CN109759082A - A kind of preparation method of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide - Google Patents

A kind of preparation method of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide Download PDF

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CN109759082A
CN109759082A CN201910132755.XA CN201910132755A CN109759082A CN 109759082 A CN109759082 A CN 109759082A CN 201910132755 A CN201910132755 A CN 201910132755A CN 109759082 A CN109759082 A CN 109759082A
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hexagonal prisms
catalyst
hollow porous
indium
composite photo
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陈亚杰
田国辉
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Heilongjiang University
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Heilongjiang University
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    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract

A kind of preparation method of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide, the present invention relates to composite materials and photocatalysis technology field.Solve the In of existing method preparation2O3The low problem of base heterojunction structure photocatalytic activity.Preparation method: one, hexagonal prisms presoma is prepared;Two, vulcanize;Three, carbon is removed, In is obtained2O3‑In2S3Hollow porous hexagonal prisms composite photo-catalyst.The present invention is used for the preparation of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide.

Description

A kind of preparation of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide Method
Technical field
The invention belongs to composite materials and photocatalysis technology field.
Background technique
In recent years, environmental pollution and energy shortages make the improvement of people's environmental pollution repair the demand with clean energy resource Give serious concern.In numerous pollutant process methods and using energy source strategy, conductor photocatalysis is as energy-efficient Green environmental protection technique, cost is relatively low, and solar energy can be absorbed and be converted into thermal energy and chemical energy etc., in degradation organic contamination There is vast potential for future development in terms of object, organic synthesis, photocatalysis Decomposition aquatic products hydrogen, production oxygen.Therefore, with traditional sewage Processing technique is compared to having great advantages, thus the extensive concern by domestic and foreign scholars.
In2O3It is n-type semiconductor, there is body-centered cubic structure, there are stable photoelectric properties.In2O3Band gap exist Between 3.5eV~3.7eV, wider band gap also causes it not absorb in visible-range, while simple In2O3Also it deposits In the compound very fast problem of photogenerated charge, this is also unfavorable for the raising of photocatalytic activity.And then also limit In2O3It is urged in light The application range in change field.In order to solve In2O3The photocatalytic applications the problem of, the research method mainly taken at present Be ion doping, plasma it is noble metal decorated, with narrowband based semiconductor its it is compound construct heterojunction structure, pass through these methods It uses, In can be significantly improved2O3Visible absorption and utilization, while improving the separation and transmission rate of photogenerated charge so that Photocatalytic activity is significantly improved.In2S3As narrowband based semiconductor (1.9-2.3eV), with higher to build photocatalysis living Property, it is widely used in light-catalyzed reaction.Research shows that In2S3And In2O3Heterojunction structure is built into show than single In2S3Or In2O3Higher photocatalytic activity.In2S3/In2O3In is usually first prepared in constructing for heterojunction structure2O3, utilize indium Source and In2O3It reacts and In is made2S3/In2O3.Such as: it is obtained by water (molten) agent thermal response to be added sulphur source, or by In2O3It is put into In tube furnace, it is passed through hydrogen sulfide gas preparation In in a heated condition2S3/In2O3Complex.For in same reaction simultaneously Obtain In2S3And In2O3And it is built into In2S3/In2O3The research of heterojunction structure is also rarely reported.Semiconductor light-catalyst is come It says, appearance structure has significant impact to photocatalytic activity.Numerous document report prove hollow porous material have than The more active sites of the solid material of identical pattern are more advantageous to penetrating and utilizing for light, while being also beneficial to anti- Answer the transmission of object.Therefore, how to pass through easy synthetic method building In2S3/In2O3Hollow porous heterojunction structure, to solve In2O3The low problem of photocatalytic activity is the research emphasis of existing art technology.
Summary of the invention
The invention solves the In of existing method preparation2O3The low problem of base heterojunction structure photocatalytic activity, and one kind is provided The preparation method of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide.
A kind of preparation method of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide, it is according to the following steps It carries out:
One, hexagonal prisms presoma is prepared:
Terephthalic acid (TPA) is dissolved in N, in N dimethyl acetamide, terephthalic acid solution is obtained, indium source is dissolved in N, N bis- In methylacetamide, indium source solution is obtained, then terephthalic acid solution is mixed, and stir to clarify with indium source solution, is obtained To mixed solution, it is 115 DEG C~125 DEG C that mixed solution, which is then heated to temperature, the condition for being 115 DEG C~125 DEG C in temperature Under, 20min~40min is heated, natural cooling and is centrifuged after heating, then with dry after ethanol washing, obtains hexagonal prisms presoma;
The concentration of the terephthalic acid solution is 2.5mg/mL~3.5mg/mL;The concentration of the indium source solution is 2.0mg/mL~3.5mg/mL;The volume ratio of the terephthalic acid solution and indium source solution are 1:(0.7~1.5);
Two, vulcanize:
Hexagonal prisms presoma and sulphur powder are uniformly mixed, mixture is obtained, mixture is laid in porcelain boat, and is placed in It is calcined in tube furnace, in a nitrogen atmosphere, calcination temperature is warming up to 500 DEG C~550 DEG C, be 500 DEG C~550 DEG C in temperature Under the conditions of, 1h~3h is calcined, then Temperature fall, obtains carbon containing In2O3-In2S3Hollow porous hexagonal prisms composite photocatalyst Agent;
The mass ratio of the hexagonal prisms presoma and sulphur powder is 1:(4~7);
Three, carbon is removed:
In air atmosphere, by carbon containing In2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst is heated to roasting temperature Degree is 450 DEG C~500 DEG C, under conditions of maturing temperature is 450 DEG C~500 DEG C, roasts 30min~60min, then naturally cold But room temperature is arrived, In is obtained2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst;
The In2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst diameter is 1 μm~2.5 μm, and length is 5 μm ~10 μm.
The beneficial effects of the present invention are: one, the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide of the present invention Preparation method is simple;
Two, cost is relatively low for the preparation method of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide of the present invention;
Three, In prepared by the present invention2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst forms hollow porous six rib The special construction of column, specific surface area with higher, can reach 96.3m2/ g or more, pattern is uniform, improves the utilization rate of light With the precipitation of product gas;
Four, photocatalytic activity enhances, In prepared by the present invention2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst is made Water Photocatalyzed Hydrogen Production can be effectively decomposed under simulated solar irradiation.50mg catalyst is added in 100 milliliters of water, using AM1.5 illumination 3h is penetrated, 226 μm of ol hydrogen can be obtained.Photochemical catalytic oxidation benzylamine generates the performance of N- benzylidenei benzylamine under simulated solar irradiation Test, the In of preparation2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst has the performance of good photochemical catalytic oxidation benzylamine Effect can obtain 91.3% yield by 5 hours radiation of visible light.
The present invention is used for a kind of preparation method of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide.
Detailed description of the invention
Fig. 1 is the SEM photograph of the hexagonal prisms presoma of one step 1 of embodiment preparation;
Fig. 2 is the XRD spectra of the hexagonal prisms presoma of one step 1 of embodiment preparation;
Fig. 3 is In prepared by embodiment one2O3-In2S3The SEM photograph of hollow porous hexagonal prisms composite photo-catalyst;
Fig. 4 is In prepared by embodiment one2O3-In2S3The XRD spectra of hollow porous hexagonal prisms composite photo-catalyst;
Fig. 5 is In prepared by comparative experiments one2O3The SEM photograph of photochemical catalyst;
Fig. 6 is In prepared by comparative experiments two2O3-In2S3The SEM photograph of porous solid hexagonal prisms composite photo-catalyst;
Fig. 7 is the performance test figure of the Photocatalyzed Hydrogen Production under simulated solar irradiation, and 1 is the In prepared using embodiment one2O3- In2S3Hollow porous hexagonal prisms composite photo-catalyst, 2 be the In prepared using comparative experiments one2O3Photochemical catalyst, 3 is using not In with hollow porous structure2O3-In2S3Composite photo-catalyst powder;
Fig. 8 is the performance test figure that photochemical catalytic oxidation benzylamine generates N- benzylidenei benzylamine under simulated solar irradiation, and 1 is to adopt The In prepared with embodiment one2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst, 2 is using without hollow porous knots The In of structure2O3-In2S3Composite photo-catalyst powder, 3 be the In prepared using comparative experiments one2O3Photochemical catalyst.
Specific embodiment
Specific embodiment 1: a kind of hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide of present embodiment Preparation method, it is to sequentially include the following steps:
One, hexagonal prisms presoma is prepared:
Terephthalic acid (TPA) is dissolved in N, in N dimethyl acetamide, terephthalic acid solution is obtained, indium source is dissolved in N, N bis- In methylacetamide, indium source solution is obtained, then terephthalic acid solution is mixed, and stir to clarify with indium source solution, is obtained To mixed solution, it is 115 DEG C~125 DEG C that mixed solution, which is then heated to temperature, the condition for being 115 DEG C~125 DEG C in temperature Under, 20min~40min is heated, natural cooling and is centrifuged after heating, then with dry after ethanol washing, obtains hexagonal prisms presoma;
The concentration of the terephthalic acid solution is 2.5mg/mL~3.5mg/mL;The concentration of the indium source solution is 2.0mg/mL~3.5mg/mL;The volume ratio of the terephthalic acid solution and indium source solution are 1:(0.7~1.5);
Two, vulcanize:
Hexagonal prisms presoma and sulphur powder are uniformly mixed, mixture is obtained, mixture is laid in porcelain boat, and is placed in It is calcined in tube furnace, in a nitrogen atmosphere, calcination temperature is warming up to 500 DEG C~550 DEG C, be 500 DEG C~550 DEG C in temperature Under the conditions of, 1h~3h is calcined, then Temperature fall, obtains carbon containing In2O3-In2S3Hollow porous hexagonal prisms composite photocatalyst Agent;
The mass ratio of the hexagonal prisms presoma and sulphur powder is 1:(4~7);
Three, carbon is removed:
In air atmosphere, by carbon containing In2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst is heated to roasting temperature Degree is 450 DEG C~500 DEG C, under conditions of maturing temperature is 450 DEG C~500 DEG C, roasts 30min~60min, then naturally cold But room temperature is arrived, In is obtained2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst;
The In2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst diameter is 1 μm~2.5 μm, and length is 5 μm ~10 μm.
The beneficial effect of present embodiment is: one, hollow porous six rib of present embodiment indium oxide-indium sulfide Preparation method is simple for column composite photo-catalyst;
Two, the preparation method of the hollow porous hexagonal prisms composite photo-catalyst of present embodiment indium oxide-indium sulfide at This is lower;
Three, the In of present embodiment preparation2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst forms hollow The special construction of porous hexagonal prisms, specific surface area with higher, can reach 96.3m2/ g or more, pattern is uniform, improves light Utilization rate and product gas precipitation;
Four, photocatalytic activity enhances, the In of present embodiment preparation2O3-In2S3Hollow porous hexagonal prisms complex light Catalyst work can effectively decompose water Photocatalyzed Hydrogen Production under simulated solar irradiation.50mg catalyst is added in 100 milliliters of water, uses AM1.5 light irradiates 3h, can obtain 226 μm of ol hydrogen.Photochemical catalytic oxidation benzylamine generates N- benzylidenei under simulated solar irradiation The performance test of benzylamine, the In of preparation2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst has good photochemical catalytic oxidation The impact of performance of benzylamine can obtain 91.3% yield by 5 hours radiation of visible light.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: indium source described in step 1 For In (NO3)3·4.5H2O.It is other same as the specific embodiment one.
Specific embodiment 3: unlike one of present embodiment and specific embodiment one or two: will in step 1 It is 115 DEG C~120 DEG C that mixed solution, which is heated to temperature, under conditions of temperature is 110 DEG C~125 DEG C, heating 20min~ 35min.It is other the same as one or two specific embodiments.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: institute in step 1 The concentration of the terephthalic acid solution stated is 3.0mg/mL~3.5mg/mL.It is other identical as specific embodiment one to three.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four: institute in step 1 The concentration for the indium source solution stated is 3.0mg/mL~3.5mg/mL.It is other identical as specific embodiment one to four.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five: institute in step 1 The volume ratio of the terephthalic acid solution and indium source solution that state are 1:(1~1.5).It is other with specific embodiment one or five phases Together.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six: in step 2 Under nitrogen atmosphere, calcination temperature is warming up to 500 DEG C~520 DEG C, under conditions of temperature is 500 DEG C~520 DEG C, calcining 1h~ 2h.It is other identical as specific embodiment one to six.
Specific embodiment 8: unlike one of present embodiment and specific embodiment one to seven: institute in step 2 The hexagonal prisms presoma stated and the mass ratio of sulphur powder are 1:(5~7).It is other identical as specific embodiment one to seven.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight: in step 3 Under air atmosphere, by carbon containing In2O3-In2S3It is 480 DEG C that hollow porous hexagonal prisms composite photo-catalyst, which is heated to maturing temperature, ~500 DEG C, under conditions of maturing temperature is 480 DEG C~500 DEG C, roast 40min~60min.Other and specific embodiment One to eight is identical.
Specific embodiment 10: unlike one of present embodiment and specific embodiment one to nine: in step 3 Under air atmosphere, by carbon containing In2O3-In2S3It is 450 DEG C that hollow porous hexagonal prisms composite photo-catalyst, which is heated to maturing temperature, ~500 DEG C, under conditions of maturing temperature is 450 DEG C~500 DEG C, roast 30min~40min.Other and specific embodiment One to nine is identical.
Beneficial effects of the present invention are verified using following embodiment:
Embodiment one:
A kind of preparation method of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide, it is characterised in that it is It sequentially includes the following steps:
One, hexagonal prisms presoma is prepared:
60.5mg terephthalic acid (TPA) is dissolved in 20mL N, in N dimethyl acetamide, obtains terephthalic acid solution, it will 60.3mg indium source is dissolved in 20mL N, in N dimethyl acetamide, indium source solution is obtained, then by terephthalic acid solution and indium source Solution mixing, and stir to clarify, mixed solution is obtained, it is 120 DEG C that mixed solution, which is then heated to temperature, is in temperature Under conditions of 120 DEG C, 35min is heated, natural cooling and is centrifuged after heating, then with dry after ethanol washing, before obtaining hexagonal prisms Drive body;
Two, vulcanize:
0.02g hexagonal prisms presoma and 0.1g sulphur powder are uniformly mixed, mixture is obtained, mixture is laid in porcelain boat In, and be placed in tube furnace and calcine, in a nitrogen atmosphere, calcination temperature is warming up to 500 DEG C, the item for being 500 DEG C in temperature Under part, 2h is calcined, then Temperature fall, obtains carbon containing In2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst;
Three, carbon is removed:
In air atmosphere, by carbon containing In2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst is heated to roasting temperature Degree is 480 DEG C, under conditions of maturing temperature is 480 DEG C, roasts 40min, then naturally cools to room temperature, obtain In2O3- In2S3Hollow porous hexagonal prisms composite photo-catalyst;
The In2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst diameter is 1 μm~2.5 μm, and length is 5 μm ~10 μm.
Indium source described in step 1 is In (NO3)3·4.5H2O。
Comparative experiments one: this comparative experiments is unlike embodiment one: sulphur powder is added without in step 2;Step 3 is last Obtain In2O3Photochemical catalyst.It is other to be the same as example 1.
Comparative experiments two: this comparative experiments is unlike embodiment one: in step 2 by 0.02g hexagonal prisms presoma and 0.2g sulphur powder is uniformly mixed, and obtains mixture;Step 3 finally obtains In2O3-In2S3Porous solid hexagonal prisms composite photocatalyst Agent.It is other to be the same as example 1.
Fig. 1 is the SEM photograph of the hexagonal prisms presoma of one step 1 of embodiment preparation;As seen from the figure, prepared by embodiment one Hexagonal prisms presoma be the smooth solid hexagonal prisms in surface, the diameter of cube is 1 μm or so, and length is 6 μm~8 μm left sides It is right.
Fig. 2 is the XRD spectra of the hexagonal prisms presoma of one step 1 of embodiment preparation;As seen from the figure, six rib of the present embodiment Column presoma is In base MIL-68 phase.
Fig. 3 is In prepared by embodiment one2O3-In2S3The SEM photograph of hollow porous hexagonal prisms composite photo-catalyst;By scheming It is found that In prepared by embodiment one2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst is the six hollow ribs of porous surface Column, the diameter of cube are 1 μm~2.5 μm, and length is 5 μm~10 μm.
Fig. 4 is In prepared by embodiment one2O3-In2S3The XRD spectra of hollow porous hexagonal prisms composite photo-catalyst;By scheming Prove that the present embodiment has prepared In2O3-In2S3The hollow hexagonal prisms catalyst of composite porous.
Fig. 5 is In prepared by comparative experiments one2O3The SEM photograph of photochemical catalyst;As seen from the figure, prepared by comparative experiments one In2O3Photochemical catalyst is solid hexagonal prisms, and the diameter of cube is 1 μm~2.5 μm, and length is 5 μm~10 μm.
Fig. 6 is In prepared by comparative experiments two2O3-In2S3The SEM photograph of porous solid hexagonal prisms composite photo-catalyst.By Figure is it is found that In prepared by comparative experiments two2O3-In2S3For porous solid hexagonal prisms, the diameter of cube is 1 μm~2.5 μm, long Degree is 5 μm~10 μm.
It is desorbed and is tested by nitrogen adsorption, obtain In manufactured in the present embodiment2O3-In2S3Hollow porous hexagonal prisms complex light Specific surface area of catalyst reaches 96.3m2/g。
In prepared by embodiment one2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst is ground, and is obtained In without hollow porous structure2O3-In2S3Composite photo-catalyst powder, the In prepared using embodiment one2O3-In2S3It is empty In prepared by the porous hexagonal prisms composite photo-catalyst of the heart, comparative experiments one2O3Photochemical catalyst and without hollow porous structure In2O3-In2S3Composite photo-catalyst powder is the performance test that catalyst decompose water Photocatalyzed Hydrogen Production, to 100 milliliters of water Middle addition 50mg catalyst irradiates 3h using AM1.5 light.
Fig. 7 is the performance test figure of the Photocatalyzed Hydrogen Production under simulated solar irradiation, and 1 is the In prepared using embodiment one2O3- In2S3Hollow porous hexagonal prisms composite photo-catalyst, 2 be the In prepared using comparative experiments one2O3Photochemical catalyst, 3 is using not In with hollow porous structure2O3-In2S3Composite photo-catalyst powder.As seen from the figure, In prepared by embodiment one2O3-In2S3 Hollow porous hexagonal prisms composite photo-catalyst has the impact of performance of good Photocatalyzed Hydrogen Production, shines by 3 hours visible lights It penetrates, 226 μm of ol hydrogen can be obtained, much higher than single catalyst In2O342 μm of ol hydrogen of photochemical catalyst, it was demonstrated that In2O3- In2S3Porous hollow hexagonal prisms photochemical catalyst can be with Photocatalyzed Hydrogen Production, and has good Photocatalyzed Hydrogen Production effect.And In2O3- In2S3Composite photo-catalyst powder obtains 168 μm of ol hydrogen, is lower than In2O3-In2S3The production of porous hollow hexagonal prisms photochemical catalyst Hydrogen amount, this proves that porous hollow hexagonal prisms structure is more advantageous to mentioning for photocatalytic activity relative to common nanoparticle powder It is high.
In prepared by embodiment one2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst is ground, and is obtained In without hollow porous structure2O3-In2S3Composite photo-catalyst powder, the In prepared using embodiment one2O3-In2S3It is empty In prepared by the porous hexagonal prisms composite photo-catalyst of the heart, comparative experiments one2O3Photochemical catalyst and without hollow porous structure In2O3-In2S3Composite photo-catalyst powder is that catalyst carries out the photochemical catalytic oxidation benzylamine generation N- benzyl Asia under simulated solar irradiation The performance test of methylbenzylamine, the reaction that photochemical catalytic oxidation benzylamine is converted into N- benzylidenei benzylamine is in 50 milliliters of quartz materials Reaction vessel in carry out, using equipped with AM1.5 optical filter CEL-HXF-300 xenon lamp as light source, infuse in the reaction vessel Enter 4 milliliters of acetonitrile solvents, 20 microlitres of benzylamine and 15mg catalyst, whole process carries out magnetic agitation, is passed through oxygen before illumination Then 30min clogs reactor.It is sampled after illumination certain time interval, filters, carried out using gas chromatography-mass spectrometry Qualitative and quantitative analysis.
Fig. 8 is the performance test figure that photochemical catalytic oxidation benzylamine generates N- benzylidenei benzylamine under simulated solar irradiation, and 1 is to adopt The In prepared with embodiment one2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst, 2 is using without hollow porous knots The In of structure2O3-In2S3Composite photo-catalyst powder, 3 be the In prepared using comparative experiments one2O3Photochemical catalyst.As seen from the figure, In prepared by embodiment one2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst has good photochemical catalytic oxidation benzylamine The impact of performance can obtain 91.3% yield by 5 hours radiation of visible light, much higher than single catalyst In2O3Light 33.3% yield of catalyst, it was demonstrated that In2O3-In2S3Porous hollow hexagonal prisms photochemical catalyst can with photochemical catalytic oxidation benzylamine, And there is good photocatalysis effect.Without the In of hollow porous structure2O3-In2S3Composite photo-catalyst powder obtains 63.2% yield is lower than In2O3-In2S391.3% yield of porous hollow hexagonal prisms photochemical catalyst, this proves porous air Heart hexagonal prisms structure is more advantageous to the raising of Photocatalytic oxidation activity relative to common nanoparticle powder.

Claims (10)

1. a kind of preparation method of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide, it is characterised in that it be by Following steps carry out:
One, hexagonal prisms presoma is prepared:
Terephthalic acid (TPA) is dissolved in N, in N dimethyl acetamide, terephthalic acid solution is obtained, indium source is dissolved in N, N dimethyl In acetamide, indium source solution is obtained, then terephthalic acid solution is mixed, and stir to clarify with indium source solution, is mixed Solution is closed, it is 115 DEG C~125 DEG C that mixed solution, which is then heated to temperature, under conditions of temperature is 115 DEG C~125 DEG C, is added Hot 20min~40min natural cooling and is centrifuged after heating, then with dry after ethanol washing, obtains hexagonal prisms presoma;
The concentration of the terephthalic acid solution is 2.5mg/mL~3.5mg/mL;The concentration of the indium source solution is 2.0mg/mL~3.5mg/mL;The volume ratio of the terephthalic acid solution and indium source solution are 1:(0.7~1.5);
Two, vulcanize:
Hexagonal prisms presoma and sulphur powder are uniformly mixed, mixture is obtained, mixture is laid in porcelain boat, and is placed in tubular type It is calcined in furnace, in a nitrogen atmosphere, calcination temperature is warming up to 500 DEG C~550 DEG C, the condition for being 500 DEG C~550 DEG C in temperature Under, 1h~3h is calcined, then Temperature fall, obtains carbon containing In2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst;
The mass ratio of the hexagonal prisms presoma and sulphur powder is 1:(4~7);
Three, carbon is removed:
In air atmosphere, by carbon containing In2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst is heated to maturing temperature and is 450 DEG C~500 DEG C, under conditions of maturing temperature is 450 DEG C~500 DEG C, 30min~60min is roasted, is then naturally cooled to Room temperature obtains In2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst;
The In2O3-In2S3Hollow porous hexagonal prisms composite photo-catalyst diameter is 1 μm~2.5 μm, and length is 5 μm~10 μ m。
2. a kind of preparation side of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide according to claim 1 Method, it is characterised in that indium source described in step 1 is In (NO3)3·4.5H2O。
3. a kind of preparation side of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide according to claim 1 Method, it is characterised in that it is 115 DEG C~120 DEG C that mixed solution, which is heated to temperature, in step 1, is 110 DEG C~125 DEG C in temperature Under conditions of, heat 20min~35min.
4. a kind of preparation side of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide according to claim 1 Method, it is characterised in that the concentration of terephthalic acid solution described in step 1 is 3.0mg/mL~3.5mg/mL.
5. a kind of preparation side of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide according to claim 1 Method, it is characterised in that the concentration of indium source described in step 1 solution is 3.0mg/mL~3.5mg/mL.
6. a kind of preparation side of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide according to claim 1 Method, it is characterised in that the volume ratio of terephthalic acid solution described in step 1 and indium source solution is 1:(1~1.5).
7. a kind of preparation side of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide according to claim 1 Method, it is characterised in that in step 2 in a nitrogen atmosphere, calcination temperature is warming up to 500 DEG C~520 DEG C, is 500 DEG C in temperature Under conditions of~520 DEG C, 1h~2h is calcined.
8. a kind of preparation side of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide according to claim 1 Method, it is characterised in that hexagonal prisms presoma described in step 2 and the mass ratio of sulphur powder are 1:(5~7).
9. a kind of preparation side of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide according to claim 1 Method, it is characterised in that in step 3 in air atmosphere, by carbon containing In2O3-In2S3Hollow porous hexagonal prisms composite photocatalyst It is 480 DEG C~500 DEG C that agent, which is heated to maturing temperature, under conditions of maturing temperature is 480 DEG C~500 DEG C, roasting 40min~ 60min。
10. a kind of preparation side of the hollow porous hexagonal prisms composite photo-catalyst of indium oxide-indium sulfide according to claim 1 Method, it is characterised in that in step 3 in air atmosphere, by carbon containing In2O3-In2S3Hollow porous hexagonal prisms composite photocatalyst It is 450 DEG C~500 DEG C that agent, which is heated to maturing temperature, under conditions of maturing temperature is 450 DEG C~500 DEG C, roasting 30min~ 40min。
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Application publication date: 20190517