catalyst and preparation method thereof Download PDF

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CN106975511A
CN106975511A CN201710269942.3A CN201710269942A CN106975511A CN 106975511 A CN106975511 A CN 106975511A CN 201710269942 A CN201710269942 A CN 201710269942A CN 106975511 A CN106975511 A CN 106975511A
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常立民
徐达
林雪
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Jilin Normal University
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/24Nitrogen compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
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    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/34Organic compounds containing oxygen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/36Organic compounds containing halogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/38Organic compounds containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts

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Abstract

The invention discloses a kind of MoS2/C60/g‑C3N4Composite photocatalyst material and preparation method thereof, belongs to nano-photocatalyst material technical field;The MoS that the present invention is prepared with hydro-thermal method2With C60With g C3N4It is combined with coprecipitation, forms the nano-complex with sheet-like morphology, middle MoS in the compound2Shared mass ratio is 3%~9%, C60With g C3N4Mass ratio is 1:1, by test, it compares MoS under visible light illumination2、C60With g C3N4Catalytic efficiency be significantly improved, 6%MoS2/C60/g‑C3N4Through radiation of visible light 70min rhodamine B degradation rates up to 100%.Preparation method process employed in the present invention is simple and easy to control, easy to operate, cost is low, product visible light catalysis activity is high.

Description

A kind of MoS2/C60/g-C3N4Composite photo-catalyst and preparation method thereof
Technical field
The invention belongs to nano-photocatalyst material technical field.
Background technology
Graphite phase carbon nitride (g-C3N4) as a kind of carbon-based material, it is wide with preparing raw material source, it is cheap, prepare Method is simple and the features such as being easy to industrialization.As visible light catalyst its have adjustable electronic structure and good physics and Chemical stability.Because its energy gap is 2.70eV, visible photocatalysis water system can be absorbed by excited by visible light Hydrogen;However, g-C3N4Also the raising that have impact on its photocatalysis performance is had disadvantages that, particularly higher electron-hole recombination rate, Its photocatalysis efficiency is seriously reduced, for improving g-C3N4Photocatalysis performance, it is always the neck to improve its electron hole separation rate The emphasis of domain research.
MoS2Laminated structure has wide application in terms of electrochemistry, is used as well-known production hydrogen catalyst, molybdenum disulfide It is considered as preferable catalyst, is widely used in the fields such as photocatalysis, sensing.
Though two kinds of materials can serve as catalysis material using how further to improve its photocatalysis efficiency and be Important topic urgently to be resolved hurrily at present.
The content of the invention
In view of the above-mentioned problems, the present invention proposes a kind of MoS2/C60/g-C3N4Composite photo-catalyst, make use of closed shell structure C60The unique Electronic Performance being had.Known C60Closed shell structure by 30 bonding molecular orbitals and 60 pi-electrons, this Plant structure and be beneficial to effective electro transfer.C60Unique texture allow it as an outstanding electron acceptor, effectively draw Quick Photoinduced Charge separation and relatively slow charge recombination are played, then can improve g-C3N4Electron hole separation rate, this is combined Due to MoS in structure2Implantation make g-C3N4Interlamellar spacing becomes big, effectively the ratio surface of increase catalyst.And due to MoS2、C60 And g-C3N4Between form hetero-junctions, improve the separative efficiency of optical charge, be effectively improved photocatalysis efficiency.
MoS2/C60/g-C3N4Composite photo-catalyst, middle MoS2Shared mass ratio is 3%~9%, C60With g-C3N4Mass ratio For 1:1;The composite catalyst is sheet-like morphology, the g-C for being 50~70nm as 1 μm, thickness using size in composite construction3N4For base Bottom, successively in its surface recombination C60It is 200~500nm with size, thickness is 50~80nm sheet MoS2Obtain.
The preparation method of the composite photo-catalyst is specific as follows:
1) hydro-thermal method prepares MoS2
2) g-C is prepared3N4
3)C60/g-C3N4The preparation of compound:According to mass ratio 1:1 weighs g-C3N4With C60, by the two according to 5mg/mL's Ratio is scattered in absolute ethyl alcohol, is continued 12h after being uniformly dispersed under additional stirring condition, is subsequently placed in 80~100 DEG C of conditions Lower drying, obtains C60/g-C3N4Compound;
4)MoS2/C60/g-C3N4The preparation of compound:0.9~2.7:30 ratios weigh the MoS of hydro-thermal method preparation2And C60/ g-C3N4Compound, the two is scattered in absolute ethyl alcohol according to 1.5~5mg/mL ratio, in additional stirring after being uniformly dispersed Under the conditions of continue 3h, under the conditions of being subsequently placed in 80~100 DEG C dry, obtain MoS2/C60/g-C3N4Compound;
Step 1) in hydro-thermal method prepare MoS2Comprise the following steps that:
It is 0.37~0.38 according to mass ratio:1 ratio weighs sodium molybdate and thiocarbamide is dissolved in deionized water, is completely dissolved More than ultrasonic disperse 30min again afterwards, it is 0.19~0.20mol/L to obtain molybdic acid na concn in mixed solution, mixed solution;Will be mixed Close solution to be transferred in reactor, packing density is 65%, room temperature is naturally cooled to after reaction 24h under the conditions of 240 DEG C;Spend from After sub- water and ethanol are washed respectively, dried under the conditions of 60 DEG C, obtain sheet MoS2
Step 2) prepare g-C3N4Comprise the following steps that:By melamine using 2.0~2.3 DEG C/min heating rate as 550 DEG C are heated to from room temperature, and 4h is incubated in 550 DEG C, is then cooled to identical speed after room temperature and obtains pale yellow powder The g-C of shape3N4
Beneficial effects of the present invention:
Preparation process of the invention is simple and easy to control, easy to operate, cost is low, product visible light catalysis activity is high, wherein, 6%MoS2/C60/g-C3N4Through radiation of visible light 70min rhodamine B degradation rates up to 100%.In the preparation of composite nano materials There is vast potential for future development with application field.
Brief description of the drawings
Fig. 1 C60With prepared MoS2、g-C3N4、MoS2/C60、MoS2/g-C3N4、C60/g-C3N4And MoS2/C60/g- C3N4X-ray diffraction (XRD) spectrogram of composite photo-catalyst;
C prepared by Fig. 260、MoS2、g-C3N4、MoS2/C60、MoS2/g-C3N4、C60/g-C3N4And MoS2/C60/g- C3N4Fourier infrared spectrum (FT-IR) figure of composite photo-catalyst;
MoS prepared by Fig. 32/C60/g-C3N4X-ray photoelectron power spectrum (XPS) figure of composite photo-catalyst;
Composite catalyst MoS prepared by Fig. 42/C60/g-C3N4Transmission electron microscope (TEM) photo;
Composite catalyst MoS prepared by Fig. 52/C60/g-C3N4High-resolution-ration transmission electric-lens (HRTEM) photo;
C prepared by Fig. 660、g-C3N4、MoS2/C60、MoS2/g-C3N4、C60/g-C3N4And MoS2/C60/g-C3N4It is multiple The photocatalytic activity curve map of closing light catalyst rhodamine B degradation under visible light conditions.
Embodiment
Technical solution of the present invention is further explained and illustrated in the way of specific embodiment below.
Embodiment 1
1.MoS2Preparation:Using hydrothermal synthesis method, 0.15g sodium molybdates and 0.4g thiocarbamides are codissolved in 32.5mL deionizations In water, 30min is stirred on magnetic stirring apparatus.Ultrasonic disperse 30min again after stirring terminates.Solution after ultrasound is loaded into liner In polytetrafluoroethylene (PTFE) stainless steel cauldron, packing density is 65%, is heated to 240 DEG C and keeps naturally cooling to room temperature after 24h.With Deionized water and ethanol are washed after 3 times respectively, and product is dried under the conditions of 60 DEG C.
2.g-C3N4Preparation:Melamine is used for raw material, takes 24mmol melamines in crucible, crucible is put into In Muffle furnace, 550 DEG C are heated to by 2.0-2.3 DEG C/min of heating rate, 4h is incubated in 550 DEG C, then with identical speed It is down to after initial temperature and takes out crucible, obtains the g-C of pale yellow powder shape3N4
3.C60/g-C3N4Preparation:By 50mg C60With 50mg g-C3N4Ultrasonic 30min is scattered in 20mL absolute ethyl alcohols, Stirred on magnetic stirring apparatus after 12h, in 80 DEG C of drying in drying box, produce C60/g-C3N4
4.MoS2/C60/g-C3N4Preparation:By 0.9mg MoS2With 30mg C60/g-C3N4Ultrasonic 1h be scattered in 20mL without In water-ethanol, stirred on magnetic stirring apparatus after 3h, in 80 DEG C of drying in drying box, produce MoS2/C60/g-C3N4
Structure and morphology characterization
As shown in figure 1, being C60With prepared MoS2、g-C3N4、MoS2/C60、MoS2/g-C3N4、C60/g-C3N4And MoS2/C60/g-C3N4The XRD of composite photo-catalyst, as can be seen from Figure 1 MoS2/C60/g-C3N4The XRD spectrum of composite photo-catalyst In contain molybdenum sulfide, g-C3N4And C60Characteristic peak, and do not occur other miscellaneous peaks, it was demonstrated that only include three of the above thing in compound Matter.
As shown in Fig. 2 all C60Characteristic peak (1427cm-1、1180cm-1、575cm-1、528cm-1) and g-C3N4's Characteristic peak (3168cm-1、1635cm-1、1574cm-1、1420cm-1、1328cm-1、1253cm-1、812cm-1) can be from MoS2/ C60/g-C3N4It is observed that in collection of illustrative plates.
As shown in figure 3, C 1s two peaks are respectively in 283.9eV (C-C) and 287.6eV (N-C=N).287.6eV with C is understood 288.0eV being close60To g-C3N4N-C=N have little to no effect.N 1s peak appears in 398.2eV (C=N- C).Mo 3d peak understands that the existence form of molybdenum is Mo in 228.2eV and 231.4eV respectively4+, S 2p peak appears in 161.5eV Knowable existence form is S2 2-
Fig. 4 is prepared MoS2/C60/g-C3N4The TEM photos of sample, its pattern is sheet.It can be measured in Fig. 5 Crystal striped distance respectively 0.366nm and 0.63nm, corresponds to g-C respectively3N4And MoS (002)2(002) interplanar distance, by This can be seen that g-C3N4And MoS2Success is compound together, according to Fig. 4 it can be seen that transparent C60Answered with the compound of sheet It is combined.
Photocatalytic activity checking test:
The photocatalysis performance of prepared sample is evaluated using Rh B as model compound.In an experiment, exist 100mL 0.01mmolL-1Rh B solutions in add and 0.01g catalyst and be put into glass reactor.Using 500W xenon lamps (λ > 420nm) irradiation.420nn wave filters are inserted between lamp and sample to remove ultraviolet light (λ < 420nm).In visible illumination Before by suspension strong agitation 30 minutes in the dark.Then solution is exposed to radiation of visible light under magnetic stirring. Given time interval, periodic collection and analysis 4mL suspension.Rh B concentration is carried out by UV-2550 ultraviolet spectrometers Analysis, absorption spectrum intensity is recorded when the maximum wave band of ultraviolet-visible is 552nm.
As a result as shown in fig. 6, prepared MoS2/C60/g-C3N4Catalyst is compared with pure phase C60、g-C3N4、C60/g-C3N4、 MoS2/C60And MoS2/g-C3N4Photocatalysis efficiency is improved largely, wherein 6%MoS2/C60/g-C3N4Rh B photocatalysis efficiencies Highest, through radiation of visible light 70min Rh B degradation rates up to 100%.

Claims (4)

1. a kind of MoS2/C60/g-C3N4Composite photo-catalyst, it is characterised in that MoS in the composite photo-catalyst2Shared mass ratio For 3%~9%, C60With g-C3N4Mass ratio is 1:1;The composite catalyst be sheet-like morphology, composite construction using size as 1 μm, Thickness is 50~70nm g-C3N4For substrate, successively in its surface recombination C60With size be 200~500nm, thickness be 50~ 80nm sheet MoS2Obtain.
2. MoS as claimed in claim 12/C60/g-C3N4The preparation method of composite photo-catalyst, is comprised the following steps that:
1) hydro-thermal method prepares MoS2
2) g-C is prepared3N4
3)C60/g-C3N4The preparation of compound:According to mass ratio 1:1 weighs g-C3N4With C60, by the two ratio according to 5mg/mL It is scattered in absolute ethyl alcohol, continues 12h after being uniformly dispersed under additional stirring condition, is done under the conditions of being subsequently placed in 80~100 DEG C It is dry, obtain C60/g-C3N4Compound;
4)MoS2/C60/g-C3N4The preparation of compound:0.9~2.7:30 ratios weigh the MoS of hydro-thermal method preparation2And C60/g-C3N4 Compound, the two is scattered in absolute ethyl alcohol according to 1.5~5mg/mL ratio, after being uniformly dispersed under additional stirring condition Continue 3h, dried under the conditions of being subsequently placed in 80~100 DEG C, obtain MoS2/C60/g-C3N4Compound.
3. MoS according to claim 22/C60/g-C3N4The preparation method of composite photo-catalyst, it is characterised in that step 1) hydro-thermal method prepares MoS in2Comprise the following steps that:
It is 0.37~0.38 according to mass ratio:1 ratio weighs sodium molybdate and thiocarbamide is dissolved in deionized water, after being completely dissolved again More than ultrasonic disperse 30min, it is 0.19~0.20mol/L to obtain molybdic acid na concn in mixed solution, mixed solution;
Mixed solution is transferred in reactor, packing density is 65%, room is naturally cooled to after reaction 24h under the conditions of 240 DEG C Temperature;After being washed respectively with deionized water and ethanol, dried under the conditions of 60 DEG C, obtain sheet MoS2
4. MoS according to claim 22/C60/g-C3N4The preparation method of composite photo-catalyst, it is characterised in that step 2) g-C is prepared3N4Comprise the following steps that:
Melamine is heated to 550 DEG C using 2.0~2.3 DEG C/min heating rate as from room temperature, and 4h is incubated in 550 DEG C, Then the g-C that pale yellow powder shape is obtained after room temperature is cooled to identical speed3N4
CN201710269942.3A 2017-04-24 2017-04-24 A kind of MoS2/C60/g‑C3N4Composite photo-catalyst and preparation method thereof Pending CN106975511A (en)

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Cited By (5)

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CN108671955A (en) * 2018-05-24 2018-10-19 西京学院 A kind of photodissociation aquatic products complex hydroformylation catalyst and preparation method thereof
CN108940332A (en) * 2018-06-04 2018-12-07 东北大学 A kind of high activity MoS2/g-C3N4/Bi24O31Cl10The preparation method of composite photo-catalyst
CN109225296A (en) * 2018-08-31 2019-01-18 中国环境科学研究院 A kind of visible light-responded photochemical catalyst and preparation method thereof
KR20200025997A (en) * 2018-08-30 2020-03-10 한양대학교 에리카산학협력단 Composite fiber, manufacturing method thereof, and gas purification system comprising the same
CN112156186A (en) * 2020-10-29 2021-01-01 南京医科大学 Infrared dye-sensitized carbon nitride ternary heterojunction nano material and preparation method and application thereof

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108671955A (en) * 2018-05-24 2018-10-19 西京学院 A kind of photodissociation aquatic products complex hydroformylation catalyst and preparation method thereof
CN108671955B (en) * 2018-05-24 2021-11-26 西京学院 Composite catalyst for photolysis of aquatic hydrogen and preparation method thereof
CN108940332A (en) * 2018-06-04 2018-12-07 东北大学 A kind of high activity MoS2/g-C3N4/Bi24O31Cl10The preparation method of composite photo-catalyst
CN108940332B (en) * 2018-06-04 2020-12-15 东北大学 High-activity MoS2/g-C3N4/Bi24O31Cl10Preparation method of composite photocatalyst
KR20200025997A (en) * 2018-08-30 2020-03-10 한양대학교 에리카산학협력단 Composite fiber, manufacturing method thereof, and gas purification system comprising the same
KR102236652B1 (en) 2018-08-30 2021-04-06 한양대학교 에리카산학협력단 Composite fiber, manufacturing method thereof, and gas purification system comprising the same
CN109225296A (en) * 2018-08-31 2019-01-18 中国环境科学研究院 A kind of visible light-responded photochemical catalyst and preparation method thereof
CN112156186A (en) * 2020-10-29 2021-01-01 南京医科大学 Infrared dye-sensitized carbon nitride ternary heterojunction nano material and preparation method and application thereof
CN112156186B (en) * 2020-10-29 2022-07-05 南京医科大学 Infrared dye-sensitized carbon nitride ternary heterojunction nano material and preparation method and application thereof

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