CN111215097A - MoS2/Sb2S3Preparation method of composite photocatalyst - Google Patents

MoS2/Sb2S3Preparation method of composite photocatalyst Download PDF

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CN111215097A
CN111215097A CN201811410612.2A CN201811410612A CN111215097A CN 111215097 A CN111215097 A CN 111215097A CN 201811410612 A CN201811410612 A CN 201811410612A CN 111215097 A CN111215097 A CN 111215097A
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parts
mos
reaction kettle
precursor
composite photocatalyst
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不公告发明人
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Qidong Mau Wood Industry Co Ltd
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Qidong Mau Wood Industry Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • 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
    • B01J27/02Sulfur, selenium or tellurium; Compounds thereof
    • B01J27/04Sulfides
    • B01J27/047Sulfides with chromium, molybdenum, tungsten or polonium
    • B01J27/051Molybdenum
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0218Compounds of Cr, Mo, W
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0274Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
    • B01J20/0285Sulfides of compounds other than those provided for in B01J20/045
    • 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
    • CCHEMISTRY; METALLURGY
    • 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4806Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00Aspects relating to sorbent materials
    • B01J2220/40Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • 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
    • C02F2101/308Dyes; Colorants; Fluorescent agents

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  • Organic Chemistry (AREA)
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  • Engineering & Computer Science (AREA)
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Abstract

The invention discloses a MoS2/Sb2S3The preparation method of the composite photocatalyst comprises the following steps: reacting SbCl3And CH3CSNH2Dissolving in anhydrous ethanol, stirring under nitrogen atmosphere for 25-35min, and centrifuging to obtain bright orange precursor; dissolving the prepared precursor in deionized water, and magnetically stirring to obtain Sb2S3Precursor solution, adding H32Mo7N6O28And CH4N2S, stirring to obtain a mixed solution; transferring the mixed solution into a reaction kettle, placing into a muffle furnace, sealing, heating to 165-175 deg.C for 25-27h, and coolingAnd after the temperature is reduced to room temperature, centrifugally separating, washing, drying and cooling to obtain the catalyst. The method is simple, convenient, rapid and easy to operate, and the prepared MoS2/Sb2S3The composite photocatalyst has higher efficiency on photocatalytic degradation of rhodamine B, shows excellent adsorption performance and photocatalytic performance, and has certain application value.

Description

MoS2/Sb2S3Preparation method of composite photocatalyst
Technical Field
The invention relates to a MoS2/Sb2S3A preparation method of a composite photocatalyst.
Background
In recent years, the nano semiconductor photocatalysis technology has attracted wide attention due to the great advantages of the nano semiconductor photocatalysis technology in the aspects of alternative energy and environmental remediation, and is also applied to industrial production. A wide variety of semiconductor photocatalytic materials such as TiO2CdS, ZnO and different morphological structures such as flower-like (SnWO)4) Rod-like (ZnO), sheet-like (BiVO)4) The binary metal oxide of (A) has a certain application in the field of photocatalysis. However, TiO2The photocatalyst such as ZnO has a wider band gap structure, has stronger response to ultraviolet light only and lower utilization rate to natural light, so that the special properties of other materials and TiO are utilized2The photocatalyst is compounded, so that the improvement of the photocatalytic performance becomes a new research hotspot.
At present, metal sulfides such as Sb2S3、Bi2S3Due to the narrow band gap structure, it has attracted a wide attention to have a strong response in the visible region. Among numerous binary metal sulfides, the direct band gap semiconductor material Sb belonging to the orthorhombic system2S3Due to strong spectral response, higher thermal band energy and excellent photoelectric property, the photocatalyst is widely applied to the fields of solar energy conversion, photocatalysis, thermoelectric cooling and the like, and simultaneously is used as a photocatalyst together with TiO2Compared with ZnO, the photocatalyst has higher photocatalytic degradation efficiency in a visible light region. Sb2S3The main disadvantages of (1) are that photogenerated electron-hole pairs are easy to recombine and the electron migration rate is slow. Increase of Sb2S3The improvement of the separation efficiency by utilizing the oxidation mechanism of electron hole pairs in water is considered as the key for effectively degrading organic pollutants, so that the design of the composite material for effectively reducing the recombination rate of photo-generated electron holes becomes a research hotspot. To promote Sb2S3Efficient separation of photogenerated carriers, some semiconductor materials (TiO)2ZnO) or conductor materials (rGO, carbon nanotube CNT) and Sb2S3Composite, as an electron transfer acceptor, greatly improves Sb2S3The photon-generated carrier migration rate and the separation efficiency.
The latest research found that MoS2As a two-dimensional (2D) layered material similar to graphene, attention is paid to its layered structure, in which each layer is formed of two hexagonal close-packed S atoms and one Mo atom in between to form a sandwich structure, adjacent layers are bonded together by weak van der waals force, MoS2The layered structure shows huge specific surface area and more active sites, so that the layered structure has certain adsorption performance and also provides rapid migration of electronsIt is possible. As a member of a transition metal disulfide (MX)2M represents transition metal, X represents chalcogenide metal such as S, Se, Te and Po), the band gap of the chalcogenide metal is 1.23-1.69 eV, the solar light utilization rate is high, and the band gap is related to factors such as layer thickness, nanometer size and doping. MoS2The crystal phase of (A) is mainly hexagonal phase 2H-MoS2Orthorhombic 3R-MoS phase2Tetragonal phase 1T-MoS2。MoS2The properties of the catalyst can be widely applied to a plurality of aspects such as sensors, super capacitors, solar panels, catalytic hydrogen production and the like, and can be used as a cocatalyst for degrading organic wastewater. Mixing MoS2And Sb2S3The composite photocatalyst is prepared by compounding, and not only can exert Sb2S3Can exert strong absorption effect on visible light and strong photocatalytic activity thereof, and can also exert MoS2The function of (1): (1) as an excellent electron transporter, the photocatalyst can efficiently prevent the self-phase recombination of electron hole pairs in the photocatalysis process so as to improve the catalytic performance of the photocatalyst; (2) mixing MoS2The photocatalyst is compounded with the photocatalyst, so that the light absorption intensity of the photocatalyst can be improved, and the absorption wavelength range of sunlight is expanded, so that the solar energy utilization rate is improved; (3) MoS with huge specific surface area2The photocatalyst carrier can increase the specific surface area of a semiconductor, so that the adsorption sites and the catalytic sites of the composite material are increased, and finally, the catalytic performance of the photocatalyst is enhanced. Simultaneously, MoS2And Sb2S3Compounding also helps to reduce MoS2The self-phase stacking phenomenon is more beneficial to the dispersion of the photocatalyst. Thus, Sb2S3And MoS2The composite photocatalyst has wide research prospect.
Disclosure of Invention
The invention aims to provide a MoS2/Sb2S3A preparation method of a composite photocatalyst.
The invention is realized by the following technical scheme:
MoS2/Sb2S3Preparation method of composite photocatalyst and packageThe method comprises the following steps: 5-7 parts of SbCl3And 8-10 parts of CH3CSNH2Dissolving in 55-65 parts of absolute ethyl alcohol, magnetically stirring for 25-35min under the atmosphere of nitrogen, and performing centrifugal separation to obtain a bright orange precursor; the prepared SbCl3Dissolving the bright orange precursor in 50-60 parts of deionized water, and magnetically stirring to obtain Sb2S3Adding 2-4 parts of H into the precursor solution32Mo7N6O28And 5-7 parts of CH4N2S, magnetically stirring to obtain a mixed solution; finally transferring the mixed solution into a reaction kettle, putting the reaction kettle into a muffle furnace, sealing and heating the reaction kettle to 165-175 ℃, keeping the temperature for 25-27h, cooling the reaction kettle to room temperature, and then, adding MoS2/Sb2S3Centrifugally separating the composite photocatalyst, washing with anhydrous ethanol and deionized water for 4-6 times, drying in a vacuum drying oven at 45-55 deg.C for 13-15h, and cooling; the raw materials are in parts by weight.
Preferably, in the preparation method, the magnetic stirring is carried out for 30min under the nitrogen atmosphere.
Preferably, in the preparation method, the mixture is placed into a muffle furnace to be hermetically heated to 170 ℃.
Preferably, the preparation method lasts for 26 h.
Preferably, in the preparation method, the mixture is dried for 14 hours in a vacuum drying oven at 50 ℃.
The invention has the technical effects that:
the method is simple, convenient, rapid and easy to operate, and the prepared MoS2/Sb2S3The composite photocatalyst has higher efficiency on photocatalytic degradation of rhodamine B, shows excellent adsorption performance and photocatalytic performance, and has certain application value.
Detailed Description
The following describes the substance of the present invention with reference to the examples.
Example 1
MoS2/Sb2S3The preparation method of the composite photocatalyst comprises the following steps: 6 parts of SbCl3And 9 parts of CH3CSNH2Dissolved in 60 parts of absolute ethyl alcoholMagnetically stirring for 30min under nitrogen atmosphere, and performing centrifugal separation to obtain a bright orange precursor; the prepared SbCl3Dissolving the bright orange precursor in 55 parts of deionized water, and magnetically stirring to obtain Sb2S3Precursor solution, 3 parts of H are added32Mo7N6O28And 6 parts of CH4N2S, magnetically stirring to obtain a mixed solution; finally transferring the mixed solution into a reaction kettle, putting the reaction kettle into a muffle furnace, sealing and heating the reaction kettle to 170 ℃, continuing for 26 hours, cooling the reaction kettle to room temperature, and then, adding MoS2/Sb2S3Centrifugally separating the composite photocatalyst, washing with anhydrous ethanol and deionized water for 5 times, drying in a vacuum drying oven at 50 deg.C for 14h, and cooling to obtain the final product; the raw materials are in parts by weight.
Example 2
MoS2/Sb2S3The preparation method of the composite photocatalyst comprises the following steps: 5 parts of SbCl3And 8 parts of CH3CSNH2Dissolving in 55 parts of absolute ethyl alcohol, magnetically stirring for 25min under the nitrogen atmosphere, and performing centrifugal separation to obtain a bright orange precursor; the prepared SbCl3Dissolving the bright orange precursor in 50 parts of deionized water, and magnetically stirring to obtain Sb2S3Precursor solution, 2 parts of H are added32Mo7N6O28And 5 parts of CH4N2S, magnetically stirring to obtain a mixed solution; finally transferring the mixed solution into a reaction kettle, putting the reaction kettle into a muffle furnace, sealing and heating the reaction kettle to 165 ℃ for 25 hours, cooling the reaction kettle to room temperature, and then, adding MoS2/Sb2S3Centrifugally separating the composite photocatalyst, washing with anhydrous ethanol and deionized water for 4 times, drying in a vacuum drying oven at 45 deg.C for 13h, and cooling to obtain the final product; the raw materials are in parts by weight.
Example 3
MoS2/Sb2S3The preparation method of the composite photocatalyst comprises the following steps: 7 parts of SbCl3And 10 parts of CH3CSNH2Dissolving in 65 parts of anhydrous ethanol, magnetically stirring under nitrogen atmosphere for 35min, and centrifuging to obtain bright orange extractDriving a body; the prepared SbCl3Dissolving the bright orange precursor in 60 parts of deionized water, and magnetically stirring to obtain Sb2S3Precursor solution, 4 parts of H are added32Mo7N6O28And 7 parts of CH4N2S, magnetically stirring to obtain a mixed solution; finally transferring the mixed solution into a reaction kettle, putting the reaction kettle into a muffle furnace, sealing and heating the reaction kettle to 175 ℃, keeping the temperature for 27 hours, cooling the reaction kettle to room temperature, and then, adding MoS2/Sb2S3Centrifugally separating the composite photocatalyst, washing with absolute ethyl alcohol and deionized water for 6 times, drying in a vacuum drying oven at 55 ℃ for 15h, and cooling to obtain the photocatalyst; the raw materials are in parts by weight.
The method is simple, convenient, rapid and easy to operate, and the prepared MoS2/Sb2S3The composite photocatalyst has higher efficiency on photocatalytic degradation of rhodamine B, shows excellent adsorption performance and photocatalytic performance, and has certain application value.

Claims (5)

1. MoS2/Sb2S3The preparation method of the composite photocatalyst is characterized by comprising the following steps: 5-7 parts of SbCl3And 8-10 parts of CH3CSNH2Dissolving in 55-65 parts of absolute ethyl alcohol, magnetically stirring for 25-35min under the atmosphere of nitrogen, and performing centrifugal separation to obtain a bright orange precursor; the prepared SbCl3Dissolving the bright orange precursor in 50-60 parts of deionized water, and magnetically stirring to obtain Sb2S3Adding 2-4 parts of H into the precursor solution32Mo7N6O28And 5-7 parts of CH4N2S, magnetically stirring to obtain a mixed solution; finally transferring the mixed solution into a reaction kettle, putting the reaction kettle into a muffle furnace, sealing and heating the reaction kettle to 165-175 ℃, keeping the temperature for 25-27h, cooling the reaction kettle to room temperature, and then, adding MoS2/Sb2S3Centrifugally separating the composite photocatalyst, washing with anhydrous ethanol and deionized water for 4-6 times, drying in a vacuum drying oven at 45-55 deg.C for 13-15h, and cooling; the raw materials are in parts by weight.
2. The method of claim 1, wherein: magnetically stir for 30min under nitrogen atmosphere.
3. The method of claim 1, wherein: putting the mixture into a muffle furnace, sealing and heating the mixture to 170 ℃.
4. The method of claim 1, wherein: lasting for 26 h.
5. The method of claim 1, wherein: drying in a vacuum drying oven at 50 deg.C for 14 h.
CN201811410612.2A 2018-11-24 2018-11-24 MoS2/Sb2S3Preparation method of composite photocatalyst Pending CN111215097A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112023985A (en) * 2020-09-28 2020-12-04 长春工业大学 Preparation method of composite nano photocatalytic material
CN112121826A (en) * 2020-10-16 2020-12-25 安徽理工大学 1T @2H-MoS2/SnS2Preparation method, product and application of visible light response photocatalyst

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112023985A (en) * 2020-09-28 2020-12-04 长春工业大学 Preparation method of composite nano photocatalytic material
CN112121826A (en) * 2020-10-16 2020-12-25 安徽理工大学 1T @2H-MoS2/SnS2Preparation method, product and application of visible light response photocatalyst

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Application publication date: 20200602