CN105080573B - One kind prepares SnS using microwave-hydrothermal method2/SnO2The method of nano-photo catalytic composite - Google Patents
One kind prepares SnS using microwave-hydrothermal method2/SnO2The method of nano-photo catalytic composite Download PDFInfo
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Abstract
The present invention discloses a kind of using microwave-hydrothermal method preparation SnS2/SnO2The method of nano-photo catalytic composite, including：1) Sn sources solution A, S sources solution B, NaSO are prepared4Solution C；2) two kinds of solution of A, B are mixed to get solution D in proportion, two kinds of solution of A, C is mixed to get solution E in proportion；3) two kinds of solution of D, E are respectively put into microwave hydrothermal reaction kettle, seal water heating kettle, microwave hydrothermal reacts to obtain presoma；4) after question response kettle naturally cools to room temperature, presoma is taken out, product SnS is dried to obtain through centrifuge washing separation2And SnO2；5) by product SnS2And SnO2Physical mixed is carried out in proportion, obtains SnS2/SnO2Nano-photo catalytic composite, its particle size is about a few to tens of nanometers, purity is high, crystallinity is strong, pattern is uniform, and being applied to degradation of organic dyes has excellent Photocatalytic Degradation Property.
Description
【Technical field】
The present invention relates to nano composite photocatalytic field of material technology, and in particular to one kind prepares nano-photo catalytic composite wood
The method of material.
【Background technology】
SnS2(Tin sulfide) is the p-type semiconductor material of II-VI group, and its optical band gap is in 1.0-1.5eV, normal
It is a kind of solid matter of brownish black under normal temperature and pressure.Artificial gold is not soluble in water, but is dissolved in the concentrated hydrochloric acid and concentrated nitric acid of heat, in heat
Concentrated hydrochloric acid in dissolving generation SnCl2.This means artificial gold has the property of acidulous material.
The space group of the crystal structure of artificial gold belongs to Pnma races.Lattice parameter is respectively：A=1.1200nm, b=
0.3987nm, c=0.4334nm, artificial gold structure are to be overlapped mutually together by two layers and formed along axle.Each sulphur atom
It is connected within the same layer by three strong bonds (0.2627~0.2665nm) and two weak bonds (0.3290nm) with adjacent atom.
Also one is connected (0.3494nm) with neighbouring one layer atom, so as to form the octahedral structure of a high distortion, every
In individual layer, atom is combined by Van der Waals force between layers by Covalent bonding together.
SnO2It is extremely unstable with two kinds of crystal structures of tetragonal crystal system (rutile structure) and rhombic system, wherein orthorhombic phase
It is fixed, can only exist under the high temperature conditions, SnO under normal circumstances2Crystal is all to belong to rutile structure.Pure SnO2Crystal is colourless
It is transparent, it is a kind of n-type semiconductor of important broad-band gap, energy gap 3.65eV.Due to Sn electron affinity compared with
It is small, SnO2More Lacking oxygen in crystal be present, thus there is N-type semiconductor characteristic.Nano SnO2With quantum size effect,
Thus there can be broader energy gap.Because the small-size effect and skin effect that are shared with nano material, SnO2
Light absorbs, photocatalysis and air-sensitive response etc. all show special effect, in storage material, gas sensor, photocatalysis
Material, electrode material and solar cell material etc. have all widely been studied and applied.
That is reported at present prepares nanometer SnS by compound2The method of material is mainly Situ Hydrothermal oxidizing process [Yong C
Z,Zhen N D,Li K W,et al.High-Performance Visible-Light-Driven SnS/
SnO2Nanocomposite Photocatalyst Prepared Via In Situ Hydrothermal Oxidation
Of SnS Nanoparticles[J].Acs Appl.Mater.interfaces, 2011,3(5):1528-1537.], tradition
Hydro-thermal method [Chen C Y, Yokoshima T, Nara H, et al.One-Step Hydrothermal Synthesis of
SnS 2/SnO 2/C Hierarchical Heterostructures for Li-ion Batteries Anode with
Superior Rate Capabilities [J] .Electrochimica Acta, 2015.], wherein hydrothermal oxidization method is to compare
Effective chemical oxidation techniques, especially suitable for toxic and organic wastewater processing, but hydrothermal oxidization method is in high temperature height
Reacted in the environment of pressure, larger potential safety hazard be present.It is easy to get although conventional hydrothermal method has to crystallinity is strong, pattern
Special product, but conventional hydrothermal method even, the problems such as the thermal efficiency is low that thermal loss, uneven heating be present.
【The content of the invention】
SnS is prepared using microwave-hydrothermal method it is an object of the invention to provide one kind2/SnO2Nano-photo catalytic composite
Method, this method cost is low, simple to operate, short preparation period, the nanometer SnS of acquisition2/SnO2Nano composite material has excellent
Different photocatalysis performance.
To achieve these goals, the present invention adopts the following technical scheme that：
One kind prepares SnS using microwave-hydrothermal method2/SnO2The method of nano-photo catalytic composite, comprises the following steps：
1) Sn sources are dissolved in deionized water, are configured to concentration and are 0.5~1.2mol/L solution A, while adjust solution A
PH be 1~9, S sources are dissolved in deionized water, be configured to concentration be 0.1~2.4mol/L solution B, by NaSO4It is dissolved in
In deionized water, the solution C that concentration is 0.1~2.4mol/L is configured to；
2) by two kinds of solution of A, B according to elemental mole ratios nSn:nS=(1.0~2.5):The ratio of (1.8~4.0) mixes
To solution D, by two kinds of solution of A, C according to elemental mole ratios nSn:nO=(1.0~2.5):The ratio of (2.0~4.3) is mixed to get
Solution E, stir to form uniform and stable mixed solution respectively；
3) two kinds of solution of D, E are respectively put into microwave hydrothermal reaction kettle, seal water heating kettle, microwave hydrothermal is reacted before obtaining
Drive body；
4) after question response kettle naturally cools to room temperature, take out presoma, separated through centrifuge washing, respectively obtain sepia and
Yellow precursor product, it is dried to obtain product SnS2And SnO2；
5) by product SnS2And SnO2According to mass ratio mSnS2:mSnO2=1:0.5~1:2 carry out physics, obtain SnS/SnO2Receive
Rice optic catalytic composite material.
Further improve of the invention is：The Sn sources are SnCl4·5H2O。
Further improve of the invention is：The S sources are NaS9H2O。
Further improve of the invention is：Using 1mol/L HCl or NH in step 1)4·H2O adjusts pH value.
Further improve of the invention is：The volume packing ratio that water heating kettle is controlled in step 3) is 50%~60%, instead
Answering temperature control, the reaction time is controlled in 15~90min at 120~200 DEG C.
Further improve of the invention is：Dried described in step 4) is specially that 1~3h is dried at 60~80 DEG C.
Further improve of the invention is：Specifically include following steps：
1) by SnCl4·5H2O is dissolved in deionized water, is configured to concentration and is 0.5mol/L solution A, while uses 1mol/L
HCl or NH4·H2The pH of O regulation solution As is 1, by NaS9H2O is dissolved in deionized water, and it is 0.1mol/ to be configured to concentration
L solution B, by NaSO4It is dissolved in deionized water, is configured to the solution C that concentration is 0.1mol/L；
2) by two kinds of solution of A, B according to elemental mole ratios nSn:nS=1.0:1.8 ratio is mixed to get solution D, by A, C
Two kinds of solution are according to elemental mole ratios nSn:nO=1.0:2.0 ratio is mixed to get solution E, respectively the magnetic agitation at 26 DEG C
10min, form uniform and stable mixed solution；
3) two kinds of solution of D, E are respectively put into microwave hydrothermal reaction kettle, seal water heating kettle, control the volume packing ratio to be
50%, at 120 DEG C, reaction time control obtains presoma in 15min, reaction for reaction temperature control；
4) after question response kettle naturally cools to room temperature, presoma is taken out, is separated through centrifuge washing, is washed with deionized 3
It is secondary, then wash 3 times with absolute ethyl alcohol and respectively obtain sepia and white precursor product, 1h is dried at 60 DEG C and is obtained finally
Product SnS2And SnO2；
5) by final product SnS2And SnO2According to mass ratio mSnS2:mSnO2=1:0.5 carries out physics, produces SnS2/SnO2
Nano-photo catalytic composite.
Relative to prior art, the invention has the advantages that：
Compared with prior art, the present invention passes through two effects pair of molecular polarization and ionic conduction using microwave hydrothermal technology
Material directly heats, and it eliminates the thermal loss of traditional heating mode, thus the thermal efficiency of microwave heating is especially high, has and adds
Thermal velocity is fast, homogeneous heating without thermograde, without hysteresis effect the features such as.
The present invention prepares SnS2/SnO2The method of composite nanometer particle catalysis material, with preparing, cost is low, operation is simple
The characteristics of list, short preparation period, prepared SnS2/SnO2Composite nanometer particle catalysis material particle size is about several to several
Ten nanometers, purity is high, crystallinity is strong, pattern is uniform, being applied to degradation of organic dyes has excellent photocatalytic degradation
Can, the degradating organic dye under Hg lamp irradiation, the disposal efficiency reaches 98.7% in 5min, and process equipment is simple, feasibility is strong,
With good industrial prospect.
【Brief description of the drawings】
Fig. 1 is SnS prepared by the embodiment of the present invention 12/SnO2The SEM figures of nano-photo catalytic composite.Can be with from figure
Find out that the surface of sample is made up of nano particle, the size of particle is about a few to tens of nanometers.
Fig. 2 is the m in mass ratio of the embodiment of the present invention 1SnS2:mSnO2=1:SnS prepared by 0.52/SnO2Nano-photo catalytic is answered
Condensation material photocatalysis performance figure.It can be seen that Hg lamp irradiation 5min, prepared SnS2/SnO2Nano composite material is to having
The degradation rate of engine dyeing material reaches 98.7%.
【Embodiment】
Embodiment 1
1) by SnCl4·5H2O is dissolved in deionized water, is configured to concentration and is 0.5mol/L solution A, while uses 1mol/L
HCl or NH4·H2The pH of O regulation solution As is 1, by NaS9H2O is dissolved in deionized water, and it is 0.1mol/ to be configured to concentration
L solution B, by NaSO4It is dissolved in deionized water, is configured to the solution C that concentration is 0.1mol/L.
2) by two kinds of solution of A, B according to elemental mole ratios nSn:nS=1.0:1.8 ratio is mixed to get solution D, by A, C
Two kinds of solution are according to elemental mole ratios nSn:nO=1.0:2.0 ratio is mixed to get solution E, respectively the magnetic agitation at 26 DEG C
10min, form uniform and stable mixed solution.
3) two kinds of solution of D, E are respectively put into microwave hydrothermal reaction kettle, seal water heating kettle, control the volume packing ratio to be
50%, at 120 DEG C, reaction time control obtains presoma in 15min, reaction for reaction temperature control.
4) after question response kettle naturally cools to room temperature, presoma is taken out, is separated through centrifuge washing, is washed with deionized 3
It is secondary, then wash 3 times with absolute ethyl alcohol and respectively obtain sepia and white precursor product, 1h is dried at 60 DEG C and is obtained finally
Product SnS2And SnO2。
5) by final product SnS2And SnO2According to mass ratio mSnS:mSnO2=1:0.5 carries out physics, produces SnS2/SnO2It is multiple
Close nanometer product.
Embodiment 2
1) by SnCl4·5H2O is dissolved in deionized water, is configured to concentration and is 0.7mol/L solution A, while uses 1mol/L
HCl or NH4·H2The pH of O regulation solution As is 7, by NaS9H2O is dissolved in deionized water, and it is 1mol/L to be configured to concentration
Solution B, by NaSO4It is dissolved in deionized water, is configured to the solution C that concentration is 1.5mol/L.
2) by two kinds of solution of A, B according to elemental mole ratios nSn:nS=2.0:3.0 ratio is mixed to get solution D, by A, C
Two kinds of solution are according to elemental mole ratios nSn:nO=2.5:4.0 ratio is mixed to get solution E, respectively the magnetic agitation at 26 DEG C
5min, form uniform and stable mixed solution.
3) two kinds of solution of D, E are respectively put into microwave hydrothermal reaction kettle, seal water heating kettle, control the volume packing ratio to be
50%, at 160 DEG C, reaction time control obtains presoma in 30min, reaction for reaction temperature control.
4) after question response kettle naturally cools to room temperature, presoma is taken out, is separated through centrifuge washing, is washed with deionized 2
It is secondary, then wash 2 times with absolute ethyl alcohol and respectively obtain sepia and white precursor product, 1h is dried at 60 DEG C and is obtained finally
Product SnS2And SnO2。
5) by final product SnS2And SnO2According to mass ratio mSnS2:mSnO2=1:1 carries out physics, produces SnS2/SnO2It is multiple
Close nanometer product.
Embodiment 3
1) by SnCl4·5H2O is dissolved in deionized water, is configured to concentration and is 1.2mol/L solution A, while uses 1mol/L
HCl or NH4·H2The pH of O regulation solution As is 9, by NaS9H2O is dissolved in deionized water, and it is 2.4mol/ to be configured to concentration
L solution B, by NaSO4It is dissolved in deionized water, is configured to the solution C that concentration is 2.4mol/L.
2) by two kinds of solution of A, B according to elemental mole ratios nSn:nS=2.5:4.0 ratio is mixed to get solution D, by A, C
Two kinds of solution are according to elemental mole ratios nSn:nO=2.0:4.3 ratio is mixed to get solution E, respectively the magnetic agitation at 26 DEG C
30min, form uniform and stable mixed solution.
3) two kinds of solution of D, E are respectively put into microwave hydrothermal reaction kettle, seal water heating kettle, control the volume packing ratio to be
60%, at 200 DEG C, reaction time control obtains presoma in 90min, reaction for reaction temperature control.
4) after question response kettle naturally cools to room temperature, presoma is taken out, is separated through centrifuge washing, is washed with deionized 3
It is secondary, then wash 3 times with absolute ethyl alcohol and respectively obtain sepia and white precursor product, 3h is dried at 80 DEG C and is obtained finally
Product SnS2And SnO2。
5) by final product SnS2And SnO2According to mass ratio mSnS:mSnO2=1:2 carry out physics, produce SnS2/SnO2It is compound
Nanometer product.
Refer to shown in Fig. 1 and Fig. 2, SnS prepared by the present invention2/SnO2Combination product is nanoparticle structure powder, its
Prepare that cost is low, reaction time is short, excellent, the degradating organic dye under Hg lamp irradiation of saving the energy, photocatalysis performance, in 5min
The disposal efficiency reaches 98.7%, and process equipment is simple, feasibility is strong, has good industrial prospect.
Claims (1)
1. one kind prepares SnS using microwave-hydrothermal method2/SnO2The method of nano-photo catalytic composite, it is characterised in that including
Following steps：
1) by SnCl4·5H2O is dissolved in deionized water, is configured to the solution A that concentration is 0.5mol/L, while with 1mol/L's
HCl or NH4·H2The pH of O regulation solution As is 1, by NaS9H2O is dissolved in deionized water, and it is 0.1mol/L's to be configured to concentration
Solution B, by NaSO4It is dissolved in deionized water, is configured to the solution C that concentration is 0.1mol/L；
2) by two kinds of solution of A, B according to elemental mole ratios nSn:nS=1.0:1.8 ratio is mixed to get solution D, by two kinds of A, C
Solution is according to elemental mole ratios nSn:nO=1.0:2.0 ratio is mixed to get solution E, respectively the magnetic agitation at 26 DEG C
10min, form uniform and stable mixed solution；
3) two kinds of solution of D, E are respectively put into microwave hydrothermal reaction kettle, seal water heating kettle, it is 50% to control volume packing ratio,
At 120 DEG C, reaction time control obtains presoma in 15min, reaction for reaction temperature control；
4) after question response kettle naturally cools to room temperature, presoma is taken out, separates, is washed with deionized 3 times through centrifuge washing, then
3 times are washed with absolute ethyl alcohol and respectively obtains sepia and white precursor product, and 1h is dried at 60 DEG C and obtains final product
SnS2And SnO2；
5) by final product SnS2And SnO2According to mass ratio mSnS2:mSnO2=1:0.5 carries out physical mixed, produces SnS2/SnO2
Nano-photo catalytic composite；
Hg lamp irradiation 5min, prepared SnS2/SnO2Nano composite material reaches 98.7% to the degradation rate of organic dyestuff.
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| CN113731444B (en) * | 2021-08-26 | 2022-11-15 | 杭州电子科技大学 | Sb-SnO for degrading organic wastewater 2 /SnS 2 Nano catalyst and preparation method and application thereof |
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| CN101609886B (en) * | 2009-07-16 | 2011-08-17 | 浙江大学 | Preparation method of SnO2/SnS2 nano composite electrode material of lithium ion battery |
| CN102671676A (en) * | 2012-05-23 | 2012-09-19 | 上海师范大学 | Preparation method for SnO2/SnS2 heterostructure photocatalyst |
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| Hydrothermal synthesis of SnO2/SnS2 nanocomposite with high visible light-driven photocatalytic activity;Yong Cai Zhang等;《Materials Letters》;20110621;第65卷;第2节 * |
| Microwave solvothermal synthesis of flower-like SnS2 and SnO2 nanostructures as high-rate anodes for lithium ion batteries;Yuqin Zou等;《Chemical Engineering Journal》;20130613;第229卷;第2.1节 * |
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