CN107803210A - One-step method prepares the excellent Bi of photocatalysis performance2S3The method of/BiOCl hetero-junctions - Google Patents
One-step method prepares the excellent Bi of photocatalysis performance2S3The method of/BiOCl hetero-junctions Download PDFInfo
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- CN107803210A CN107803210A CN201610810768.4A CN201610810768A CN107803210A CN 107803210 A CN107803210 A CN 107803210A CN 201610810768 A CN201610810768 A CN 201610810768A CN 107803210 A CN107803210 A CN 107803210A
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- biocl
- junctions
- nacl
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- urea
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- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 23
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 23
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 34
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000004202 carbamide Substances 0.000 claims abstract description 20
- 239000011780 sodium chloride Substances 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 5
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000035484 reaction time Effects 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 4
- 239000011941 photocatalyst Substances 0.000 abstract description 14
- 239000007864 aqueous solution Substances 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 4
- 239000000975 dye Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- 239000010842 industrial wastewater Substances 0.000 abstract description 2
- 231100000719 pollutant Toxicity 0.000 abstract description 2
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 13
- 239000000243 solution Substances 0.000 description 13
- 230000015556 catabolic process Effects 0.000 description 9
- 238000006731 degradation reaction Methods 0.000 description 9
- 238000005406 washing Methods 0.000 description 7
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 6
- 229940043267 rhodamine b Drugs 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 239000005864 Sulphur Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- HFZWRUODUSTPEG-UHFFFAOYSA-N 2,4-dichlorophenol Chemical class OC1=CC=C(Cl)C=C1Cl HFZWRUODUSTPEG-UHFFFAOYSA-N 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- VDQVEACBQKUUSU-UHFFFAOYSA-M disodium;sulfanide Chemical compound [Na+].[Na+].[SH-] VDQVEACBQKUUSU-UHFFFAOYSA-M 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 231100001231 less toxic Toxicity 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention discloses a kind of one-step method to prepare the excellent Bi of photocatalysis performance2S3The method of/BiOCl hetero-junctions, comprises the following steps：By Bi (NO3)3·5H2O, NaCl and thioacetamide are codissolved in the aqueous solution of urea；45 hours are stirred at room temperature；Reaction is washed after terminating and produces Bi2S3/ BiOCl heterojunction photocatalysts.The Bi obtained by the method for the invention2S3/ BiOCl hetero-junctions, specific surface area is big, and Bi2S3It can reach microcosmic close contact with BiOCl, therefore the activity of more excellent photocatalytic degradation of dye decomposition is shown than homogenous material, show that it has preferable application prospect in terms of the pollutant such as dyestuff in removing industrial wastewater.
Description
Technical field
The present invention relates to the Bi that photocatalysis performance is excellent2S3/ BiOCl hetero-junctions and preparation method thereof, it is particularly a kind of to use
One-step method prepares Bi2S3The method of/BiOCl hetero-junctions, belongs to field of inorganic nano-material preparation.
Background technology
In recent years, single photochemical catalyst due to light abstraction width it is narrow, light induced electron is easily compound with hole, causes photocatalysis
Performance can not meet actual industrial requirement.Heterojunction photocatalyst effectively prevents light induced electron due to that can expand light abstraction width
It is compound with hole, thus photocatalysis performance can be improved, and increasingly attract attention.
With industrial expansion, dyestuff and organic pollution have become main environmental contaminants.Removed by photocatalysis
Depollute thing, makes full use of the sunshine of green to have become a kind of most important method for removing pollutant as the energy.
BiOCl is due to less toxic or nontoxic, layer structure feature and has excellent ultraviolet and visible light catalysis activity, is likely to become new
Catalysis material.But when homogenous material is as photochemical catalyst, it is narrow to there is light abstraction width, it is seen that light utilization efficiency is low and carrier
The shortcomings of easily compound, by the Bi with photosensitive property2S3After being compounded to form hetero-junctions with BiOCl, photocatalysis performance will obtain significantly
Improve.
Bi2S3There is/BiOCl hetero-junctions excellent photocatalysis performance, Baibiao Huang etc. to first pass through hydro-thermal method preparation
BiOCl, then at room temperature, Bi is prepared for using ion-exchange2S3/ BiOCl hetero-junctions, have studied obtained Bi2S3/
The photocatalysis performance of 2,4- Dichlorophenols is catalytically decomposed in BiOCl hetero-junctions.Bi is prepared currently without on one-step method2S3/ BiOCl is different
The report of matter knot photochemical catalyst.
The content of the invention
It is an object of the invention to provide a kind of Bi with excellent photocatalysis performance2S3The preparation of/BiOCl hetero-junctions
Method.
The technical solution for realizing the object of the invention is：One-step method prepares the excellent Bi of photocatalysis performance2S3/ BiOCl is different
The method of matter knot, comprises the following steps：By Bi (NO3)3·5H2O, NaCl and thioacetamide（TAA）It is dissolved in urea liquid
Reaction solution is obtained, is reacted under normal temperature；Reaction is washed after terminating and produces Bi2S3/ BiOCl hetero-junctions.
In above-mentioned steps, Bi (NO3)3·5H2Molar concentrations of the O in reaction solution is 2/3 mol/L.
In above-mentioned steps, the molar concentration of urea liquid is 5.5-5.6 mol/L.
In above-mentioned steps, molar concentrations of the NaCl in reaction solution is 2/3 mol/L.
In above-mentioned steps, thioacetamide and NaCl mol ratio are 0.20-0.30.
In above-mentioned steps, the reaction time is 4-5 h.
Compared with prior art, the present invention has following remarkable advantage：
1st, method is simple, and without adding template, at room temperature, one-step method reacts to have obtained Bi2S3/ BiOCl heterojunction photocatalysis
Agent；
2nd, obtained Bi2S3/ BiOCl hetero-junctions has larger specific surface area；
3rd, the Bi2S3/ BiOCl heterojunction photocatalysts show excellent catalysis under excited by visible light to rhodamine B degraded
Performance, the activity than single photochemical catalyst BiOCl improve 3.3 times, are expected to have good application in industrial wastewater treatment field.
Brief description of the drawings
Fig. 1 is that one-step method of the present invention prepares Bi2S3The schematic flow sheet of/BiOCl heterojunction photocatalysts.
Fig. 2 is Bi made from embodiment 12S3The TEM figures of BiOCl prepared by/BiOCl heterojunction photocatalysts and comparative example,
Wherein, (a) comparative example 3；And (c) embodiment 1 (b)；(d) comparative example 4.
Fig. 3 is that the present invention obtains Bi2S3The degradation rate figure of/BiOCl heterojunction photocatalysts to rhodamine B.
Fig. 4 is comparative example various sulphur sources such as Na2Prepared Bi when S and thiocarbamide are as sulphur source2S3/ BiOCl is to rhodamine B
Degradation rate figure.
Fig. 5 is comparative example urea amount to prepared Bi2S3The influence figure of/BiOCl catalysis rhodamine B degradeds.
Fig. 6 is the comparative example reaction time to prepared Bi2S3The influence figure of/BiOCl catalysis rhodamine B degradeds.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
With reference to Fig. 1, the present invention is solvent using urea, prepares the excellent Bi of photocatalysis performance2S3/ BiOCl hetero-junctions light is urged
The method of agent, its feature comprise the following steps：
Step 1：By Bi (NO3)3·5H2O, NaCl and TAA are dissolved in aqueous solution of urea, Bi (NO3)3·5H2O molar concentrations are
2/3 mol/L, the molar concentration of urea is 5.5 ± 0.1 mol/L, and NaCl molar concentration is 2/3 mol/L, TAA and NaCl
Mol ratio be 0.3 ± 0.5；
Step 2：Step 1 solution is placed in beaker and reacts 4-5 h at room temperature；
Step 3：Reaction is washed after terminating and produces Bi2S3/ BiOCl heterojunction photocatalysts.
With reference to embodiment, comparative example and accompanying drawing, the present invention will be further described in detail：
Embodiment 1：
Step 1：By 2 mmol Bi (NO3)3·5H2O, 2mmol NaCl, 0.5mmol TAA are dissolved in 30 ml and contain 166
In the aqueous solution of mmol urea；
Step 2：Solution obtained by step 1 is reacted at room temperature in beaker, the reaction time is 5 h；
Step 3：Bi will be produced after product washing obtained by step 22S3/ BiOCl heterojunction photocatalysts.
Shown in the transmission electron microscope picture 2 of products therefrom, product is nanometer sheet.
Tested and found by its degradation rate to RhB solution in Fig. 3：Under excited by visible light, in 20min, degradation rate reaches
To 98%.Than not adding Bi2S3Single BiOCl activity improve 3.3 times.Comparative example 1：（Influence-the Na of sulphur source2S）
Step 1：By 2 mmol Bi (NO3)3·5H2O、2 mmol NaCl、0.5mmol Na2S is dissolved in 30 ml and contains 166
In the aqueous solution of mmol urea；
Step 2：Solution obtained by step 1 is reacted at room temperature in beaker, the reaction time is 5 h；
Step 3：Bi will be produced after product washing obtained by step 22S3/ BiOCl heterojunction photocatalysts.
The photocatalysis performance of products therefrom is as shown in Figure 4.
Comparative example 2：（Influence-thiocarbamide of sulphur source）
Step 1：By 2 mmol Bi (NO3)3·5H2O, 2 mmol NaCl, 0.5mmol thiocarbamides are dissolved in 30 ml and contain 166
In the aqueous solution of mmol urea；；
Step 2：Solution obtained by step 1 is reacted at room temperature in beaker, the reaction time is 5 h；
Step 3：Bi will be produced after product washing obtained by step 22S3/ BiOCl heterojunction photocatalysts.
The photocatalysis performance of products therefrom is as shown in Figure 4.
Comparative example 3：（The influence -0 of urea）
Step 1：By 2 mmol Bi (NO3)3·5H2O, 2 mmol NaCl, 0.5mmol TAA are dissolved in the 30 ml aqueous solution；
Step 2：Solution obtained by step 1 is reacted at room temperature in beaker, the reaction time is 5 h；
Step 3：Bi will be produced after product washing obtained by step 22S3/ BiOCl heterojunction photocatalysts.
Transmission electron microscope picture such as Fig. 2 of products therefrom, photocatalysis performance are as shown in Figure 5.
The photocatalysis performance of products therefrom is shown, when being not added with urea, RhB degradation rate is 30% in 20 min.
Comparative example 4：（The influence -60 of urea）
Step 1：By 2 mmol Bi (NO3)3·5H2O, 2mmol NaCl, 0.5mmol TAA are dissolved in 30 ml and contain 60 mmol
In the aqueous solution of urea；
Step 2：Solution obtained by step 1 is reacted at room temperature in beaker, the reaction time is 5 h；
Step 3：Bi will be produced after product washing obtained by step 22S3/ BiOCl heterojunction photocatalysts.
Transmission electron microscope picture such as Fig. 2 of products therefrom, the photocatalysis performance of products therefrom are as shown in Figure 5.Products therefrom
Photocatalysis performance is shown, when adding 60 mmol of urea amount, the degradation rate of rhodamine B is 80% in 20min.Degradation rate is all not so good as
Urea amount is 166mmol height.Comparative example 5：（Influence-the 3h in reaction time）
Step 1：By 2 mmol Bi (NO3)3·5H2O, 2mmol NaCl, 0.5mmol TAA are dissolved in 30 ml and contain 166
In the aqueous solution of mmol urea；
Step 2：Solution obtained by step 1 is reacted at room temperature in beaker, the reaction time is 3 h；
Step 3：Bi will be produced after product washing obtained by step 22S3/ BiOCl heterojunction photocatalysts.
The photocatalysis performance of products therefrom is as shown in fig. 6, degradation rate is not so good as 5h height.
Comparative example 6：（Influence-the 6h in reaction time）
Step 1：By 2 mmol Bi (NO3)3·5H2O, 2mmol NaCl, 0.5mmol TAA are dissolved in 30 ml and contain 166
In the aqueous solution of mmol urea；
Step 2：Solution obtained by step 1 is reacted at room temperature in beaker, the reaction time is 6 h；
Step 3：Bi will be produced after product washing obtained by step 22S3/ BiOCl heterojunction photocatalysts.
The photocatalysis performance of products therefrom is as shown in fig. 6, degradation rate is not so good as 5h height.
Claims (6)
1. one-step method prepares the excellent Bi of photocatalysis performance2S3The method of/BiOCl hetero-junctions, it is characterised in that including following step
Suddenly：By Bi (NO3)3·5H2O, NaCl and thioacetamide, which are dissolved in urea liquid, obtains reaction solution, is reacted under normal temperature；Reaction
Washed after end and produce Bi2S3/ BiOCl hetero-junctions.
2. the method as described in claim 1, it is characterised in that Bi (NO3)3·5H2Molar concentrations of the O in reaction solution is 2/3
mol/L。
3. the method as described in claim 1, it is characterised in that the molar concentration of urea liquid is 5.5-5.6 mol/L.
4. the method as described in claim 1, it is characterised in that molar concentrations of the NaCl in reaction solution is 2/3 mol/L.
5. the method as described in claim 1, it is characterised in that thioacetamide and NaCl mol ratio are 0.20-0.30.
6. the method as described in claim 1, it is characterised in that the reaction time is 4-5 h.
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| CN201610810768.4A CN107803210B (en) | 2016-09-08 | 2016-09-08 | One-step method for preparing Bi with excellent photocatalytic performance2S3Method for preparing/BiOCl heterojunction |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110227502A (en) * | 2019-06-11 | 2019-09-13 | 杭州电子科技大学 | A kind of method that one step of room temperature prepares the colored hetero-junctions of bismuthyl chloride/bismuth sulfide nano |
| CN110882705A (en) * | 2019-12-10 | 2020-03-17 | 武汉纺织大学 | Microwave synthesis oxygen vacancy BiOCl/Bi2S3Catalyst and preparation method and application thereof |
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2016
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110227502A (en) * | 2019-06-11 | 2019-09-13 | 杭州电子科技大学 | A kind of method that one step of room temperature prepares the colored hetero-junctions of bismuthyl chloride/bismuth sulfide nano |
| CN110882705A (en) * | 2019-12-10 | 2020-03-17 | 武汉纺织大学 | Microwave synthesis oxygen vacancy BiOCl/Bi2S3Catalyst and preparation method and application thereof |
| CN110882705B (en) * | 2019-12-10 | 2022-10-21 | 武汉纺织大学 | Microwave synthesis oxygen vacancy BiOCl/Bi 2 S 3 Catalyst and preparation method and application thereof |
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